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SB Eh
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The D. Van Nostrand Company
intend this book to be sold to the Public
at the advertised price, and supply it to
the Trade on terms which will not allow
of discount.
A MANUAL OF
CEMENT TESTING
FOR THE USE OF ENGINEERS
AND CHEMISTS IN COLLEGES
AND IN THE FIELD
BY
WILLIAM ALLYN RICHARDS, B.S. IN M.E.
Instructor in the University of Chicago , Junior Member A *S.M.E.
Member A merican Gas Institute, A merican Chemical Society
AND
HENRY BRIGGS NORTH, D.Sc.
Associate Professor of Chemistry in Rutgers Collegt
Member of the A merican Chemical Society
A merican Electrochemical Society
Societe chimique de France
ILLUSTRATED
NEW YORK
D. VAN NOSTRAND COMPANY
25 PARK PLACE
1912
COPYRIGHT, 1912,
BY
D. VAN NOSTRAND COMPANY
Stanbope jpress
F. H. GILSON COMPANY
BOSTON, U.S.A.
PREFACE.
IN order to insure uniformity of results in the testing of
cement, it is essential that each test should invariably be
made in precisely the same manner and under exactly the
same conditions. A committee of the American Society
of Civil Engineers has, with this aim in view, prepared and
published a set of Standard Methods of Testing Cement,
and these methods are to-day employed throughout the
United States.
This little volume, as its name implies, is a laboratory
manual on cement testing, and is intended to assist in
bringing about uniformity in the testing of cement. The
authors have endeavored to present, in a somewhat con-
densed form, such directions as will enable a student in the
laboratory or an operator in the field office to correctly
interpret the Standard Methods of Testing and Specifica-
tions for Cement as published by the committee of the
American Society of Civil Engineers, American Society for
Testing Materials, Association of American Portland Cement
Manufacturers, and the American Railway Engineers and
Maintenance of Way Association; they have endeavored
to give sufficient detail to enable all students to learn the
same manipulations and thus be able to perform each test
in a certain well defined and similar manner.
ill
268767
IV PREFACE
All of the tests described have been performed in the
laboratory under the eyes of the writers and have been
found to produce uniformly good results.
Acknowledgment has been made to various authorities
on the subject by special mention or as references at the
end of the several chapters.
Any corrections or suggestions will be gratefully received.
W. A. R.
H. B. N.
June i5th, 1912.
CONTENTS.
PART I.
PAGE
INTRODUCTION ix
CHAPTER I.
CLASSIFICATION, COMPOSITION, MANUFACTURE.
Definition — Classification — Portland — Natural — Pozzuo-
lana — Mixed — Distinguishing Features — Composition — Silica
— Lime — Alumina — Iron Oxide — Magnesia — Sulphuric Acid
— Sulphur — Alkalies — Carbonic Acid — Manufacture — Raw
Materials — Cement Rock — Limestone — Marl — Clay — Chalk
- Alkali Waste — Mixing (Wet Process, Dry Process) — Kilns
(Stationary, Rotary) — Grinding — References i
CHAPTER II.
SAMPLING.
Storage — Collecting the Sample — Sample Cans — References . . 7
CHAPTER III.
FINENESS.
Importance — Method — Apparatus (Sieves, Scales) — To
Make the Test — Results — Deductions — References 9
CHAPTER IV.
SPECIFIC GRAVITY.
Definition — Significance — Apparatus (Le Chatelier Specific
Gravity Flask, Funnel, Chemical Balance) — To Make the Test —
Calculation — Cleaning the Flask — Conclusion — References ... 14
v
vi CONTENTS
CHAPTER V.
NORMAL CONSISTENCY, MIXING, TIME OF SET.
PAGE
Significance — Standard — Apparatus (Vicat Apparatus, Scales,
Burette) — Mixing — To Make the Test — Time of Set — Sig-
nificance — To Make the Test — Conclusions — References 20
CHAPTER VI.
CONSTANCY OF VOLUME.
Significance — Kinds of Tests (Normal, Accelerated) — Appara-
tus (Boiling Apparatus) — To Make the Tests — Conclusions —
References 28
CHAPTER VII.
TENSILE STRENGTH.
Use — Factors Affecting Strength — Composition — Fineness —
Amount of Water — Apparatus (Molds, Testing Machines) — To
Make the Tests (Neat Cement) — To Make the Test (Mortar) —
Determine the Percentage of Water — Method of Mixing —
Breaking (Briquettes) — Conclusions — References 33
CHAPTER VIII.
COMPRESSIVE STRENGTH AND TRANSVERSE TESTS.
Compressive Strength — Molds — To Make the Test (Neat,
Mortar) — Breaking — Conclusions — Transverse Tests (Modu-
lus of Rupture) — Molds — To Make the Test — Breaking —
Calculations — Conclusions — References 41
CHAPTER IX.
SAND AND STONE.
Sand — Test of Natural Sand — Per Cent of Loam — Mechani-
cal Analysis — Apparatus — To Make the Test — The Uniformity
Coefficient — The Effective Size — To Find the Uniformity Co-
efficient and Effective Size — Voids — Apparatus — To Make the
Test — Stone — Mechanical Analysis (Apparatus, To Make the
Test) — Voids (Apparatus, Specific Gravity, To Make the Test) —
References 49
CONTENTS vii
CHAPTER X.
LABORATORY EQUIPMENT.
PAGE
Special Apparatus — Machines (Tension Test) — Long Lever —
Shot — Spring Balance — Clips — Transverse Tool — Compres-
sion Tool — Universal Testing Machine — Sand Shaker — Scales
and Balance — Boiling Apparatus — Moist Closet — Storage —
Tanks — Table — Burette — Molds (Briquette, Cube, Bar) -
Miscellaneous Apparatus 63
PART II.
INTRODUCTION
Part played by Chemical Analysis; Preparation of Sample for
Analysis 80
ANALYSIS OF CEMENT
Determination of Loss on Ignition — Silica (SiO2) — Iron and
Alumina (Fe2O3 and A12O3) — Lime (CaO) — Magnesia (MgO) —
Sulphuric Acid (SO3) — Total Sulphur (S) — Sulphur as Sulphide
(S) — Moisture — Alkalies (K2O and Na2O) — Carbon Dioxide
(CO.) 84
ANALYSIS or LIMESTONE 106
ANALYSIS OF MARL 107
ANALYSIS OF SLAG 107
ANALYSIS OF CLAY 107
PART I.
INTRODUCTION.
THE Portland Cement Industry in the United States has
had a most marvelous development. In 1880 the United
States produced 82,000 barrels of Portland Cement, while
in 1910 the output was estimated to be 70,000,000 barrels.
This great increase in the use of cement is fitting testi-
mony of its great value as a material of construction.
Like all other materials used in construction, cement
must be tested. Iron, steel, wood and stone, in their
preparation for use or tests, have only their shapes changed ;
but it is quite different with cement, which comes from the
manufacturer to the testing laboratory, or wherever it is to
be used, in the form of a fine powder, there to be mixed with
water into a paste and deposited in forms till hardened
into a solid. It is evident that of all materials of construc-
tion subjected to a system of testing, cement is probably
the most dependent on the judgment and skill of the person
making the tests. It was with a view to eliminating this
personal factor as far as possible, and thereby placing the
tests of one operator, or one laboratory, on a basis of
comparison with another operator or laboratory, that the
American Society of Civil Engineers and several other
societies appointed a committee to draw up specifications
to be used in all tests of cement in the United States.
X INTRODUCTION
These specifications form the basis of this manual, and
whenever the term " Standard Specifications," is used, it
refers to the "Standard Methods of Testing and Specifi-
cations for Cement," of the American Society of Civil
Engineers.
Classes. Cement tests are of two classes: (i) Experi-
mental Tests, made for scientific purposes, and comprising
such tests as modulus of elasticity, coefficient of expansion,
etc., and (2) Routine Tests, made to ascertain if a certain
consignment of cement will answer the requirements of a
set of specifications, as regards soundness and strength.
The routine tests usually employed are fineness, spe-
cific gravity, soundness, tensile strength (both neat and
sand), and time of set, while compression and transverse
tests are sometimes used.
The tests for soundness and strength are called primary
tests, while fineness, specific gravity, etc., are called second-
ary, since they give only additional information, which is
of little value in itself.
Routine tests alone will be considered in this work.
CEMENT TESTING
CHAPTER I.
CLASSIFICATION, COMPOSITION, MANUFACTURE.
Definition. Hydraulic cement is a material, which, when
pulverized and mixed into a more or less pasty mass with
water, has the property of setting or hardening under water.
Classification. Cements are usually classified as follows :
(i) Portland, (2) natural, (3) Pozzuolana, (4) blended or
mixed.
Portland cement is the finely ground powder of a clinker
resulting from the incipient fusion of an intimate artifi-
cial mixture of finely ground calcareous and argillaceous*
materials, and must contain no materials added after cal-
cination other than a small amount of calcium sulphate to
regulate setting.!
Natural cement is the finely ground powder of a clinker,
* Calcareous — partaking of the nature of calcite or calcium carbonate
Argillaceous — of a clayey nature.
t This definition is sometimes further limited by stating: The finished
product must contain at least 1.7 times as much lime, by weight, as silica
alumina and iron oxide combined.
; CGEMENT TESTING
resulting from the burning, at a heat below incipient fusion,
of argillaceous limestone or other suitable natural rock.
Pozzuolana cement results from grinding and mixing in
definite proportions slaked lime and blast furnace slag, or
certain volcanic lava.
Mixed cement is, as the name implies, a cement made up
of different brands or kinds of cements, and sometimes
inert substances.
Distinguishing Features. Natural or common cements
are light or dark gray, according to the stone from which
they are made. The specific gravity is from 2.7 to 3.0, with
an average about 2.85. Portland cements have a specific
gravity of from 3.0 to 3.5, averaging about 3.15. Natural
cements have much quicker set and are lower in strength
in the earlier tests.
Pozzuolana cement made from slag is characterized
chiefly by its light lilac color, absence of grit, low specific
gravity (2.6-2.8), and by the intense bluish green color of
a fresh fracture after long submersion in water.
Composition. The basic elements of Portland cement
are silica, alumina and lime. Ingredients such as iron,
magnesia, alkalies, sulphuric acid, carbonic acid, and water
also occurs in varying quantities, replacing some of the
basic elements.
The following represents about the limits within which
fall the constituents of various American Portland cements,
which pass the Standard Specifications for soundness,
setting time and tensile strength:
CLASSIFICATION, COMPOSITION, MANUFACTURE 3
Per Cent.
Silica 20 to 24
Alumina 5 to 9
Iron Oxide 2 to 4
Lime 60 to 63.5
Magnesia i to 2
Sulphur Trioxide 1.5
The following represents an average:
Per Cent.
Silica 22.0
Alumina 7.5
Iron Oxide 2.5
Lime 62.0
Magnesia 2.5
Sulphur Trioxide 1.5
Silica (Si02). 19-24 per cent, exists in combination with
lime as calcium silicate, which is an active hardening
factor. It should not be present as free silica.
Lime (CaO). 59-67 per cent, depending on the relative
proportions of alumina and silica and care with which the
cement has been manufactured. When in the combined
state the greater the amount the stronger the cement.
Excess of lime, or lime in the free state, will make an un-
sound cement by expanding due to slaking. The more
lime, the slower the setting.
Alumina (A1203). 5-10 per cent, mostly combined as
calcium aluminate. The greater the proportion, the quicker
the setting and the lower ultimate tensile strength. Le
Chatelier believes calcium aluminate to be the greatest
factor in hardening.
Iron Oxide (Fe20s). Usually less than 4 per cent.
Probably has little influence on the cement, though be-
lieved by some to act the same as alumina.
4 CEMENT TESTING
Magnesia (MgO). 2-4 per cent, by some considered as
an impurity, while other investigators claim it acts the
same as lime. Four per cent is placed as the limit by the
Standard Specifications.
Sulphuric Acid or Sulphur Trioxide (SOs). 1.25-1.75
per cent, due mostly to the introduction of calcium sul-
phate into the finished cement to regulate setting. The
more calcium sulphate (CaSO4) the slower the set. It
should never exceed 2-3 per cent, while the Standard
Specifications limits it to 1.75.
Sulphur (S). Found only in small amounts, usually
comes from the coal used in burning the clinker, though
sometimes from the raw materials. Sulphides, when in any
considerable quantity, cause discolorations (dark blue
spots) in the cement on hardening, and disintegration due
to oxidation.
Alkalies (K2O and Na20). 0.5-2 per cent, have little
or no effect on cement unless in large quantities.
Carbonic Acid (CO2). 0.5-1.5 per cent, due mostly to
absorption from the air; a large proportion shows under-
burning or excess of lime.
Natural and Pozzuolana Cements. The constituents of
natural and Pozzuolana cements are practically the same
as those of Portland cement, except that in the natural they
are found in varying proportions.
The following analyses* will serve to illustrate.
* From Eckel's " Cement Materials and Industry."
CLASSIFICATION, COMPOSITION, MANUFACTURE
Portland.
Natural.
Pozzuolana.
Silica
21 . ^O
26.40
28 o<
Alumina
7.65
6.28
II .40
Iron
2.85
I .OO
o. 54
Lime
60 (K
4< 22
^O 20
M^agnesia
2 (K
O OO
2 06
Sulphuric acid
I 8l
I 37
Alkali
I . 1^
4.00
Carbonic acid and water
7.86
•2 . 7Q
As the composition of natural cement from different
plants, and frequently from the same plant, varies greatly,
the analysis just given must not be considered as an aver-
age, but simply as an illustration.
MANUFACTURE.
Raw Materials. The essentials, silica, lime and alumina,
are obtained from six different sources.
(1) Cement rock and limestone.
(2) Limestone and clay.
(3) Marl and clay.
(4) Chalk and clay.
(5) Slag and limestone.
(6) Alkali waste and clay.
Cement rock, from which about two- thirds of the cement
manufactured in the United States is made, is an argilla-
ceous limestone, low in magnesia.
Marl, an almost pure calcium carbonate, is a soft, wet,
calcareous earth.
Clay is a more or less plastic substance composed chiefly of
aluminum silicate, formed by the decomposition of minerals.
6 CEMENT TESTING
Chalk, a soft, earthy variety of limestone or carbonate
of lime, is usually of a yellowish-white color, but is some-
times snow white. It is easily broken, has an earthy frac-
ture, is rough, dry and harsh to the touch, and adheres
slightly to the tongue. It sometimes contains a little
silica, alumina, or magnesia, and occasionally all three.
Limestone is a substance formed when clay has been
deposited with calcareous matter.
Alkali waste is the refuse from the manufacture of soda.
It exists as caustic lime.
These materials are very carefully analyzed and propor-
tioned before mixing. The mixing is done in one of two
ways, (i) by a wet or (2) by a dry process, after which the
mixture is calcined. For this there are two kinds of kilns
in use: (i) the stationary and (2) the rotary. Including
the grinding of the clinker, the manufacture of cement,
regardless of the process or method used, consists of three
steps: (i) mixing and grinding, (2) calcining the mixture,
and (3) reducing the clinker to a powder.
REFERENCES.
"Practical Cement Testing," by Taylor; "Concrete: Plain and
Reinforced," by Taylor and Thompson; "Examination of Portland
Cement," by R. K. Meade; "Manufacture of Portland Cements,"
by A. V. Bleininger; "Fourth Series," Bulletin 3, Ohio Geological
Survey.
CHAPTER II.
SAMPLING.
Storage. Cement is shipped in wooden barrels, cloth or
paper bags, none of which furnish very good protection
for its contents. Therefore, it is necessary to provide a
good dry storage place.
Inspection. The material, the condition of the packages,
and, if possible, the transporting medium of each shipment
should be thoroughly examined. Be very careful in the ex-
amination of the storage room or warehouse. It must be dry
and free from leaks. All packages should bear the manu-
facturer's name or trade-mark, and any unmarked packages
should be rejected. If the specifications call for sealed
packages, all packages should be sealed and all seals should
be similar. The cement should contain no hard lumps, as
these indicate injury from moisture, which has caused
partial set. Soft lumps easily broken by the fingers indi-
cate aging, which is not harmful. It is well to ascertain
the average weight of the packages.
Collecting the Sample. The selection of the sample for
testing must be left largely to the discretion of the party
taking it. The quantity must depend upon the importance
of the work and the number of tests to be made, as well as
the facilities for making them — usually 8 to 10 pounds.
7
8 CEMENT TESTING
The sample must be a fair average of the shipment and also
of the package. One barrel in ten is a fair average for a
large shipment, but on small work or in small shipments
samples should be taken more often; and never less than
five bags should be sampled.
To obtain an average of the shipment, the samples should
be taken from packages in different parts of the pile. An
average of the package is
K obtained by means of a
sampling auger (Fig. i), such
FIG i as is used by butter or sugar
inspectors, inserting it from
top to center in bags, and from side to center in barrels,
midway between the heads.
Sample cans * marked with all necessary information as
to the shipment, brand, manufacturer, etc-., should be used
to store the sample in, until tested. Each sample should
be thoroughly mixed and passed through a sieve having
twenty meshes per linear inch, in order to break up lumps
and remove foreign material and further mix the sample.
REFERENCE.
"Practical Cement Testing," by Taylor.
* Mason (fruit) jars make good sample jars.
CHAPTER III.
FINENESS.
Importance. In itself, fineness is of little importance,
but because it affects the other properties it becomes of
considerable moment.
In the early stages of hardening only the finer particles
have any effect, as water is slow in reaching the interior of
the larger particles, thereby delaying the hydraulic action.
Also, the finer particles will more easily cover the sand
grains, making mortar much stronger, and allowing the use
FIG. 2.
of a larger percentage of sand. Neat cement mixtures are
usually less strong with fine than with coarse cement.
Seasoning can take place more easily with finely ground
cement; because of this, fine cement is less liable to un-
soundness.
9
10 CEMENT TESTING
Method. Fineness is determined by passing the cement
through sieves (Fig. 2) ; other methods by means of currents
of air or liquids have been proposed but are little used.*
Apparatus. Sieves, numbers 20, 50, 100 and 200, pan
and cover, shot and scales. The sieves should be circular,
between 6 and 8 inches in diameter and i\ inches deep,
provided with a pan 2 inches deep, and a cover.
The wire cloth should be woven from brass wire having
diameters as follows :
Inches.
No. 20 0.034
No. 50 0.0090
No. zoo 0.0045
No. 200 0.0024
The cloth should be mounted on the frames without dis-
tortion; the mesh should be regular in spacing and within
the following limits :
No. 50 not less than 48 nor more than 50 per linear inch.
No. 100 not less than 96 nor more than 100 per linear inch.
No. 200 not less than 188 nor more than 200 per linear inch.
* "The classification of coarse materials according to size is very readily
accomplished by means of sieves." But with cement and other fine materials
a large proportion will pass the finest sieve; it is, therefore, desirable to
have some way of separating these very fine particles.
"It is well known that homogeneous substances fall in liquids with a
speed that varies with their size, that is to say, the larger fall more rapidly
than the smaller ones; and if a stream of liquid can be given a definite
upward flow, certain relatively coarse particles will settle out and other
relatively fine particles will be floated away."
Classifiers for laboratory use have been made for the separation of fine
particles, but the experiments so far take from two to four hours, and for
cement are otherwise not entirely satisfactory.
See article by G. W. Thompson, Proc. Am. Socy. for Testing Materials,
1910, vol. x, p. 601, also Taylor's " Practical Cement Testing, " p. 64.
FINENESS
II
Scales. The scales used in tests for fineness should be
sensitive to 5 centigrams. Figs. 3 and 4 show the two
types generally used. That
shown in Fig. 4 is designed
especially for fineness tests.
The beam is graduated so
as to represent percentages
of 50 grams.*
To Make the Test.
Weigh out 50 grams of the
FIG. 3.
thoroughly dried and
coarsely screened sample, and place in the No. 200 sieve
with about 200 grams of rather coarse shot. Then,
FIG. 4.
with pan and cover attached, hold all in the hands in a
slightly inclined position, and move backward and forward,
* The cuts for Figs. 3 and 4 were loaned by the E. H. Sargent Co., of
Chicago.
12 CEMENT TESTING
changing the plane of inclination, and allowing the sieve to
strike the palm of the hand a sharp blow, squarely on the
side, at the rate of about two hundred strokes a minute,
for ten minutes. Empty the cement that has passed the
sieve, clean the pan, and shake for one minute more.*
When the amount passing the sieve in one minute of con-
tinuous shaking is less than o.i per cent (0.05 gram), the
residue is passed through the No. 20 sieve, to separate it
from the shot, and is weighed. This weight in grams,
multiplied by 2, gives the per cent retained on the No. 200
sieve. Place the residue on the No. 100 sieve and con-
tinue the operation as above.
Results should be reported to o.i per cent on forms
similar to the one shown at the end of the chapter.
A convenient method of determining when less than o.i
per cent has passed a sieve is to weigh out 0.05 gram of
cement; form it into a compact heap and lay it aside for
reference. Then, by comparing the cement being tested
with this, it can be told at a glance if the shaking should
be continued.
The difference in color and structure between the several
residues should be observed and noted.
Deductions from Test. Specifications generally state
that for natural cement a residue of not more than 15 per
cent shall be left on the No. 100 sieve, nor 30 per cent on
* Should the residue after the one minute of continuous shaking be
greater than o.i per cent the operation must be continued till not more
than o.i percent remains on the sieve after one minute of continuous shaking.
FINENESS
the No. 200 sieve; and for Portland cement not more than
8 per cent on the No. 100, nor 25 per cent on the No. 200
sieve; but unless the cement acts badly in the other tests
it is not well to reject a cement, except when variation from
these requirements is great.
REFERENCES.
"Taylor's Practical Cement Testing," pp. 75-78; Johnson's
" Materials of Construction," Art. 310; "Standard Methods of
Testing and Specifications for Cement," Pars. 19-27.
FINENESS.
Apparatus
Condition of Sample
Brand
Ho.
Weight
of
A/G
Weight ^o fie-
Pefa'inecl hxineoi
JZefarxxf
tarmecf
Remarks
CHAPTER IV.
SPECIFIC GRAVITY.
Definition. The specific gravity of a substance is the
ratio of the weight of a given volume of that substance to
the weight of an equal volume of water. In the metric
system it is the ratio of the weight of the substance in
grams to its volume in cubic centimeters.
Significance. " The specific gravity of cement is lowered
by adulteration and hydration, but the adulteration must be
in considerable quantity to affect the results appreciably."
As the differences in specific gravity are usually very
small, every precaution must be taken to make the results
accurate. At the best, it is now believed, the test is of but
little value, as can be seen from the following, which are the
conclusions reached by R. K. Mead and Lester C. Hawk
after a series of experiments.*
" The specific gravity test is of no value whatever in
detecting underburning, as underburned cement will show
a specific gravity much higher than that set by the stand-
ard specifications. Underburned cement is readily and
promptly detected by the soundness tests, and no others
are needed for this purpose.
* Proceedings of the loth annual meeting of the Am. Socy. for Testing
Materials, vol. vii, p. 363.
14
SPECIFIC GRAVITY 15
" The value of the specific gravity test as an indication
of adulteration is much exaggerated. While a large admix-
ture of any light adulterant with the cement would be
shown, there is at the same time much slag and also
Rosendale cement which could be mixed with cement
in large quantities without lowering the specific
gravity below the limit of our standard specifications.
" Low specific gravity is usually caused by sea-
soning of the cement or clinker, either of which
improves the product.
"'The proposition to ignite the cement sample
which falls below specifications and determine the
specific gravity upon the ignited portions is of no
value because adulterated cements also have
their specific gravity very much raised by such
ignition."
Apparatus. Le Chatelier specific gravity flask,
glass funnel, ring stand, settling jar, glass rod
and pipette (Fig. 5), chemical balance (Fig. 20).
Various forms of specific gravity flasks have been
devised, most of them on the same principle;
but the one now used almost exclusively is the
Le Chatelier apparatus (Fig. 6).
This consists of a flask (a) of 120 c.c. capacity,
with a neck (6) about 9 mm. in diameter and 20 cm. long,
which has a bulb (c) at the middle, with graduation marks
immediately above and below; the volume between these
marks is 20 c.c. The neck, from the mark above the bulb
i6
CEMENT TESTING
for about 6 cm., is graduated into tenths of a cubic centi-
meter.
To Make the Test. Fill the Le Chatelier flask with
benzine (62° Baume naphtha) to the lowest mark, taking
care not to wet the side of the neck above the bulb. Let
this stand while 65 grams* of the cement to be tested is
weighed out on a chemical
balance. With a pipette,
adjust the lower meniscus
exactly to the mark under
the bulb taking care to avoid
parallax by sighting on a
distant horizontal line of
about the same level as the
eye. Support funnel (a) by
a ring stand (&), (Fig. 7),
allowing the stem to project
into the flask about one
inch. A pad of paper should
be placed under the flask
for protection from breaking.
Introduce the cement all at one time into the funnel,
holding a glass rod in the bottom to control the dis-
charge of the cement. By slightly raising and lowering
the glass rod, a small portion of the cement will pass through
* While the Standard Specifications give 64 grams the authors have been
in the habit of using 65 grams. Other cases are known in which the test is
made with 65 grams of Portland or 64 of natural cements.
Poet,
FIG. 7.
SPECIFIC GRAVITY 17
the funnel into the flask; and by slightly jarring the flask
on the paper pad, all of the cement may be made to pass
to the bottom of the flask with almost perfect elimination
of air, thereby displacing the benzine. See that all of the
cement enters the flask, by brushing scale pan, weighing
paper, rod and funnel. The funnel used in introducing
the cement must be perfectly dry; otherwise some of the
cement will be prevented from entering and the test will
be spoiled.
The displaced benzine rises to some division in the
graduated neck, as 0.8, shown by the line in Fig. 7; and
this plus 20 c.c. (the vol. of bulb), making 20.8 c.c., is the
volume of the 65 grams of cement; and
~ p _ weight of the cement _ 65 gms. _
displaced volume 20.8 c.c.
To prevent evaporation the flask should always be
grasped above the benzine. The room should be cool and
free from air currents. The flask may be immersed in
water to keep it at a constant temperature.
Cleaning the Flask. To empty the flask, shake it
vigorously to loosen the cement, then invert quickly over
a large jar and shake with a vertical motion. Add a small
amount of clear benzine and repeat the operation until all
the cement is removed.*
The benzine should be filtered and used again.
* A thorough cleaning of the lower bulb is not necessary between tests,
but the neck must always be kept clean.
l8 CEMENT TESTING
Conclusion. In order to draw conclusions from a specific
gravity test, the operator must be familiar with the specific
gravity of the brand of cement he is working with, as
different brands vary greatly. When a sample tests below
the known average of the brand it must be subjected to
further examination for adulterants, and an additional
specific gravity test should be made on an ignited sample,
to see that the low specific gravity is not due to excessive
seasoning.
The final rejection or acceptance must be based on the
results of the strength tests, modified by the specific gravity,
as the experience of the operator indicates.
REFERENCES.
Taylor's "Practical Cement Testing," pp. 46-51, 58-63; John-
son's, "Materials of Construction," Art. 311; "Standard Methods
of Testing and Specifications for Cement," Pars. 8-19.
SPECIFIC GRAVITY
SPECIFIC GRAVITY.
Apparatus
Condition of Sample
Brand
fa
Wefyhf
6>f
Sample
frtcre&fe
of
Vo/ume
$p*cffic
Gr&v/ty
Average
Remarks
CHAPTER V.
NORMAL CONSISTENCY, MIXING, TIME OF SET.
Significance. Different percentages of water used in
making the pastes,* for soundness tests, setting tests,
briquettes for strength tests, etc., cause the same sample
of cement to give widely varying results. Likewise, these
results are affected by a difference in the amount of working
that the pat receives. Therefore, it is necessary to fix some
standard by which the amount of water may always be
kept uniform, and the amount of working always the same.
Standard. The standard requires the use of such a
quantity of water as will, with a definite amount of working,
reduce the cement to a certain state of plasticity, called
normal consistency. The plasticity recommended by the
Standard Specifications is such that the plunger of a Vicat
apparatus will sink to a point in the mass 10 mm. below the
top of the ring.
Apparatus. Vicat apparatus, scales, glass plate and rub-
ber ring, burette (Fig. 8 or Fig. 36). The Vicat apparatus
is the one now used almost entirely. This consists of a
frame (k), (Fig. 9), in which a rod (/) moves. There are two
caps (a and d) which may be placed on the upper end of
* The term paste is used to designate a mixture of cement and water,
and the term mortar a mixture of cement, sand and water.
20
NORMAL CONSISTENCY, MIXING, TIME OF SET 21
the rod (/) and a needle (k) i mm. in diameter, or cylinder
(b) i cm. in diameter (0.39 in.), at the lower end and held
by a thumbscrew (g). The caps (d and a)
are of such weight that when used with
the needle or cylinder respectively, their
FIG.
FIG. 9.
weight together with the rod (/) is 300 grams. To the
rod (/), which can be held in any desired position by the
thumbscrew (/), is attached an indicator, which moves
over a scale (graduated to millimeters) attached to
the frame (k). The paste is placed in a rubber ring (i)
4 cm. high and 7 cm. in diameter at the base and slightly
tapering to the top, resting on a glass plate (/) about
10 cm. square.
Mixing. Weigh out 500 grams of cement and form it
into a crater about 4 inches in diameter (Fig. 10). For
first trial, into this crater pour, all at one time, a quantity
22 CEMENT TESTING
of water equal in amount to about 20 per cent of the weight
of the cement. With a trowel turn the cement from the
outside edges, into the water, a little at a time, till the
crater is filled and the water is absorbed. This should
take about a minute's time. Now turn this mixture over
two or three times with the trowel
to distribute equally the wet
cement, and form into a pile.
Knead the mixture vigorously for
1 1 minutes, much as dough is
kneaded for bread. The process is
best described as follows : Place the
hands, with the fingers and thumbs touching, over the top
of the pile, the wrists resting on the table. Then push
rapidly forward with a downward pressure of about 15
pounds and at the same time close the fingers in, so as to
squeeze the pile. Do this two or three times. Then turn
the pile at an angle of 90 degrees and continue the kneading.
At the end of a minute and a half, form the paste into a ball
and toss from one hand to the other six times, holding the
hands 6 inches apart.*
To Make the Test. Press the ball into the large end of
the rubber ring of the Vicat apparatus, smooth off and
place on a glass plate with the large end down. Smooth
the top with a trowel, using light pressure. Place the ring
under the Vicat plunger; set the plunger in contact with
* To secure uniformity of results, these directions must be followed to
the letter.
NORMAL CONSISTENCY, MIXING, TIME OF SET 23
the surface, read the scale and quickly release the
plunger.
Take the final reading on the scale when perceptible
motion has ceased. The paste is of normal consistency
when the plunger penetrates 10 mm. below the surface.
If the correct penetration is not obtained, discard the sample
and make another trial, using more or less water as re-
quired. Continue until the right percentage of water is
found. Record on blanks similar to the one shown at the
end of the chapter.
The Vicat apparatus must always be kept exceptionally
clean.
During all mixing operations the hands should be pro-
tected with rubber gloves.
TIME OF SET.
Significance. The time of set gives no indication of the
strength or soundness of a cement. But it is very important
to know the time of initial set (the time which elapses from
the moment water is added to the cement until the paste
ceases to be plastic, or when crystallization begins), and
final set (the time taken to become a hard mass).
Handling the cement after it commences to set, or after
the process of crystallization or hardening has begun, will
weaken it and cause it to disintegrate. It is, therefore,
very important to know how long a time may be allowed
in mixing and placing a batch of cement without injury to
24 CEMENT TESTING
it, and after it is placed how long it will take it to harden
so that the forms may be removed. It should harden as
quickly as possible after initial set. It usually takes con-
siderable time for mixing and placing concrete (the form
in which cement is most generally used) ; therefore, a cement
should have a slow " initial set " but reach " final set " soon
after.
These periods are arbitrarily measured by the penetration
of weighted wires of given diameter, as the needle of the
Vicat apparatus.
Things Affecting the Time of Set. Fineness, allowing
the water to reach the interior of the particles more easily,
increases the rapidity of setting.
Long standing cements absorb moisture from the air
and lose their hydraulic property.
The greater the amount of water used in mixing, the
slower will be the set.
Increased temperature of the mixing water hastens the
time of set.
To Make the Test. The Vicat apparatus with needle
is used. Mix 500 grams of cement to a paste of normal
consistency. Record the time of adding the water. Place
the paste in the Vicat ring as in normal consistency tests,
bring the Vicat needle into contact with the surface, and
release quickly. Find to what mark the needle should
descend to be 5 mm. from the bottom of the ring. Release
needle at intervals till set occurs.
Initial set is said to have occurred when the needle
NORMAL CONSISTENCY, MIXING, TIME OF SET 25
ceases to penetrate beyond a point 5 mm. from the bot-
tom, and final set when it makes no indentation.
Always see that the needle and apparatus are clean.
If Portland and natural cements are to be tested at the
same time, mix the Portland first, as it requires more time
to attain set. Test Portland cement for initial set after
15 minutes, and natural after 5 minutes.
The rings with the samples being tested should be stored
in a damp closet during the test.
Conclusions. Time of set being influenced by so many
conditions, tests made by the' same operator often do not
check closer than 10 per cent and by different operators
vary even more. Therefore, considerable allowance should
be made in judging a cement for time of set. It requires
from 20 to 30 minutes to mix and place a batch of concrete
in large work, but it also takes much longer to set than in
the tests; so that, in general, a cement need not be rejected
unless the mixing and placing on the work takes two or
three times as long as the test set.
REFERENCES.
Normal Consistency. Taylor's, "Practical Cement Testing,"
pp. 92 to 95, 120 to 126; Johnson's, "Materials of Construction," Arts.
316, 318; "Standard Methods of Testing and Specifications for
Cement," Pars. 27, 37, 52, 59.
Time of Set. Taylor's "Practical Cement Testing," pp. 80 to 83,
88 and 89; Johnson's, "Materials of Construction," Arts. 164, 312,
421; "Standard Methods of Testing and Specifications for Cement,"
Pars. 37 to 44.
26
CEMENT TESTING
NORMAL CONSISTENCY.
Temperature of
Temperature of
Humidity
Mixii
Room
ig Water
»-,
Mo.
'of
Per Cent
of
Water
*-»*
Remarks ..
NORMAL CONSISTENCY, MIXING, TIME OF SET 27
TIME OF SET.
Apparatus
Temperature of Room
Temperature of Mixing Water . .
Humidity
1
1
A
^^k
fcli
^t
Initia/ $*f
/V>7^/ ^/
355?
77>77<P
E/erpsea
77me
C/ock
Time
E/apseJ
Time
Remarks
CHAPTER VI.
CONSTANCY OF VOLUME.
Significance. A cement to be of value must be per-
fectly sound; that is, it must remain constant in volume
and not disintegrate or crumble. Although normal tests
give more reliable results, it usually takes considerable
time for the natural causes to take effect; and it is neces-
sary to know these effects at once. It has, therefore, be-
come necessary to develop, in some way, those qualities
which tend to destroy the strength and durability of a
cement.
Tests devised to do this are known as accelerated tests.
Failure is revealed by cracking, checking, swelling, or dis-
integrating, or by a combination of all of these phenomena.
Causes of Unsoundness. Excess of free or loosely com-
bined lime, which has not become sufficiently hydrated,
excess of magnesia and alkalies, and sometimes sulphides,
insufficient seasoning and coarse grinding are all causes of
unsoundness.*
Kinds of Tests. There are two classes of tests, viz.,
normal and accelerated, (i) Normal tests are made in
either air or water, kept at a constant temperature as near
* For a very complete treatise on soundness, see Taylor's " Practical
Cement Testing."
28
CONSTANCY OF VOLUME 2Q
70° as possible. (2) Accelerated tests are made in air,
steam or water at a temperature of 115° F. and higher.
Apparatus. Glass plate 4 ins. by 4 ins. by f in.; small
trowel (Fig. n), boiling apparatus (Fig. 32).
To Make the Tests. Weigh out 500 grams of cement,
and mix into a paste of nor-
mal consistency, from which
make four pats and one
ball.* FIG. ii.
The pats must be about 3 inches in diameter and from
| to | inch thick at the center, sloping to a very thin,
smooth edge at the circumference. In shaping these pats,
place on a glass plate about
4 inches square (using no
oil on glass) an amount of
cement which will almost
cover the plate and will
FIG. 12. i . , . , . n
measure ^ inch in thick-
ness at the center. Holding the plate in the left hand,
shape the cement into a cone with an altitude from f inch
to J inch and a base about 3 inches in diameter. Work
the cement to a thin, smooth and uniform surface by
troweling and turning the pat, the trowel being inclined
from handle to point at an angle (about 18°) which will
reduce the thickness of the cement from \ inch in the
center to a very thin edge at the circumference (Fig. 12).
To shape the ball, take enough of the paste to form a ball
* The ball test is no longer a standard test.
i
30 CEMENT TESTING
ij inches in diameter and shape by rolling in the hand, as
in making a snowball.
Date all specimens, and if different cements are being
tested give each pat and ball a distinguishing mark. Store
in a damp closet for 24 hours.
For the normal tests, one pat is placed in a water storage
tank for 28 days. The water must be maintained as near
70° F. as possible. A second pat must be placed in air
maintained at ordinary temperature and humidity. These
pats must be observed at intervals of 3, 7, 14, 21 and 28
days, and any changes in their condition should be noted on
suitable blanks, as shown at the end of the chapter.
For accelerated tests, place the two remaining pats on
the wire screen above the water of the boiling apparatus*
(Fig. 32), and the ball on the wire screen in the water.
Boil for five hours and examine for signs of failure, such as
cracking, discoloration, loosening from the plate, warping,
etc., and record condition. The water in the boiling ap-
paratus should be changed often.
Conclusions. To pass satisfactorily, pats should remain
hard and firm and show no signs of cracking, distortion or
disintegration.
Experience is necessary to judge correctly from the ap-
pearance of test specimens whether a cement be rejected
or not.f Shrinkage or expansion cracks, small radial
cracks at the edge or a short, circumferential split, must
* See description in Chapter X, p. 75.
f Taylor, pp. 178, 179, 182.
CONSTANCY OF VOLUME 31
not be confused and interpreted as disintegration. These
usually come from a too wet mixture or poor working.
Leaving the plate cannot be considered as dangerous,
unless curling, thickening at the center, or other distortion
is very marked. Cracking of the plate, which takes place
only in the case of water pats, does not indicate unsound-
ness. A blotched or discolored pat usually means an
adulterated or underburned cement and needs investigation
as to the cause.
Usually, if pats, either in the normal or accelerated tests,
show only slight signs of failure, it is well to hold the
cement for further tests and development of the present
one. The further tests should always be made in such a
case, as well as a continuation of the first one. Sometimes
a new cement which appears unsound in the first test will
show perfectly sound after aging a short time.
REFERENCES.
Taylor's, "Practical Cement Testing," pp. 156, 162, 166, 171;
Johnson's, "Materials of Construction," Arts. 313, 314; "Standard
Methods of Testing and Specifications of Cement," Pars. 69 to 76.
32
CEMENT TESTING
CONSTANCY OF VOLUME.
Percentage of Water used in Mixing
W
^^
Concf/tien of Pat
</•
Cement Brand
\
^
•S
*>
%
*
7
14
tl
28
Pat-$ /n water
7
14
71
28
Condition of Ball
Condition of Pat steamed 3 Hours
Conclusions
CHAPTER VII.
TENSILE STRENGTH.
Use. Cement is used in compression, but since there is
a certain fairly definite relation between its strength in
compression and tension, the accepted method for deter-
mining this strength is the use of a tensile test, which is the
test most easily performed. It is made by mixing the
cement into a paste, or the cement and sand into a mortar,
and molding into test specimens or briquettes, which are
allowed to set and are tested at the end of i, 7 and 28 days,
or, in some cases, at longer intervals. Strength tests of
mortar briquettes are of much greater importance than are
neat cement tests, as it is in the form of a mortar that
cement is used.
FACTORS AFFECTING STRENGTH.
Composition. Aluminates are presumably responsible
for the setting, and silicates for the final hardening; there-
fore, high aluminates will give a cement a higher early
strength and a lower ultimate, and vice versa.
Aging. Cement should not age longer than necessary
for manufacture, as this will lower the initial strength and,
if it is allowed to continue much longer, the ultimate
strength.
33
34
CEMENT TESTING
Fineness. Fineness will, in general, weaken neat cement,
but will strengthen sand mortar. This increase in strength
of sand mortar is due to the fact that fine cement more
thoroughly covers the sand grains, while in the neat the
weakening seems to be due to the fact that, in a coarse
briquette, the line of break passes around, rather than
through the grains, thereby increasing the breaking area.
Amount of Water. The amount of water used in mixing
and the method employed seem to affect the strength of
the cement greatly. (Chap. V.)
Apparatus. Briquette molds, either
single (Fig. 13) or gang (Fig. 14),
glass plate the size of the mold.
To Make the Test. (Neat
Cement.) Weigh out 800 grams of
cement (which will make 5 bri-
quettes), mix to normal consistency and fill the molds as
FIG. 13.
FIG. 14.
follows. (The molding of the briquettes is perhaps the
most important factor in cement testing.)
Place a well-oiled mold on an oiled glass plate,* sides
toward the operator, put enough cement to half fill the
molds into each opening, and press it lightly and evenly
* Plate should be of the same width as the outside of the molds and
enough longer tc rest on the cleats of the damp closet to be used.
TENSILE STRENGTH 35
into the bottom of the molds. Do this with the fingers
and thumbs, never with a tamper of any sort. Place
enough cement in and above the molds to more than fill
them; turn the molds 90° and begin at the end farthest
away to press, without ramming, the cement into the molds
with the thumbs, gripping the sides of the molds with the
fingers so as to exert a pressure of about 25 pounds. Press
each briquette in this manner three times, once at each
end and once in the middle. Turn the mold back to the
original position, add more material and smooth off with
a trowel, using about 5 pounds pressure. The smoothing
should be a cutting action, taking away the excess material
and yet filling in all the openings. With a few final strokes
of the trowel, make the surface perfectly smooth and press
the cement well up to the sides. Place a glass plate on top
and turn the mold over, and smooth the bottom in the same
manner as the top, by adding material and troweling. The
mold resting on the glass plate is now placed in a damp
closet for 24 hours, when the briquettes are removed from
the molds and stored on edge in water. They must remain
here until they are to be broken, which should be done
immediately after removal from the water.
Make enough briquettes so that five may be broken at
each period called for, usually i, 7 and 28 days, though
often the i-day tests are omitted.
36 CEMENT TESTING
MORTAR BRIQUETTES.
To Make the Test. Weigh out materials as follows:*
For Portland cement, i to 3 mortar, cement 250 grams,
sand 750 grams.
For natural cement, i to 2 mortar, cement 300 grams,
sand 600 grams.
Determine the percentage of water by Taylor's formula,
as follows :
4 (n + i)
where
X = per cent of water for the sand mixture;
N = per cent of water for the neat cement ;
n = parts of sand to one of cement by weight;
S = a constant depending on the character of the
sand and consistency desired. (For Ottawa sand,
S = 25; for bar sand, 5 = 27 to 33; usually
use 33.)
The method of mixing and filling the molds is the same
as for the neat briquettes, except that the amount of water
is determined as above, and the cement and sand are
mixed dry to a uniform color before forming into a crater.
Make six briquettes of each cement, three to be tested
at each period of 7 and 28 days. Briquettes should be
stored in water in a damp closet (the same as the neat),
after being marked with the necessary information as to
brand, proportions of sand, etc.
* This amount should be sufficient to fill 4 3-gang molds.
TENSILE STRENGTH
37
BREAKING.
Test pieces must be broken as soon as they are taken
from the water. Any standard machine (Figs. 21-25)
may be used, but it should be supplied with the solid metal
clips (Fig. 15), as they are the ones recommended by the
Standard Specifications. Clips should be
used without cushioning the points of
contact. Great care must be observed
to center the briquettes in the clips and
to see that they are free from sand, in
order to avoid cross-strains, which cause
clip breaks. Apply the load slowly, as
a suddenly applied load may produce
vibration or shock, which will cause the
briquette to break before the ultimate
strength is reached. The Standard Spec-
ifications recommend that the rate of
application of pressure be 600 pounds per minute. The
average value of the briquettes of one sample broken
should be taken, with high or low results excluded.
Conclusions. A cement, to be acceptable, should fulfil
the following conditions in the tension test: " (i) Both neat
and sand briquettes shall pass a minimum specified amount
at 7 and 28 days. (2) That the neat value at 7 days shall
not be excessive. (3) There shall be no falling off between
7 and 28 days in neat test. (4) Sand tests must show an
increase of at least 10 to 15 per cent. (5) Sand tests are
the true tests of the strength. A cement failing in sand
FIG. 15.
38 CEMENT TESTING
tests should be rejected even if it passes the neat test.
When the reverse is true, i.e., when it passes the sand test
and fails in the neat, cement may be accepted if no signs of
unsoundness have developed."
The following rules, given by Taylor in " Practical Cement
Testing," should be followed.
" At 7 days: Reject on a decidedly low sand strength.
Hold for 28 days on low or excessively high neat strength,
or a sand strength barely failing to pass requirements.
"At 28 days: Reject on failure in either neat or sand
strength. Reject on retrogression in sand strength, even
if passing the 28-day requirements. Reject on retrogres-
sion in neat strength, if there is any indication of poor
quality, or if the 7-day test is low; otherwise accept.
" Accept if failing slightly in either neat or sand at 7
days and passing at 28 days."
REFERENCES.
For Neat. Taylor's "Practical Cement Testing," pp. 120-125;
Johnson's, "Materials of Construction," Arts. 315, 316, 319, 320,
323, 324 and 325; "Standard Methods of Testing and Specifications
for Cement," Pars. 59-69.
For Mortar. Taylor's "Practical Cement Testing," pp. 108, 114,
120-125; Johnson's "Materials of Construction," Arts. 317-319,
406-411; Taylor and Thompson's "Concrete: Plain and Rein-
forced," pp. 132, 133; "Standard Methods of Testing and Specifica-
tions for Cement," Pars. 35-36.
TENSILE STRENGTH
39
TENSILE STRENGTH.
(Neat Cement.)
Machine used for Breaking
Per cent of Water used in Mixing..
Aye
Brarnaf Afo.
£5r&r?af f\fo.
7er75//e
$fre/7q/h
Pev/artier?
from Mearr?
7ef?s//e
$trer?gJJ?
Pe war tier?
frem Macrr?
Rrunds
Per- Cent
founds
frr&nf
7
Pays
Mean
Remarks
CEMENT TESTING
TENSILE STRENGTH.
(Mortar.)
Machine used for Breaking...
Brarnef
.*
Cement
*
ll
^
**
a*
ll
75/75/%P
Zfrengfh
Deviation from Mean.
Pounds
Per Cent
Pays
28
Pays
P0r/£
?8
Pays
Pay*
~z.e
Pt*y*^
/
/
Remarks
CHAPTER VIII.
COMPRESSIVE STRENGTH AND TRANSVERSE TESTS.
Compressive Strength. In the United States, compres-
sion tests are not used as standard tests for the reception
of a cement, but where a concrete is required to be tested,
or where a comparison test of different sands and stones
that are to be used in concrete is to be made, the com-
pression test is necessary as the size of the aggregate
requires the use of larger specimens than the regular bri-
quettes of the tension tests.
The form and size of the specimen most generally used
are two-inch cubes for mortar and six-inch cubes for con-
crete. Cylinders six inches in diameter and ten inches to
twelve inches deep are preferable for concrete because the
ease of rilling and packing them makes the specimens of
this size more uniform.
In order that there may be proper contact between the
testing machine and the specimen, the bearing surfaces of
the specimen should be smoothed to true planes, and to
correct any slight angle between the bearing surfaces, one
surface should rest on a plate having a ball and socket
joint.
Blotting paper or plaster of Paris should be placed be-
tween the block and the machine to counteract the irregu-
41
42 CEMENT TESTING
larities in the specimen; this will, however, slightly lower
the strength.
Molds. Four gang 2-inch cube molds (Fig. 16) are gen-
erally used, but the size depends to some extent on the
capacity of the machines obtainable for breaking the
specimens.
To Make the Test. Oil the molds and glass plate thor-
oughly before mixing.
Neat. Weigh out 900 grams of cement (if 2-inch cubes
are to be used) and mix by standard methods, as given
FIG. 16.
under Normal Consistency. Fill the molds in a manner
similar to that described for briquettes, mark and place in
the damp closet for 24 hours. Remove the cubes from the
molds and place in water. Do not take from the water until
ready to break. Test the cubes at the end of 7 and 28 days.
Mortar. Weigh out 400 grams of cement and 1 200 grams
of sand for 1:3 mortar, or 550 grams of cement and
1 1 oo grams of sand for i : 2 mortar.
Determine the amount of water to use and fill the molds,
following directions given for mortar briquettes. Place in
a damp closet, remove from the molds, store and break,
using directions given under Neat.
COMPRESSIVE STRENGTH AND TRANSVERSE TESTS 43
Breaking. Use an ordinary universal testing machine
(Fig. 29) of 30,000 capacity (for 2-inch cubes), with com-
pression tool in the moving head. Place the cube exactly
in the center of the machine. (This can be done by means
of the circles cut in the table of the machine.) Run the
head down until nearly in contact with the cube, with
medium speed; change to the slowest speed and apply
load, keeping the beam balanced until the cube yields under
the load.
Conclusion. The results of compressive tests are to be
interpreted in accordance with the same general rules as for
tension tests. There is a ratio between compression and ten-
sile strength, which varies from 5 to 10 for average results.*
TRANSVERSE TESTS.
(Modulus of Rupture.)
Molds. The molds for this test are usually i-in. by i-in.
by i3-in. beam molds, though sometimes i^-in. by ij-in. by
i3-in. or 2-in. by 2-in. by i3~in. molds are used; 6 beams
will give a very good average result. Fig. 17 shows a gang
mold.
To Make the Tests. Oil the molds and the glass platef
thoroughly. Weigh out 1000 grams of cement; mix and
fill the molds in the same manner as for briquettes or cubes.
When using gang molds do not try to turn the molds over,
* See discussion in "Materials of Construction " by J. B. Johnson, and
Practical Cement Testing, p. 215.
t If glass plate large enough for gang mold is wanting, a water-soaked
asbestos board may be used.
44 CEMENT TESTING
but use extra precautions to see that the cement fills the
bottom of the molds. Place in damp closet for 24 hours;
remove from the molds and place in storage water for 7
days, and then break.
FIG. 17.
Breaking. Beams should be broken on the long lever
testing machine with special attachment (see description
on p. 70), using, if possible, a 1 2-inch span. Should any
beams be broken in handling before being tested, they may
be broken at shorter spans. Reports of this test should
include the calculations.
Calculations. The modulus of rupture is calculated by
the formula
i • W L
R = ° — ^77;' which for i-inch square specimens becomes
R=$W.L,m which
2
W = the center load in pounds,
L = the length of span in inches,
B = width of the specimen,
H = the depth.
COMPRESSIVE STRENGTH AND TRANSVERSE TESTS 45
Illustration. Suppose a beam i in. by i in. on a 1 2-inch
span breaks with a center load of 50 pounds; then
R = $W.L = - X 50 X 12 = 900 inch-pounds.
2 2
Another beam 2 ins. by 2 ins. on a 1 2-inch span breaks with
400 pounds, center load.
3 -W.L 3 X 400 X 12
R = — : = — — = ooo inch-pounds.
2-B.H2 2X2X4
Conclusion. There is a ratio* between transverse
strength and tensile strength varying between 1.3 and 2.5.
By assuming an average of 1.5 and multiplying the modulus
of rupture by this average, an approximate estimate of the
tensile strength may be obtained. However, this is rather
unsatisfactory, since transverse specimens are subject to so
many variations. A cement should never be condemned by
a transverse test alone, unless a series of tests shows a very
low value.
REFERENCES.
Compression Tests (Neat). Taylor's "Practical Cement Testing,'*
pp. 212-216; Johnson's "Materials of Construction," Arts. 280, 315,
326. (Mortar) Taylor, pp. 212-216; Taylor and Thompson's "Con-
crete: Plain and Reinforced," p. 136; Sabin's "Cement and Con-
crete," Art. 52.
Modulus of Rupture. Taylor's " Practical Cement Testing,"
pp. 216, 217, 231-234.
* The student should compare tension and transverse tests and ascertain
the ratio.
CEMENT TESTING
COMPRESSIVE STRENGTH.
(Neat Cement.)
Machine used for Crushing.
Per Cent of Water used in Mixing
!
1
<b <b
^ N
^ ^
U/t/mc*fe
Load
\ ^
^ ^
H
v2 ^
Peviaf/en from
Mean 5frenqttt
R>unci$
<rf&
1
K
Mean
1
JO
«^J
Mean
Remarks . . .
COMPRESSIVE STRENGTH AND TRANSVERSE TESTS 47
COMPRESSIVE STRENGTH.
(Mortar.)
Machine used in Crushing.
Cement
Bran
11
28
Peviath'orr
from Mecrrr
fhs.
Remarks
CEMENT TESTING
MODULUS or RUPTURE.
(Neat.)
Brand of Cement
Per Cent of Water used in Mixing. .
Machine used in Breaking
Section
of
Be&rr?
Spar?
Central
Load
Modulus of Rupture
Ibs. per 5a. inch.
Mean
-
Remarks
CHAPTER IX.
SAND AND STONE.
_ .aa**""'"'
SAND.
THE variation in the strength of mortars, due to different
kinds of sand, is so great that to obtain uniformity of tests
in different laboratories and by different workers in cement,
it was necessary to adopt a standard sand. There are two
in use: one, a standard quartz, open to objection on
account of its high per cent of voids, the difficulty of com-
pacting in the molds, and lack of uniformity; the other, a
natural sand from Ottawa, Illinois, screened to pass a sieve
20 meshes per linear inch, and retained on a sieve having
30 meshes per linear inch. The Ottawa sand is recom-
mended by the committee on Standard Specifications, and
should be the one used.
Test of Natural Sand. When a natural sand is to be
used for tests or work, it becomes necessary to determine
the percentage of voids, the uniformity coefficient and the
effective size, in order to properly proportion the sand and
cement. It is also well to know the amount of foreign
matter, as loam, clay and organic substances, to determine
its effect on the strength.
Per Cent of Loam. (Apparatus: Scales, settling jar,
glass stirring rod, evaporating dish, ring stand or tripod,
49
50 CEMENT TESTING
Bunsen burner). Weigh the sand very carefully and place
it in a settling jar. Add about 250 c.c. of water and stir
vigorously with a glass rod, allow fifteen
seconds for settling and decant the water,,
taking care that none of the sediment at
the bottom escapes. Repeat the opera-
tion until the water remains clear after
%to r--«ay fifteen seconds of stirring; wash the en-
e^f tire contents of the jar into a shallow pan
or evaporating dish; drain off the water,
J X^S^ place the pan and contents on a ring
FlG i8 stand over a Bunsen burner (Fig. 18),
and thoroughly dry. When cool, weigh
and determine the per cent of loam. The loss in weight is
the weight of the loam.
MECHANICAL ANALYSIS.
The mechanical analysis of a sand or a stone consists in
determining the fineness (by passing through various
sieves), the uniformity coefficient and the effective size.
Apparatus. Sieves 7 inches in diameter, numbers 200,
150, 100, 70, 60, 50, 40, 30, 20, 10, with pan and cover;
scales and mechanical shaker. (See p. 74.)
To Make the Test. Weigh out 100 grams of sand, ar-
range nest of sieves with largest on top, if a mechanical
shaker is to be used; if the shaking is to be done by hand,
only two or three sieves can be used at a time.
Put the 100 grams of sand in the top sieve, cover and
SAND AND STONE
tighten the sieves in the machine and run it for 5 minutes.
A like, time of shaking is required for each set of sieves taken
Percent Passing Sieves.
200
-100
-40
-10
FIG. 19.
at a time, when shaken by hand. Weigh the amounts
retained on each sieve and caught in the pan. Record in
blanks similar to the one shown, and plot curve (Fig. 19),
52 CEMENT TESTING
showing size of sieves as abscissas and the per cent passing
sieves as ordinates. From the curves, determine the effective
size and uniformity coefficient.
The uniformity coefficient is the ratio of the diameter of
the particles represented at the point where the curve
crosses the 60 per cent line, to the diameter of the parti-
cles represented at the point where the curve crosses the
10 per cent line.*
The effective size is the size of the particles at the 10 per
cent point on the curve.
To Find the Uniformity Coefficient. Project down from
the point a on the curve (Fig. 19), where the 60 per cent line
intersects the curve, to the point b on the scale of sand
diameters, and likewise from point c to d. Divide the
reading at b by that at d and the result is the uniformity
coefficient, or 0.032 4- 0.006 = 5.25.
The effective size is the reading at the point d. f
Voids are the spaces between the grains of sand or pieces
of crushed stone.
Apparatus. Le Chatelier flask, funnel, glass rod, pipette,
wooden rammer and small settling jar.
To Make the Test. Weigh out 55 grams of the sand and
determine its specific gravity as directed in Chapter IV,
substituting water for the benzine in the Le Chatelier flask.
Determine the weight of sand per unit of volume (i c.c.)
* Sand having a coefficient over 4.5 is a good coarse sand. The larger
the value, the better the sand.
f The effective size is but little used in concrete.
SAND AND STONE 53
by filling a jar of known capacity* (about i liter, 1000 c.c.)
with thoroughly dry sand. Fill the jar by introducing a
layer of sand i inch thick and compacting it with a wooden
rammer, add another layer and tamp, and so on, till the
jar is level full. Get the net weight of the sand; i.e., weigh
the jar and sand, subtract the weight of the jar, and com-
pute the weight of i c.c. The weight of sand in grams
divided by the volume in cubic centimeters will give the
weight of sand per cubic centimeter.
Example:
Weight of jar and sand 2650 gms.
Weight of jar 980 gms.
Weight of sand (1000 c.c.) 1670 gms.
Weight of i c.c. = 1.67 gms.
With the weight of i c.c. and the specific gravity, com-
pute the per cent of voids as follows: Divide the weight
of sand per cubic centimeter by the specific gravity and
multiply by 100. This product subtracted from 100 gives
the per cent of voids, or
weight of sand per c.c. , .,
100 .,. — X ioo = per cent of voids
specific gravity
Example:
Weight of sand per c.c. = 1.67
Specific gravity =2.7
1.67 X ioo £ .j
ioo — = 38 = per cent of voids.
* The capacity can be obtained by filling the jar with a measured amount
of water or by filling with water and getting the weight of the water in
grams, when each gram will equal a cubic centimeter of volume.
54 CEMENT TESTING
Weight per Cubic Foot. With the per cent of voids just
obtained and the specific gravity, the weight per cubic foot
can be computed, as follows: Multiply the weight of a
cubic foot of water (62.35 Iks.) by the specific gravity, and
this product by 100 minus the per cent of voids. The result
is the weight per cubic foot, or
62.35 Ibs. (wt. of cu. ft. of water) X sp. gr.
X (100 — per cent of voids) = wt. per cu. ft.
Example:
62.35 Ibs. X 2.70 X (100 — 38) = 104.16 Ibs.
STONE.
Mechanical Analysis.
Apparatus. Sieves with pan and cover (same as those
used for sand); also, 7 -inch sieves with o.i 5-inch, o.2o-inch
and o.3o-inch openings, and 1 2-inch sieves with o.45-inch,
o.67-inch and i.oo-inch openings. A mechanical sifter will
greatly lessen the work of the test.
To Make the Test. Weigh out 10 pounds of crushed
stone, and place it on the i.oo-inch sieve; shake over a sheet
of paper till none will pass; weigh that retained on the
sieve; put that caught by the paper in the o. 67-inch sieve,
shake and weigh as before; repeat with the 0.45-01 ch
sieve. Arrange the sieves used in the sand tests, together
with the o.3o-inch, o.2o-inch and o.i 5-inch in order of
their size, the largest on top, in the mechanical shaker,
and place the shakings from the o. 45-inch sieve in the
top one. Shake for five minutes and find the weight
SAND AND STONE
55
retained on each sieve and caught in the pan. Plot curve
for the stone, using the same method as for sand, and deter-
mine the uniformity coefficient and efficient size.
VOIDS.
First Method.
Apparatus. Chemical balance with specific gravity
bench, small beaker, cubic foot measure and platform
scales.
Specific Gravity. Determine the specific gravity by the
loss of weight in water method; that is, weigh on the chemi-
FIG. 20.
cal balance (Fig. 20), a piece of the stone, first in air, and
then suspended in water. The specific gravity will be the
result obtained by dividing the weight in air by the loss of
weight in water, or
weight in air
bp. gr.
loss of weight in water
56 CEMENT TESTING
To Make the Test. Determine the weight in air in the
ordinary manner. To get the weight in water, tie a very
fine thread around the stone, arrange the balance bench and
beaker as shown in Fig. 20, see that the stirrup and pan are
free from the bench, and have the beaker about three-
quarters full of water. Tie the free end of the thread to
the stirrup hook — so that when balanced the stone will
hang about the middle of the water, and will not touch the
sides of the beaker — and weigh. Subtract this weight from
the first, which will give the loss of weight in water. Divide
the first weight by this loss of weight in water and the
result will be the specific gravity.
Example:
Weight in air 25.02 gms.
Weight in water 15-76 gms.
Loss of weight in water 9.26 gms.
Sp.gr. =^f = 2.7
9.20
Weight of the Stone per Cubic Foot. Use the cubic foot
measure. First get its weight empty. Then fill it with
the stone, add a layer of about 3 or 4 inches at a time, tamp
each layer well with a light wooden rammer and weigh.
Subtract weight of the measure and get the net weight of
the stone.
Example:
Weight of measure and stone 104 Ibs.
Weight of measure ••.;. 6 Ibs.
Net weight of stone 98 Ibs.
With this net weight and the specific gravity found
above, calculate the per cent of voids. The per cent of
SAND AND STONE 57
solid content is the weight of stone in pounds (i cu. ft.) in
the measure, multiplied by 100 and divided by the product
of the weight of a cubic foot of water (62.35 Ibs.) and the
specific gravity of the stone. This subtracted from 100
gives the per cent of voids, or
wt. of stone (in measure) in Ibs.
_
sp. gr. (of stone) X 62.35 (wt. of cu. ft. of water)
X ioo = per cent voids.
Example:
Weight of cu. ft. of stone 98 Ibs.
Sp. gr. of stone 2.7
08 X ioo , . ,
ioo — -r* = 42 = per cent of voids.
62.35X2.7
Second Method.
This method is more adapted to use in the field and is
probably more accurate than the method just described.
Apparatus. Platform scales, gallon jar or 8- to 10-
quart pail.
To Make the Test. Weigh the pail (which must be per-
fectly dry and clean), fill the pail brim full of water and
weigh again. Get the net weight of the water and calcu-
late the volume of the pail. (Weight of water in pounds
X 0.01602 = volume in cubic feet). Empty out the
water, dry the pail and fill it level full with the stone to be
tested, having it well tamped. Get the net weight of the
stone. Without changing the stone in any manner, pour
into the pail of stone as much water as it will hold (pour
slowly to allow the air to escape) and get weight of the
58 CEMENT TESTING
water added and its volume. The percentage of this last
volume of water to the first will be the percentage of voids
in the stone. Calculate the weight of a cubic foot of the
stone from the weight and volume found in the first weigh-
ings. The specific gravity can be found by substituting
these values in the following equation:
wt. of cu. ft. of stone (solid)
wt. of cu. ft. of water
or
wt. of cu. ft. (crushed stone in Ibs.)
x
100 — per cent voids (solid content)
-s- 62.35 Ibs. (wt. of cu. ft. of water) = specific gravity.
Example: Pounds.
Weight of pail and water ...................... 34. 50
Weight of pail ................................ 4.5
Weight of water .............................. 30.00
Weight of pail and stone ....................... 47.5
Weight of pail ................................ 4.5
Weight of stone .............................. 43.00
Weight of pail, stone and water ................. 61.00
Weight of pail and stone ...................... 47-5°
Weight of water in the voids ................... 13.50
Volume of the pail = 30 X 0.01602 = 0.4806 cu. ft.
Volume of the voids = 13.5 X 0.01602 = 0.216 cu. ft.
Per cent of voids = 0.216 X IOO-T- 0.481 = 44.9.
Weight of a cubic foot of the crushed stone = 43 Ibs. -5- 0.481
cu. ft. = 89.4 Ibs. per cu. ft.
Specific gravity is
89.4 X IPO _ 8Q4Q
62.35 X (100 - 44-9) 3435485
SAND AND STONE
59
REFERENCES.
Per cent of Loam, Taylor's "Practical Cement Testing," p. 223;
Baker's " Masonry Construction," Art. 114^; Taylor and Thompson's
"Cement: Plain and Reinforced," p. 154; Mechanical Analysis, Tay-
lor's "Practical Cement Testing," p. 223; Taylor and Thompson's
" Concrete: Plain and Reinforced, "pp. 187-194; Turneaure and Rus-
sell's "Public Water Supply," Art. 511; Voids in Sand and Stone,
Taylor's "Practical Cement Testing," pp. 224, 225; Baker's "Ma-
sonry Construction," Arts. 114 /, 115 d; Taylor and Thompson's
" Concrete: Plain and Reinforced," p. 210.
PERCENTAGE OF LOAM.
(Sand.)
Kin J of
5&f70f
We/ghfof
5a/77p/e
We/ghfof
Pry&s/tf.
We/ghf
ofLcar/r?
Per Cent
ofLo&m
Ms cm.
Remarks
Example:
Weight of sand before washing
Weight of sand after washing . .
Loss
Hence per cent of loam = 2.
50 gms.
49 gms.
i gm.
6o
CEMENT TESTING
MECHANICAL ANALYSIS.
i*
vS*
Pi am of
Openings
in /nches
5arnaf:
5 fane:
Weight
Retained
Per Cent
Retained
Weight
Refa/ned
ftrCent
Refainea/
Passed ZOO
Tofa/
Loss
SAND:
Effective Size
Uniformity Coefficient.
STONE :
Effective Size
Uniformity Coefficient.
SAND AND STONE
6l
WEIGHT OF SAND PER CUBIC FOOT.
Capacity
of
Jar
Wf.of
Conc/ft/or?
of
5cmd
Wtper
Cu.Cm.
Jar
/
Jar +
50rnaf
5ar?d
SPECIFIC GRAVITY OF SAND.
A7/?y of
Wf. of
ment.
Av Specific
Gr&v/fy
SPECIFIC GRAVITY OF STONE.
Weight of 5 tone
P/sp/ace-
menf'.
5pec/f/c
Gr&vrfy
Av5pec/ffc
Orarvtfy
Ir? Air
/n Wafer
62
CEMENT TESTING
WEIGHT OF CRUSHED STONE PER CUBIC FOOT.
m of
Condition
of
5tone
m
perCu.fi
Measure
Measure
+ 5for?e
5tone
CHAPTER X.
LABORATORY EQUIPMENT FOR PHYSICAL TESTS.
THE special pieces of apparatus for the different tests
have been described under the various tests in which they
were used. In this chapter, brief mention will be made of
the laboratory equipment now in general use.
MACHINES AND ACCESSORIES.
Tension Tests. There are three types of machines used
in the United States for briquette breaking (tension tests) ;
namely, long lever, shot and spring balance.
The long lever machine shown by Figs. 21 and 22 is the
most accurate, and has the advantage of being adapted to
transverse and small cube tests.
The Olsen (Fig. 21) and Riehle (Fig. 22) are the two
makes generally used. The poise on these machines is
moved out, either by power or by hand, and can be regu-
lated to travel at different rates of speed. The load is
applied by turning a large hand wheel in the center of the
machine, which operates a lever, — thereby putting tension
on the briquette.
The shot machines (Fig. 23-25) are compact and speedy,
and operate without constant attention. The Fairbanks
63
64
CEMENT TESTING
(Fig. 23), Riehle (Fig. 24) and Olsen (Falkenau-Sinclair)
(Fig. 25) are the representative machines of this type.
A description of the operation of the Fairbanks machine
FIG. 21
is as follows: Place a briquette in the clips (N)(N) (Fig. 23)
and tighten up the hand wheel (P) till the beam is raised
to (K), open the shot outlet (7); the weight of the shot in
the pail (F) will put tension on the briquette through the
LABORATORY EQUIPMENT FOR PHYSICAL TESTS 65
lever system, till it breaks. The flow of the shot is auto-
matically stopped by the dropping of the beam when the
FIG. 22.
briquette breaks. The pail and shot are now hung on (E),
poise (G) is placed on the beam where the pail was, and the
breaking load is read as in an ordinary weighing operation.
66
CEMENT TESTING
The Riehle (Fig. 24) is slightly different. A weight on
one end of a lever is counterbalanced by shot; as this shot
is allowed to pass out, the weight is allowed to descend,
thereby putting tension on the specimen. When the
specimen breaks, the flow of shot is automatically stopped.
The shot is weighed on a spring balance so calibrated as to
FIG. 23.
read the breaking load directly. These machines can only
be used in tension.
The operation of the Falkenau-Sinclair or Olsen shot
machine (Fig. 25) is as follows, as described in the catalog
of Tinius Olsen & Co. : " Referring to the cut, it will be seen
that the machine consists, as usual, of a mechanism for ap-
plying the load on the test briquette, and means for weighing
LABORATORY EQUIPMENT FOR PHYSICAL TESTS 67
this load. The load is applied through a system of levers by
means of the weight shown on the extreme right. Before
J
FIG. 24.
starting a test this weight on the right is counterbalanced
by shot held in the kettle on the left end of the same beam.
To make the test the valve in the bottom of this kettle is
68
CEMENT TESTING
opened, and as the shot escapes its equivalent of the weight
on the right-hand end of the beam acts on the briquette.
At the instant the briquette breaks the escaping stream of
FIG. 25.
shot is cut off by the closing of the valve in the bottom of
the kettle. This is effected by the upper grip striking the
horizontal arm which extends just above it, and thus
LABORATORY EQUIPMENT FOR PHYSICAL TESTS 69
releasing the curved arm carried on the spindle immedi-
ately to the left, this curved arm in turn striking the valve
and closing it. The briquette having broken, and the
stream of shot having been cut off, it only remains to weigh
the amount of shot that has escaped from the pan and
multiply it by the proper factor to give the load per square
inch to which the briquette has been subjected.
''' This shot might be weighed on any scale desired, but for
facility in making tests, the machine is furnished with a
spring balance on which is placed the pan into which the
shot falls. The dial of this spring balance is graduated, so
as to read in terms of pounds to the square inch on the
specimen. It follows that, as the test proceeds, the opera-
tor can watch the application of the load, and knows at any
instant exactly what the load is on the briquette. When the
briquette breaks, the load which broke it is read at a glance
and jotted down without further manipulation or calcula-
tion. The shot is then poured back into the kettle and
the machine is ready for the next test.
"The small hand wheel for adjusting the lower grip is
arranged so that it will automatically slip on the adjusting
screw as soon as a predetermined load has been applied to
the briquette. This hand wheel having been properly
adjusted, there can be no strain on the briquette by pulling
too hard on the hand wheel."
The crank at the base is for taking up the motion of the
lever system as the strain increases.
The spring balance machines (Fig. 26) are compact and
CEMENT TESTING
cheap, but are neither accurate nor speedy, and are suitable
only for field tests or where
only occasional tests are made.
Clips. There are several
forms of clips on the market,
but the one recommended by
the committee on standard
specifications is to be desired.
Its construction may be seen
from Fig. 15.
Transverse test attachment
(Fig. 27) consists of a bar (a)
about 13 inches long, with link
(b) attached at the center so
that it can be suspended from
the beam of the machine in
place of the upper tension
clip. V's are cut in bar (a)
2, 3, 4, 5 and 6 inches distant
from the center on each side, and in these the stirrups (c)
are placed, according to the span of the test specimen.
The test specimen (d) is placed on stirrups (c-c) and a
third stirrup (e), which is attached to the hand wheel
lever in place of the lower tension clip applies the load
at the center of the specimen. (Points / are blunt knife
edges) .
Compression Tool. This attachment consists of four
plates about 3! inches square. The plates (a) and (d) (Fig.
FIG. 26.
LABORATORY EQUIPMENT FOR PHYSICAL TESTS 71
FIG. 27.
FIG. 28.
FIG. 29.
72 CEMENT TESTING
28) have ears in the center, by which they are attached to
the machine, in place of the tension clips. Plate (c) is con-
nected to (a), and (b) to (d), by four bolts, in such a way
that when (a) and (d) move apart, (b) and (c) will move
towards each other and compress the cube between them.
Universal Testing Machine. The universal machine
(Fig. 29) is better adapted for compression tests than the
long lever machines and has the further advantage of very
wide range in the size of blocks.
Figure 30 shows the Olsen Hydraulic Compression
Machine. This machine is a small hydraulic press, having
an adjustable head above, which can be lowered or raised
to the desired position by means of a hand wheel and screw.
The cylinder is placed below and pressure is applied to the
ram in a peculiar manner. Instead of the usual pump, a
small plunger is forced into the cylinder by means of a
worm drive shown at the right-hand side. The motion of
the ram is limited, as the plunger is of small diameter, but
in testing incompressible material, like cement, a short
stroke is all that is required. The worm can be slipped out
of mesh with the worm wheel, and the plunger can be
quickly moved in either direction by means of the hand
wheel. The table is on a spherical bearing, which accom-
modates itself to the specimen so as to bring a uniform
pressure. The load is read directly by a hydraulic gage
connected with the cylinder through a safety valve, which
prevents injury to the gage by sudden shock due to failure.
The capacity of the machine is 200,000 pounds. The diam-
LABORATORY EQUIPMENT FOR PHYSICAL TESTS 73
FIG. 30.
74 CEMENT TESTING
eter of the head and table is 6 inches, while the extreme
distance between the head and table is 6j inches.
Sand Sifter. The sifter shown in Fig. 31 is a very close
attempt at producing the desired motion for sifting by
giving the sieves a circular motion and also a jar. It
FIG. 31.
consists of bevel gears driven by a hand wheel, which
imparts a circular and an up and down motion to two up-
right rods, between which the sieves are securely held.
These rods extend downward so that on the down motion
they strike the bottom plate of the machine a sharp blow.
LABORATORY EQUIPMENT FOR PHYSICAL TESTS 75
A very good homemade mechanical sifter can be made when
occasion demands. A simple one is shown in " Practical
Cement Testing," page 73.
Scales and Balance. The laboratory must have a chemi-
cal balance (Fig. 20). It need not be an expensive make.
A small balance sensible to 5 centigrams (Fig. 3) is used
for the general weighing, and ordinary platform scales will
be needed for test of concrete.
FIG. 32.
Boiling Test Apparatus. This apparatus can be as
simple or as elaborate as desired. It need consist only of a
copper vessel, with a cover in which there is a small outlet
for excess steam and two wire
netting shelves, one near the
bottom, the other above the
water line. It is an advantage
to have an opening near the
bottom, for a connection to a
constant level bottle. The
vessel should have legs, or be FIG. 33.
76
CEMENT TESTING
placed on a tripod, so that a Bunsen burner can be placed
underneath for heating. Fig. 32 shows a very good design.
Fig. 33 shows a constant level bottle.
Moist Closet. The moist closet (Fig. 34) is best made of
cement, slate or similar material, and may be any size
desired. It should be long enough to take in the longest
size of gang molds used. The ends should have cleats so
arranged that glass strips with molds on them can be slipped
in, with enough room between tiers for free circulation of
FIG. 34.
air. A pan for holding water should be placed in the
bottom. A most excellent closet made of waste cement is
described by E. B. McCready, vol. vii, p. 598, Proc. of
Am. Socy. for Testing Materials. Ordinary tin boxes are
sometimes used for damp closets. A temporary damp
closet can be made by bending a wire screen to form a roof
over the specimens, over which a wet cloth is placed.
There should be some means of keeping the cloth uniformly
damp, as letting the ends dip into a pan of water.
Storage Tanks. Any tank that will hold water and has
capacity enough can be used for a storage tank. Fig. 35
LABORATORY EQUIPMENT FOR PHYSICAL TESTS 77
shows the very elaborate tanks in the Lesley Cement
Laboratory at the University of Pennsylvania.
Table. Any ordinary strong table may be used, but it
must have a mixing plate of slate, marble or glass.* A
* The writer believes the ordinary laboratory bench is too high for good
and comfortable working, and therefore advises the use of a bench or table
about 3 ft. i in. to 3 ft. 3 ins. high.
CEMENT TESTING
special table, 2 feet 6 inches wide and about 3 feet 3 inches
high, covered with a glass plate and having a tin spout
leading from the top, at the back, or one
end to a refuse can is very convenient.
The spout must be open and 5 or 6 inches
wide; otherwise it is likely to clog.
Burette (Fig. 8). This is one of the in-
dispensable pieces of apparatus in a cement
laboratory. It is used almost constantly
for measuring the water used in mixing
and for other purposes. Fig. 36 shows
the burette used in the Lesley Cement
Laboratory, University of Pennsylvania.
A water pipe is connected to each bench to
which the burette is attached.
Briquette molds should be made of brass, bronze, or
some equally noncorrodible material, and have sufficient
metal in the sides to prevent spreading during molding.
There are two types of molds, single (Fig. 13) and gang
(Fig. 14). Gang molds, permitting the molding of 3, 4 or
5 briquettes at a time, are to be preferred, since a greater
quantity of mortar can be mixed at one time, giving more
uniform results.
Cube molds are shown in Fig. 16. What has been said in
regard to briquette molds applies equally well to cube molds.
Bar molds, shown in Fig. 17, are used for making bars for
the transverse test. Like the other molds, they must be
strong and noncorrodible.
FIG. 36.
LABORATORY EQUIPMENT FOR PHYSICAL TESTS 79
Miscellaneous articles, such as are found in all physical
and chemical laboratories, are needed in the testing of
cement. Most of these, if not all, have been mentioned
under the tests in which they are used, but they are re-
peated in the following list: glass rod, glass tubing, small-
stemmed glass funnel, J-inch camel's hair brush, pipette,
scoop, thermometer, ringstand, tripod, Bunsen burner,
evaporating dish, oil can and light machine oil, settling jar,
bottles of various sizes, trowel, etc.
For list of equipment needed for a cement laboratory,
or for a simple field outfit for a contractor, see " Practical
Cement Testing," pp. 239-240.
PART II.
THE CHEMICAL ANALYSIS OF CEMENT, LIMESTONE,
MARL, ETC.
IT is doubtful if chemical analysis plays any part in the
testing of cement for defects in manufacture, inasmuch as
the results show only the proportions of the various in-
gredients and not their arrangement. Chemical analysis
does, however, serve as a valuable means of detecting
adulterations in cement, and also shows whether those
elements believed to be harmful are present in too large
quantities.
Cement, limestone, marl and clay are all composed of
essentially the same elements, though in different propor-
tions and in different combination. The latter statement
can be better appreciated from the fact that although
cement, limestone and marl are easily decomposed by
hydrochloric acid, clay is scarcely affected at all. The va-
rious determinations made in the analysis of a cement are,
therefore, practically the same as those made in the analysis
of a limestone, marl, clay, slag or any other cement material,
though in the case of the latter substances, an entirely
different preliminary treatment is often necessary before
these determinations can be made.
80
THE CHEMICAL ANALYSIS OF CEMENT, ETC. 8 1
The analysis of any of the above-mentioned substances
requires a considerable knowledge of analytical chemistry —
a knowledge which can be acquired only by actual practice
in the laboratory, and not from books alone. The chem-
ical Npart of this manual has been written for the use of
students who presumably have a knowledge of at least the
rudiments of quantitative analysis.
The method for the analysis of cement hereafter given is,
in general, the same as that reported by the New York
section of the Society of Chemical Industry, and subse-
quently indorsed and published by a committee of the
American Society of Civil Engineers. The authors have,
however, somewhat enlarged upon the methods for the
various determinations in the hope of making them more
readily understood by less practiced chemists. Further-
more, in one or two places the method has been modified
in such a way as to make it, in their estimation, far more
satisfactory for general use. Alternate methods have been
included for certain determ nations.
The methods of analysis given are for cement, and the
raw material from which it is made, among which may
be mentioned clay, limestone, marl, and slag. Of these
materials clay alone is not at all decomposed by hydro-
chloric acid and hence must be subjected to a different
treatment as described later. The analysis of a cement
should consist of determinations of the following:
82 CEMENT TESTING
Loss on ignition CaO.
Moisture. MgO.
CO2. Alkalies.
SiO2. S.
Fe203. SO3.
A1203.
Aside from these constituents, a cement always contains
slight amounts of organic matter and sometimes also traces
of manganese and phosphoric acid. The two latter , how-
ever, are so unusual the authors have not deemed it neces-
sary to include methods for their determination. Average
analyses of usual grades of cement have been given on p. 3,
Chapter I.
Loss on ignition is always determined and represents the
sum of CO2, organic matter, and moisture. But the
results are always somewhat affected by other factors as,
for example, the changing of Fe2O3 to Fe3O4, of FeS to
Fe2O3, and if manganese happens to be present, the chang-
ing of MnO to Mn3O4. Furthermore, small amounts of the
alkalies are liable to be lost by volatilization during the
ignition. With an ordinary cement, however, the error
due to these factors is negligible.
Sulphur may be present in a cement as sulphate or as
sulphide — both are usually present. The sulphur as
sulphate is first determined, and then the total sulphur is
determined as sulphate. From the difference between
these two determinations the amount of sulphur existing
as sulphide can be easily calculated.
THE CHEMICAL ANALYSIS OF CEMENT. ETC. 83
Frequently C02 is not determined directly, but is calcu-
lated from the loss on ignition, and likewise many chemists
determine the alkalies only by difference. Obviously this
practice is far from good for very exact analyses and for
this reason the authors have included methods for all
determinations. For ordinary practical work, however,
the calculation of CO2 and of alkalies is probably entirely
sufficient. In all analyses it is advisable to run duplicates,
or " checks."
PREPARATION or THE SAMPLE FOR ANALYSIS.
The sampling of cement has been discussed rather fully
in a previous chapter (p. 7), but inasmuch as only a small
FIG. 37.
sample is employed in the chemical analysis, usually about
25 grams, a few words may be said as to the method em-
ployed in reducing the sample to this size. This is ac-
complished by " quartering." The sample is spread out
on a large sheet of paper and divided into four equal parts
by means of two lines drawn perpendicular to each other,
as shown in Fig. 37. Two diagonally opposite quarters
are then brushed away (Fig. 38), and the two remaining
quarters are combined and thoroughly mixed. This is
84
CEMENT TESTING
again spread out and quartered, etc., the process being
continued until about 25 grams are left.
FIG. 38.
In sampling limestone, slag, clay, etc., it is not necessary
to reduce the entire sample to fine powder. The material
should be broken up to pea size and then quartered until
about 100 grams are left. This 100 grams should then be
finely powdered on a bucking board or in a mortar, and
passed through a loo-mesh sieve. Of the finely powdered
sample, 25 grams are sufficient.
The finished sample should (be transferred to a tightly
stoppered bottle or weighing flask, and should be properly
labeled with number, date received, source and any other
data which may be peculiar to the sample.
ANALYSIS OF CEMENT.
Loss on Ignition. (C02 + H2O + organic matter).*
Weigh out into a platinum crucible about 0.5 gram of the
finely divided sample. Place the crucible on a triangle
and apply heat, gently at first, then with the full force of a
good blast lamp for 15 minutes. The blast flame should
never be directed vertically against the bottom of the
* See p. 82 for causes of error in this determination.
THE CHEMICAL ANALYSIS OF CEMENT, ETC. 85
crucible but preferably at an angle against the side and
bottom.
Cool the crucible in a dessicator and weigh. Heat again
for 5 or 10 minutes in the blast flame, cool and weigh.
Repeat until the weight is constant. The loss in weight
is known as the " loss on ignition," and represents the sum
of the C02, H2O and organic matter.
SILICA (SiO2).
Carefully transfer the residue from the above determina-
tion of loss on ignition* to a platinum dish and carefully
rinse out the crucible two or three times with dilute HC1,
adding the rinsings, of course, to the contents of the dish.
Add enough more dilute HC1 to entirely cover the powder,
place the dish on a water bath and evaporate to dryness —
that is, until the odor of HC1 can no longer be detected.
Treat the residue with 10 c.c. strong HC1, digest on the
water bath for 10 minutes with occasional stirring, and
dilute with 35 c.c. of water. Allow the dish to digest on
the water bath for 15 minutes. Filter through a small
filter and wash the residue (Si02) thoroughly with hot
water.
Transfer the filtrate to a platinum dish and again evapo-
rate | to dryness on the water bath. Allow to stand on the
* A fresh sample may be used instead of taking the residue from the
determination of loss on ignition. Such a procedure is certainly advisable
if time is a factor.
t The second evaporation for silica is frequently omitted where great
accuracy is not desired. The authors strongly advise two evaporations,
however.
86 CEMENT TESTING
water bath until the odor of HC1 is no longer perceptible.
Moisten the residue with 5 c.c. strong HC1, digest for 10
minutes, and dilute with 35 c.c. of water. Allow to digest
on the water bath for 10 or 15 minutes. Filter through a
small filter and wash thoroughly with hot water. (The
filtrate, A, is used for the determination of Fe2O3 and
A1203.)
Transfer the two papers containing silica, while still wet,
to a weighed platinum crucible, cover and apply heat,
gently at first to dry and char the paper, then remove the
cover and gradually increase the temperature to burn the
paper. After the paper is burned, heat the crucible for
15 minutes over a good blast flame, being careful to prevent
the blast from playing in or close to the mouth of the
crucible. Cool in a desiccator and weigh. The process of
heating, cooling and weighing should be continued until
the weight is constant. This gives total silica (SiCfe).
The ignited silica should be white. If it is dark colored
it is impure and may contain some particles which were
not decomposed by the acid. In order to purify the silica,
it must first be fused with sodium carbonate. Add to the
silica in the crucible about five times its weight of pure,
dry sodium carbonate and mix thoroughly by means of a
platinum spatula or glass rod. Fuse over a good Bunsen
burner as described later under the heading, " Analysis
of Clay " (p. 107). After the fused mass has cooled, dis-
solve it in water, carefully add dilute HC1 until in excess,
and evaporate to dryness on the water bath. Take up the
THE CHEMICAL ANALYSIS OF CEMENT, ETC. 87
silica as described above, etc. (The filtrate should be
added to the main filtrate, A .)
IRON AND ALUMINA (Fe2O3 + A12O3).
To the filtrate, A, from the second evaporation for silica,
add a little NH4C1 solution and a few drops of strong
HNO3. Heat to boiling and precipitate the iron and
alumina as hydrates by adding a slight excess of NH4OH.
Again heat to boiling for a moment,* wash once by de-
cantation with boiling water containing a drop of NH4OH,
and filter as rapidly as possible. Wash the precipitate on
the filter once or twice with boiling water containing a
drop of NH4OH. In this precipitation an effort should be
made to keep the solution as hot as possible and to filter
as quickly as possible. If allowed to cool, some alumina is
changed to a soluble form and hence results in loss, f The
filtration may be advantageously hurried by use of a force
filter and platinum cone as suggested by Treadwell.}
(The filtrate, B, is used for the determination of lime, CaO.)
Redissolve the precipitated Fe(OH)3 and A1(OH)3 on the
filter by means of a small amount of hot dilute HC1, and
allow the solution to run into a clean beaker. Wash the
paper well with hot water. Heat to boiling and reprecipi-
tate the iron and alumina by adding a slight excess of
* If boiled too long the precipitate becomes gelatinous and filtration
is difficult.
t Alumina lost here will appear later in the precipitate of calcium and
will be weighed as CaO.
t See "Analytical Chemistry," Treadwell-Hall.
88 CEMENT TESTING
NH4OH as before. Quickly filter while hot and wash with
hot water containing a drop of NH4OH. (The filtrate, C,
is added to filtrate B from the first precipitation of iron and
alumina and is used for the determination of lime, CaO.)
Dry the filter paper containing the iron and alumina in
a drying oven. When thoroughly dry fold the paper to a
small volume and twist it onto the end of a platinum wire.
Carefully burn the paper on the wire, holding it so that the
ash will fall into a weighed platinum crucible. When the
wire is cool, brush any adhering particles of oxide into the
crucible. Place the crucible without cover on a triangle and
ignite by means of a good Bunsen burner. Do not use the
blast lamp. Cool and weigh. The combined weight of
the Fe203 and the A12O3 is thus obtained.*
Fe203.
To the crucible containing the Fe203 and A12O3 add about
3 grams of K2S2O7t and apply heat by means of a Bunsen
burner turned low. Gradually increase the heat until the
bottom of the crucible looks red as seen from above. Allow
* If the material under examination contains phosphoric acid, the latter
will be present in the precipitate of iron and alumina and will be weighed
as P2O5.
To determine the amount present, a separate sample should be employed,
the phosphoric acid being precipitated from nitric acid solution by means
of ammonium molybdate solution, and weighed as magnesium pyrophos-
phate, Mg2P2Oy, or as phosphomolybdic anhydride, 24 MoO3.P2Os, as
described in vol. ii, " Analytical Chemistry," by Treadwell-Hall.
The result is calculated to P2OS and the amount subtracted from the
total Fe2O3 and A12O3 found.
f KHSC>4 is frequently employed instead of K^SaO?. The latter salt
is preferable.
THE CHEMICAL ANALYSIS OF CEMENT, ETC. 89
to cool; then dissolve in water. The solution thus ob-
tained contains the iron and alumina in the form of sul-
phates together with the excess of K2SO4.
To determine the Fe2Os, the solution is acidified with
H2SO4, the iron reduced to the ferrous condition, and then
titrated with a standardized KMnO4 solution. The re-
duction of the iron may be brought about by one of the three
methods described below.
Reduction by Means of Zinc. Introduce the solution of
iron and alumina from the bisulphate fusion into a 200 c.c.
Erlenmeyer flask fitted with a one-hole rubber stopper,
carrying an exit tube as shown in the
drawing (Fig. 39). Add about 3 grams
of pure, finely divided zinc and a few
cubic centimeters of concentrated H2S04.
Tightly stopper the flask and allow the
outer end of the exit tube to dip into a
beaker of water as illustrated. This
serves as a trap. The hydrogen generated by the sul-
phuric acid and zinc completely reduces the iron to the
ferrous condition and drives all air from the flask.
When the zinc is entirely dissolved, filter rapidly through
a Gooch crucible and wash the crucible several times with
small amounts of water. Remove the stopper and quickly
titrate the solution in the filter flask with a standardized
solution of KMnO4. The number of cubic centimeters of
KMnO4 solution used, multiplied by its Fe203 factor, gives
the total weight of Fe2O3.
9°
CEMENT TESTING
Reduction with a Jones Reductor. A very convenient,
as well as quick, method of reduction is accomplished by
the aid of a Jones reductor. This apparatus is a glass tube
of the form shown in Fig. 40, and is fitted to a filter flask
by a tightly fitting rubber stopper. The
reductor is filled as follows: Directly over
the stopcock a few glass beads are placed and
over these a little glass wool. This is then
covered with a layer of sand. The balance
of the tube, up to the enlargement at the top,
is then filled with pure granulated zinc, after
which the apparatus is ready for use.
Once filled, it may be used indefinitely
with no care save the occasional addition of
a little zinc as the column of this metal is
reduced by the action of acid. When not
in use, the reductor should be tightly stop-
pered to prevent evaporation, and under no circumstances,
either when in use or not in use, should the surface of the
liquid be allowed to recede below the top of the column of
zinc.
The operation of reduction is as follows: Suction is
applied to the filter flask and the stopcock of the reductor
is so regulated as to allow the liquid to be slowly drawn
through the reductor into the filter flask. At first a little
dilute H2SO4 is drawn through the apparatus. The liquid
to be reduced, which should contain enough H2S04 to have
a moderate action on zinc, is then run through, and this is
FIG. 40.
THE CHEMICAL ANALYSIS OF CEMENT, ETC. QI
followed by successive small quantities of water to displace
all acid. The reductor is then removed from the flask
and the solution in the latter is rapidly titrated to a per-
manent pink color by means of standardized KMnO4 solu-
tion. As before mentioned, great care must be exercised
during the process of reduction to prevent the surface of
the liquid from falling below the top of the column of zinc.
Reduction by Means of H2S. The solution from the bi-
sulphate fusion is placed in a 200 c.c. flask, tightly stoppered
with a rubber stopper provided with two tubes through
which gas can enter and leave the flask (Fig. 41). The
tube through which the gas enters should dip below the
surface of the liquid, as is shown in the drawing. The
solution is heated to boiling and a current HS
of pure H2S is passed through until the
solution is saturated. The tube through
which the gas enters is now connected with
a C02 generator, and while the solution in
the flask is still boiling C02 is passed
FIG. 41.
through until all H2S has been removed -
until wet lead acetate paper held near the exit tube is no
longer blackened. The solution is then allowed to cool in
the atmosphere of CO2, after which it is filtered and then
titrated with standard KMnO4 as previously described.
A1203.
The total weight of A1203 is simply the difference between
the combined weight of Fe203 and A1203, and Fe203 alone.
92 CEMENT TESTING
LIME (CaO).
Combine the filtrates B and C from the two precipita-
tions of iron and alumina, acidify with HC1 and evaporate
to a volume of about 250 c.c. Make alkaline with NH4OH
and heat to boiling.* While the solution is still boiling,
add an excess of a boiling solution of (NH4)2C2O4. Boil
for a moment longer and then allow to stand and settle for
20 minutes, or, better still, over night. Filter and wash
thoroughly with hot water containing a little (NH4)2C2O4.t
(The nitrate, D, is used for the determination of magnesia,
MgO.)
Place the filter paper containing the precipitate while
still wet in a weighed platinum crucible and heat carefully
in the Bunsen flame until the paper
is burned. Cover the crucible and
ignite for 15 or 20 minutes in a good
strong blast, to completely reduce
the oxalate to oxide. After ignition
quickly transfer the hot crucible to
a desiccator, preferably one fitted with a U-tube containing
soda lime as shown in Fig. 42. When cool, weigh. The
crucible should be reheated, cooled and weighed until the
weight is constant. This gives total lime, CaO.
* A little A1(OH)3 often separates at this point. This will not happen,
however, if the Fe(OH)3 and A1(OH)3 precipitates were kept hot while being
filtered. If any separates, it should be filtered off, ignited and weighed.
f Some chemists prefer to redissolve and reprecipitate the calcium, but
this is entirely unnecessary in ordinary analytical work.
THE CHEMICAL ANALYSIS OF CEMENT, ETC. 93
MAGNESIA (MgO).
To the filtrate D from the calcium oxalate precipitation,
add HC1 until acid. Evaporate to a volume of about 75 or
100 c.c. Then add an excess of Na2HPO4 or NaNH4HPO4
solution and ammonia in moderate excess. Allow to stand
at least 4 hours (better over night).* Filter and wash once
or twice with a 2.5 per cent solution of NH4OH.
Dissolve the precipitate on the paper in a little hot,
dilute HNO3. Add a few drops of Na2HPO4 solution and
then NH4OH, drop by drop, until in moderate excess, with
constant agitation of the solution. Allow to stand 4 hours,
or over night if convenient. Filter and wash with 2.5 per
cent NH4OH. Reject the filtrate.
Transfer the precipitate and paper while still wet to a
weighed platinum crucible and heat with a low Bunsen flame
to dry and char the paper. Burn the paper at as low a
temperature as possible. When entirely burned, ignite
the crucible in a weak blast flame, cool and weigh. Repeat
until constant weight is obtained. This gives weight of
MgO as Mg2P207. This weight, multiplied by the factor
0.3621, gives total magnesia, MgO.
SULPHURIC ACID (SO3).
Into a porcelain evaporating dish or casserole, weigh out
one gram of the finely powdered sample, add dilute HC1 to
* It is not necessary to remove ammonium salts before making this first
precipitation of magnesia. Large amounts of ammonium salts do, however,
greatly retard precipitation.
94 CEMENT TESTING
cover the powder and take to dryness on the water bath.
(By this treatment all the sulphur which was present in the
cement as sulphide will be expelled as H2S.) Dissolve the
residue in water,* treat with NH4OH and (NH4)2C03 in
excess, filter and wash thoroughly. Concentrate the fil-
trate, acidify with HC1, heat to boiling for a moment and
precipitate the sulphuric acid as BaS04 by adding a boiling
solution of BaCl2, drop by drop, with constant stirring, until
in excess. Allow to stand on the water bath about two hours,
filter and wash. Or, if convenient, allow to stand over night
at the ordinary temperature before filtering. Transfer the
filter and precipitate to a platinum crucible and burn the
paper at as low a temperature as possible. Ignite for 10
or 15 minutes with the cover off, cool and weigh as BaSO4.
The weight of BaSO4 obtained multiplied by the factor
0.3430 gives weight of sulphuric acid (SO3).
TOTAL SULPHUR.
For the determination of total sulphur, two methods are
available. The first to be described below, the fusion
method, is the one reported by the committee on uniform
methods of analysis. The alternate method is a very good
one and is especially good for the determination of sulphur
in cement.
* Many chemists filter the solution at this point and precipitate the sul-
phuric acid immediately without going through the NH4OH and (NH^COa
treatment. This procedure seems to be very satisfactory though it is
liable to give too high results, inasmuch as the BaSC>4 brings down other
substances mechanically.
THE CHEMICAL ANALYSIS OF CEMENT, ETC. 95
Fusion Method. About i gram of the powdered sample
is weighed out into a large platinum crucible and about
5 or 6 grams of pure dry Na2C03 (free from sulphur) and
0.3 gram of KNOa are added.* This charge should be
intimately mixed by means of a platinum spatula or glass
rod, and then fused. In order to protect the contents of
the crucible from sulphur in the flame, the crucible should
be placed through a hole in a piece of asbestos board held
in a slightly inclined position. A good Bunsen burner is
sufficient to bring about the fusion. Heat until a quiet
fusion is obtained.
After cooling, the melt is treated in the crucible with
boiling water and the solution poured into a tall beaker.
More hot water is added and the whole is agitated until
disintegration is complete. The solution is then filtered,
the filtrate is acidified with HC1 and diluted to about
250 c.c. It is then heated to boiling and the S03 is pre-
cipitated as BaS04, by the addition, drop by drop, of a
boiling solution of BaCk as previously described in the de-
termination of sulphuric acid. The precipitate is filtered,
washed, ignited and weighed as described in the same place.
The weight of BaSO4 obtained, multiplied by the factor
0.1374, gives total sulphur.
Bromine Method. This method depends upon the oxida-
tion of S to 80s by means of Br water. Weigh out i gram
* As the reagents here used, Na2COs and KNOs, are liable to contain
sulphur, a blank should be run first. Results of subsequent analyses can
then be corrected for the amount found.
96 CEMENT TESTING
of the sample into a porcelain evaporating dish or casserole
and treat with Br water in excess. Allow to digest on the
water bath for 10 or 15 minutes, then acidify with HC1 and
evaporate to dryness. Moisten the residue with i c.c. of
concentrated HC1 and dilute with 200 c.c. of water. This
solution is then treated with NH4OH and (NH4)2CO3, etc.,
as described previously in the determination of sulphuric
acid (SO3). This result gives all the sulphur as BaS04;
this figure, multiplied by the factor 0.1374, gives total
sulphur.
SULPHUR EXISTING IN THE CEMENT AS SULPHIDE.
From the weight of BaSO4, obtained in the determination
of total sulphur, subtract the weight of BaSO4 obtained
in the determination of sulphuric acid (SO3). The dif-
ference will represent the sulphur existing in the cement as
sulphide, weighed in the form of BaSO4. By multiplying
this weight by the factor 0.1374 the weight of sulphur (S)
existing as sulphide will be ascertained.
MOISTURE.
If a determination of moisture is desired, it can be made
in the following simple manner. Weigh out into a platinum
crucible i or 2 grams of the sample and heat for an hour in
an air bath maintained at a temperature of 110°. The
crucible is then cooled in a desiccator and weighed. This
procedure should be repeated until the weight is con-
THE CHEMICAL ANALYSIS OF CEMENT, ETC. 97
slant. The loss in weight represents moisture in the
cement.*
ALKALIES.
In the analysis of cement, many chemists determine
alkalies solely by difference, a procedure which is entirely
satisfactory for all ordinary purposes. In accurate work,
however, and especially in the analysis of clay, the alkalies
must be determined gravimetrically. For this determina-
tion the J. Lawrence Smith method alone is satisfactory.
About 0.5 gram of the sample is intimately mixed with
an equal weight of pure NH4C1 and 3 grams of pure CaCO3.
This mixing is usually done in an agate mortar. The mix-
ture is transferred to the crucible and
covered with about i gram of pure
CaCOs.
The J. Lawrence Smith crucible, which
was especially designed for this determi-
nation, is a long tube-like receptacle
with a cap for the open end. When the
crucible is filled it is capped and placed
in an inclined position in a clay cylinder,
as shown in Fig. 43. The outer end of
the crucible remains cool and thus prevents loss by volati-
lization. Instead of a clay cylinder a piece of asbestos
* A rough determination of moisture is sometimes made in testing
laboratories, with a 100 or 200 gram sample in a porcelain evaporating dish,
the weighings being made with an ordinary scale as described on page n.
Such a determination is probably entirely satisfactory for all practical
purposes.
FIG. 43-
98
CEMENT TESTING
board with a hole in the center to admit the crucible may be
conveniently used by clamping it in a vertical position.
An ordinary platinum crucible of 25 or
30 c.c. capacity may be used for this de-
termination with equally good results,
though it requires a little more care during
the process of heating. If an ordinary
crucible is employed, it should be fitted
into a hole in a piece of asbestos board
so that about half or two-thirds of the
crucible protrudes below the board (Fig.
44). The crucible should be covered
FIG. 44. with a platinum lid.
Heat is at first applied by means of a Bunsen burner
turned very low, or placed some distance below the crucible.
If a regular J. Lawrence Smith crucible is employed, a flat
flame should be used. When the odor of ammonia is no
longer perceptible, the temperature is gradually raised until
the full flame of a strong Bunsen burner is employed.
Two burners can be used with the J. Lawrence Smith
crucible. This heat is continued for about 40 minutes.
After the crucible is cool, the cintered mass is loosened by
gently tapping the crucible and is then transferred to a
porcelain or platinum dish, and treated with 50-75 c.c. of
water. Any of the mass which sticks to the crucible is
loosened by digesting with a little water, and washed into
the dish.
The dish containing the cintered mass and water is
THE CHEMICAL ANALYSIS OF CEMENT, ETC. 99
digested on the water bath for 30 minutes and any large
particles are broken by means of a glass rod. Water lost
by evaporation should be replaced.
When disintegration is complete, the solution in the dish
is decanted through a filter and the residue washed 3 or 4
times by decantation. The residue is then transferred to
the filter and washed until free from chlorides.*
The filtrate is then treated with an excess of NH4OH
and (NH4)2CO3, heated to boiling, filtered and washed once
or twice. Inasmuch as the precipitate probably still con-
tains traces of alkalies, it should be dissolved in HC1 and
reprecipitated by mean's of NH4OH and (NH4)2CO3 in
excess. It is now filtered and washed thoroughly. The
two filtrates are combined, evaporated to dry ness on the
water bath and then gently ignited to expel all ammonium
salts. Dissolve the residue in a small amount of water
and treat with a little NH4OH and (NH4)2C2O4 to remove
the last traces of Ca. Allow to stand over night; filter
and wash, allowing the filtrate and washings to run into a
weighed platinum dish or large crucible. Evaporate to
dry ness and ignite to expel ammonium salts as before.
Allow to cool; moisten with HC1 to change any carbonate
into chloride, again evaporate tp dryness and ignite at a
low red heat. Cool in a desiccator and weigh. This gives
total alkali as chloride.
Determination of Potassium (K2O). Dissolve the ignited
chlorides in a small amount of water and treat with a slight
* The residue on the filter should be entirely soluble in HC1.
100 CEMENT TESTING
excess of platinum chloride solution. The approximate
amount of platinum chloride solution necessary can be
easily calculated from the weight of the alkali as chloride
determined above. The solution should be so dilute that
the precipitate redissolves when heated on the water bath.
Allow to evaporate on the water bath until the residue
solidifies on cooling. Drench the solidified mass with
absolute alcohol or with 80 per cent alcohol, and decant
the liquid through a very small filter. Wash by decanta-
tion with alcohol of the same strength, being careful to
bring as little as possible of the precipitate on the paper.
The dish and filter are allowed to dry for a few moments,
after which the contents of the dish are transferred to a
weighed platinum crucible. Any particles of the K2PtCl6
precipitate still adhering to the dish should now be washed
through the filter by means of hot water, the solution being
caught in the crucible. The latter is then placed on the
water bath for a time and then heated for a few moments
in an air bath at 135°. The dish should be covered during
the first few moments in the air bath to prevent loss due
to decrepitation. The crucible is cooled in a desiccator and
weighed. The weight of K2PtCl6 thus obtained, multiplied
by the factor 0.1937, gives the weight of potassium as K2O.
Determination of Sodium Oxide (Na2O). To calculate
the weight of Na20, multiply the weight of K2PtCl6 above
found by the factor 0.3067 to find the weight of potassium
as KC1. This weight should be subtracted from the total
weight of alkalies as chloride previously determined. The
THE CHEMICAL ANALYSIS OF CEMENT, ETC. IOI
difference, which represents the weight of sodium as Nad,
should be multiplied by the factor 0.5303, which gives the
weight of sodium as Na2O.
CARBON DIOXIDE (CO2).
The determination of CO2 may be made by either of two
totally different methods, the " indirect " and the " direct,"
both of which are described below.
The " indirect " method has the advantage of being
rapid and requires less apparatus. It is not as accurate as
the direct method, although for determinations in limestone,
marl, or other substances rich in CO2, it yields very satis-
factory results. This method is far less satisfactory for
cement, inasmuch as the percentage of C02 therein is very
small.
The " direct " method is very accurate and especially
well adapted to substances containing only small amounts
of CO2. The apparatus required, although somewhat com-
plicated, is easily assimilated and consists only of such
pieces as are ordinarily found in a chemical laboratory.
INDIRECT METHOD.
The principle involved in the " indirect " method is the
determination of the loss in weight due to expulsion of the
CO2. A special form of apparatus is needed for this deter-
mination, the Schrotter apparatus,* shown in Fig. 45, being
one of the more common forms.
* Many other forms of apparatus have been described for this de-
termination, among them those of Bunsen, Fresenius, Mohr, Geissler,
IO2
CEMENT TESTING
FIG. 45-
Procedure. The apparatus is first cleaned and dried.
Compartment b is then about one-third filled with concen-
trated H2S04 and compartment c is
nearly filled with dilute HC1 (i to 3).
The glass stopper is then replaced in c
and the end of b is closed by means of
a piece of rubber tubing carrying a
piece of glass rod in one end. The
apparatus is then weighed.
The sample is then introduced into
the apparatus through #, after which
the stopper is quickly replaced and
the apparatus is again weighed. The
increase in weight is the weight of the sample.
The rubber stopper is now removed from the end of b
and stopcock d is partially opened to allow the HC1 in c
to run slowly down into the flask and come into contact
with the sample. The C02 is thus liberated and is forced
out of the apparatus through b, the concentrated H2SO4 in
this compartment preventing the escape of moisture. The
flow of HC1 is so regulated that the C02 bubbles through
the H2SO4 slowly — not faster than two bubbles per
second.
After decomposition is complete and all HC1 has run from
c into the flask, stopcock d is closed and the flask is gradually
Rohrbeck, etc. All of these are designed on the same principle as the
Schrotter apparatus and all are equally well adapted to the determination
of CC>2 in carbonates, etc.
THE CHEMICAL ANALYSIS OF CEMENT, ETC. 103
heated until the boiling point is reached, in order to expel
any CO2 remaining in solution.
The stopcock d is then quickly opened and the stopper in
c is quickly replaced by a one-hole rubber stopper carrying
a drying tube filled with soda lime. The end of compart-
ment b is now connected with a CaCl2 tube which in turn is
connected with an aspirator and a current of air is slowly
drawn through the apparatus to drive out all CO2.
After several liters of air have been drawn through the
apparatus, and the liquid contents of the latter are cool, the
glass stopper is again placed in c, and the end of b is again
closed by means of the rubber tube and glass rod. The
apparatus is now carefully weighed. The loss in weight
represents the weight of CO2.
DIRECT METHOD.
In the direct determination of CO2, the gas, evolved by
the action of acid, is first passed through a number of drying
tubes, after which it is absorbed in soda lime or a concen-
trated solution of KOH. By weighing the absorption tubes
before and after the experiment, the actual weight of the
CO2 is obtained.
The apparatus employed is shown in Fig. 46. The flask
b is of about 100 c.c. capacity and is used for the decompo-
sition of the sample. The U-tube c contains a few glass
beads moistened with a little concentrated H2SO4.* The
* A small condenser can be advantageously employed between b and c,
so arranged as to cause moisture condensed to run back into b.
IO4
CEMENT TESTING
first half of d is filled with CaCk and the second half with
anhydrous CuSO4 and glass wool or pumice, e contains
CaCl2 to remove final traces of moisture. Glass stoppered
U-tubes / and g are the absorption tubes. The former is
THE CHEMICAL ANALYSIS OF CEMENT, ETC. 105
filled with soda lime and the latter contains soda lime in the
first half and CaCl2 in the other half. This CaCl2 absorbs
any moisture liberated by the absorption of CO2 in the soda
lime, h is a Liebig bulb filled with concentrated H2SO4.
This prevents moisture from backing up into the absorption
tubes, and also indicates the rate at which the gas is passing
through the apparatus. The bulb h is connected directly
to the aspirator. The small U-tube a is filled with soda lime,
and is attached as shown in the figure while air is being
drawn through the apparatus, thus freeing it from CO2.
After filling the various tubes as described above, they
are joined together as shown in the drawing, by means of
small pieces of rubber tubing. Every joint should be
securely wired.
Procedure. Air is first passed through the apparatus for
some time in order to free it from traces of CO2. During
this process h may be connected directly to e, as it is not
necessary for the absorption tubes to be in position. The
weighed sample is then introduced into the flask b, which is
immediately closed. The tube a is now removed and the
funnel tube in b is filled with dilute HC1 (about 1:3). The
two absorption tubes, which should be tightly closed, are
now weighed, after which they are connected with the
apparatus, as shown, and the joints tightly wired.
The dilute HC1 in the funnel tube is now allowed to run
into b a little at a time, to decompose the carbonate. The
rate of flow must be so regulated that not more than two
bubbles a second pass through h. When all HC1 has run
106 CEMENT TESTING
into b, the stopcock in the funnel tube is closed and the
contents of the flask are gradually heated to the boiling
point to drive out any CO2 in solution in the acid. The
flame is then removed, the stopcock in the funnel tube is
opened and the U-tube a connected as shown in the draw-
ing. By means of the aspirator, air is now drawn through
the apparatus to completely sweep all CO2 into the absorp-
tion tubes.
After several liters of air have been aspirated through the
apparatus, the stoppers in / and g are tightly closed, after
which they are taken from the apparatus and weighed.
The increase in weight is the weight of the CC>2.
ANALYSIS or LIMESTONE.
Limestone is essentially a carbonate of calcium, but it
always contains more or less silica, iron, alumina, and
magnesia as impurities. Limestone is very readily at-
tacked by dilute HC1, hence no preliminary treatment is
necessary to prepare it for the various determinations.
Procedure. Weigh out 0.5 gram of the finely powdered
sample into a good- sized platinum dish and add water to
cover the powder. Add dilute HC1, a little at a time,
being careful to cover the dish quickly with a watch glass
after each addition. When sufficient acid has been added
and effervescence no longer takes place, wash the cover
glass, allowing the washings to run into the dish, place the
latter on the water bath and evaporate to dryness. Take
up with HC1 and water, etc., and proceed with the
THE CHEMICAL ANALYSIS OF CEMENT, ETC. 107
various determinations as heretofore described under the
heading, " Analysis of Cement."
Moisture, loss on ignition, and C02 are made with sepa-
rate samples. Frequently CO2 is determined by difference
— a method which yields results entirely satisfactory for
all ordinary purposes.
Determinations of SO3, total S, and alkalies are not
necessary.
ANALYSIS or MARL.
In the analysis of marl, decomposition is effected by
means of HC1 as described under the heading, " Analysis
of Limestone." Marl may, however, contain more or less
clay which is not decomposed by the acid. If this is the
case, as can readily be told from the appearance of the
silica, the latter must be fused with dry Na2CO3, as de-
scribed under the heading, " Analysis of Clay."
In the analysis of marl the same determinations should
be made as in the case of cement — the analysis should
always include determinations of S, SO3 and alkalies.
ANALYSIS or SLAG.
In the analysis of slag, proceed exactly as in the case of
cement, making all the determinations as described under
the heading, " Analysis of Cement."
ANALYSIS OF CLAY.
In the analysis of clay, practically the same determina-
tions are made as in the case of cement, although a far
108 CEMENT TESTING
different preliminary treatment is necessary on account of
the insolubility of clay in HC1. This preliminary treat-
ment consists in fusing the clay with Na2CO3, thereby
changing its ingredients into forms which are readily de-
composed by HC1.
About 0.5 gram of the finely powdered sample* is weighed
out into a platinum crucible of 25 or 30 c.c. capacity, 3 or
4 grams of pure dry Na2CO3 are added, and the whole is
intimately mixed by stirring with a platinum spatula or
glass rod. A little Na2CO3 is now sprinkled on top, the
crucible covered, placed on a triangle and heated. Heat
should be applied gently at first by means of a Bunsen
burner turned low. The temperature is then gradually
raised until the full force of a Teclu burner or blast lamp
is used. The heating is continued until CO2 is no longer
evolved, and the contents of the dish are in a state of quiet
fusion.
When the crucible is cool it is placed in a beaker and
partially covered with water. It is then allowed to digest
until the melt is thoroughly disintegrated. The crucible
is then withdrawn and washed with water and a little
dilute HC1, the washings being added to the contents of
the beaker.
The beaker is then covered with a watch glass and HC1
is added a little at a time, the watch glass being quickly
replaced after each addition of acid. When C02 is no
* It is customary to dry the sample at 105 or 110° in the air bath before
making the analysis.
THE CHEMICAL ANALYSIS OF CEMENT, ETC. 109
longer evolved, the contents of the beaker are transferred
to a platinum dish and evaporated to dryness on the water
bath. The various determinations Si02, Fe2O3, etc., are
then made as heretofore described in the analysis of cement.
For the determination of alkalies in clay, exactly the same
procedure is employed as for the determination of alkalies
in cement.
APPENDIX
STANDARD SPECIFICATIONS AND UNIFORM
METHODS OF TESTING AND ANALYSIS
FOR PORTLAND CEMENT
EMBRACING
THE REPORT OF THE COMMITTEE ON STANDARD SPECIFICATIONS FOR CEMENT
OF THE AMERICAN SOCIETY FOR TESTING MATERIALS; THE REPORT OF
THE COMMITTEE ON UNIFORM TESTS OF CEMENT OF THE
AMERICAN SOCIETY OF CIVIL ENGINEERS; AND THE
REPORT OF THE COMMITTEE ON UNIFORMITY IN
TECHNICAL ANALYSIS FOR LIMESTONES, RAW
MIXTURES AND PORTLAND CEMENTS
OF THE SOCIETY FOR CHEM-
ICAL INDUSTRY (NEW
YORK SECTION)
(Reprinted by permission)
APPENDIX.
STANDARD SPECIFICATIONS FOR PORTLAND CEMENT
Adopted by the American Society for Testing Materials, August i6th,
1909.
GENERAL OBSERVATIONS.
These remarks have been prepared with a view of pointing out the
pertinent features of the various requirements and the precautions
to be observed in the interpretation of the results of the tests.
The Committee would suggest that the acceptance or rejection
under these specifications be based on tests made by an experienced
person having the proper means for making the tests
SPECIFIC GRAVITY.
Specific gravity is useful in detecting adulteration. The results
of tests of specific gravity are not necessarily conclusive as an indi-
cation of the quality of a cement, but when in combination with the
results of other tests may afford valuable indications.
FINENESS.
The sieves should be kept thoroughly dry.
TIME OF SETTING.
Great care should be exercised to maintain the test pieces under
as uniform conditions as possible. A sudden change or wide range
of temperature in the room in which the tests are made, a very dry
or humid atmosphere, and other irregularities vitally affect the rate
of setting.
CONSTANCY OF VOLUME.
The tests for constancy of volume are divided into two classes,
the first normal, the second accelerated. The latter should be re-
garded as a precautionary test only and not infallible. So many
114 APPENDIX
conditions enter into the making and interpreting of it that it should
be used with extreme care.
In making the pats the greatest care should be exercised to avoid
initial strains due to molding or to too rapid drying-out during the
first twenty-four hours. The pats should be preserved under the
most uniform conditions possible, and rapid changes of temperature
should be avoided.
The failure to meet the requirements of the accelerated tests
need not be sufficient cause for rejection. The cement may, how-
ever, be held for twenty-eight days, and a retest made at the end of
that period, using a new sample. Failure to meet the requirements
at this time should be considered sufficient cause for rejection,
although in the present state of our knowledge it cannot be said
that such failure necessarily indicates unsoundness, nor can the
cement be considered entirely satisfactory simply because it passes
the tests.
SPECIFICATIONS.
GENERAL CONDITIONS.
All cement shall be inspected.
Cement may be inspected either at the place of manufacture or
on the work.
In order to allow ample time for inspecting and testing, the cement
should be stored in a suitable weather-tight building having the floor
properly blocked or raised from the ground.
The cement shall be stored in such a manner as to permit easy
access for proper inspection and identification of each shipment.
Every facility shall be provided by the contractor and a period
of at least twelve days allowed for the inspection and necessary
tests.
Cement shall be delivered in suitable packages with the brand
and name of manufacturer plainly marked thereon.
A bag of cement shall contain 94 pounds of cement net. Each
barrel of Portland cement shall contain 4 bags, and each barrel of
natural cement shall contain 3 bags of the above net weight.
Cement failing to meet the seven-day requirements may be held
awaiting the results of the twenty-eight day tests before rejection.
All tests shall be made in accordance with the methods proposed
APPENDIX 115
by the Committee on Uniform Tests of Cement of the American
Society of Civil Engineers, presented to the Society, January 21,
1903, and amended January 20, 1904, and January 15, 1908, with
all subsequent amendments thereto.
The acceptance or rejection shall be based on the following re-
quirements:
PORTLAND CEMENT.
DEFINITION. — This term is applied to the finely pulverized
product resulting from the calcination to incipient fusion of an inti-
mate mixture of properly proportioned argillaceous and calcareous
materials, and to which no addition greater than 3 per cent has been
made subsequent to calcination.
SPECIFIC GRAVITY.
The specific gravity of cement shall not be less than 3.10. Should
the test of cement as received fall below this requirement, a second
test may be made upon a sample ignited at a low red heat. The
loss in weight of the ignited cement shall not exceed 4 per cent.
FINENESS.
It shall leave by weight a residue of not more than 8 per cent on
the No. 100, and not more than 25 per cent on the No. 200 sieve.
TIME OF SETTING.
It shall not develop initial set in less than thirty minutes; and
must develop hard set in not less than one hour, nor more than ten
hours.
TENSILE STRENGTH
The minimum requirements for tensile strength for briquettes
one square inch in cross section shall be as follows and the cement
shall show no retrogression in strength within the periods specified :
Age. Neat Cement. Strength.
24 hours in moist air 175 Ibs.
7 days (i day in moist air, 6 days in water) 500 Ibs.
28 days (i day in moist air, 27 days in water) 600 Ibs.
One Part Cement, Three Parts Standard Ottawa Sand.
7 days (i day in moist air, 6 days in water) 200 Ibs.
28 days (i day in moist air, 27 days in water) 275 Ibs.
Il6 APPENDIX
CONSTANCY OF VOLUME.
Pats of neat cement about three inches in diameter, one-half inch
thick at the center, and tapering to a thin edge, shall be kept in
moist air for a period of twenty-four hours.
(a) A pat is then kept in air at normal temperature and observed
at intervals for at least 28 days.
(b) Another pat is kept in water maintained as near 70° F. as
practicable, and observed at intervals for at least 28 days.
(c) A third pat is exposed in any convenient way in an atmos-
phere of steam, above boiling water, in a loosely closed vessel for
five hours.
These pats, to satisfactorily pass the requirements, shall remain
firm and hard and show no signs of distortion, checking, cracking, or
disintegrating.
SULPHURIC Aero AND MAGNESIA.
The cement shall not contain more than 1.75 per cent of anhydrous
sulphuric acid (SO3), nor more than 4 per cent of magnesia (MgO).
REPORT OF COMMITTEE ON UNIFORM TESTS OF CEMENT
OF THE AMERICAN SOCIETY OF CIVIL ENGINEERS.
Presented at the Annual Meeting, January i8th, ign.
Your Committee on Uniform Tests of Cement presents the fol-
lowing report:
SAMPLING.
i. — Selection of Sample. — The selection of the sample for test-
ing is a detail that must be left to the discretion of the engineer;
the number and the quantity to be taken from each package will
depend largely on the importance of the work, the number of tests
to be made and the facilities for making them.
2. — The sample shall be a fair average of the contents of the
package; it is recommended that, where conditions permit, one bar-
rel in every ten be sampled.
3. — Samples should be passed through a sieve having twenty
APPENDIX 117
meshes per linear inch, in order to break up lumps and remove for-
eign material; this is also a very effective method for mixing them
together in order to obtain an average. For determining the char-
acteristics of a shipment of cement, the individual samples may be
mixed and the average tested; where time will permit, however, it
is recommended that they be tested separately.
4. — Method of Sampling. — Cement in barrels should be sampled
through a hole made in the center of one of the staves, midway
between the heads, or in the head, by means of an auger or a sampling
iron similar to that used by sugar inspectors. If in bags, it should
be taken from surface to center
CHEMICAL ANALYSIS.
5. — Significance. — Chemical analysis may render valuable
service in the detection of adulteration of cement with considerable
amounts of inert material, such as slag or ground limestone. It is
of use, also, in determining whether certain constituents, believed
to be harmful when in excess of a certain percentage, as magnesia
and sulphuric anhydride, are present in inadmissible proportions.
6. — The determination of the principal constituents of cement
— silica, alumina, iron oxide and lime — is not conclusive as an in-
dication of quality. Faulty character of cement results more fre-
quently from imperfect preparation of the raw material or defective
burning than from incorrect proportions of the constituents. Cement
made from very finely-ground material, and thoroughly burned, may
contain much more lime than the amount usually present, and still
be perfectly sound. On the other hand, cements low in lime may,
on account of careless preparation of the raw material, be of danger-
ous character. Further, the ash of the fuel used in burning may
so greatly modify the composition of the product as largely to de-
stroy the significance of the results of analysis.
7. — Method. — As a method to be followed for the analysis of
cement, that proposed by the Committee on Uniformity in the
Analysis of Materials for the Portland Cement Industry, of the
New York Section of the Society for Chemical Industry, and pub-
lished in Engineering News, Vol. 50, p. 60, 1903; and in The Engineer-
ing Record, Vol. 48, p. 49, 1903, is recommended.
n8
APPENDIX
SPECIFIC GRAVITY.
8. — Significance. — The specific gravity of cement is lowered by
adulteration and hydration, but the adulteration must be in con-
siderable quantity to affect the results appreciably.
9. — Inasmuch as the differences in specific gravity are usually
very small, great care must be exercised in making the determina-
tion.
10. — Apparatus and Methqd. — The determination of specific
gravity is most conveniently 'made with Le Chatelier's apparatus.
I
FIG. i.
This consists of a flask (D), Fig. i, of 120 cu. cm. (7.32 cu. in.)
capacity, the neck of which is about 20 cm. (7.87 in.) long; in the
middle of this neck is a bulb (C), above and below which are two
marks (F) and (£); the volume between these marks is 20 cu. cm.
(1.22 cu. in.). The neck has a diameter of about 9 mm. (0.35 in.),
and is graduated into tenths of cubic centimeters above the mark
(F).
11. — Benzine (62° Baume naphtha), or kerosene free from water,
should be used in making the determination.
12. — The specific gravity is determined as follows:
The flask is filled with either of these liquids to the lower mark
(£), and 64 gms. (2.25 oz.) of powder, cooled to the temperature of
APPENDIX IIQ
the liquid, is gradually introduced through the funnel (B) [the stem
of which extends into the flask at the top of the bulb (C)], until all
the powder is introduced, and the level of the liquid rises to some
division of the graduated neck. This reading plus 20 cu. cm. is the
volume displaced by 64 gms. of the powder.
13. — The specific gravity is then obtained from the formula:
Weight of Cement, in grams
Specific Gravity =
Displaced Volume, in cubic centimeters
14. — The flask, during the operation, is kept immersed in water
in a jar (^4), in order to avoid variations in the temperature of the
liquid. The results should agree within o.oi. The determination
of specific gravity should be made on the cement as received; and,
should it fall below 3.10, a second determination should be made on
the sample ignited at a low red heat.
15. — A convenient method for cleaning the apparatus is as
follows: The flask is inverted over a large vessel, preferably a glass
jar, and shaken vertically until the liquid starts to flow freely; it
is then held still in a vertical position until empty; the remaining
traces of cement can be removed in a similar manner by pouring
into the flask a small quantity of clean liquid benzine or kerosene
and repeating the operation.
FINENESS.
16. — Significance. — It is generally accepted that the coarser
particles in cement are practically inert, and it is only the extremely
fine powder that possesses adhesive or cementing qualities. The
more finely cement is pulverized, all other conditions being the
same, the more sand it will carry and produce a mortar of a given
strength.
17. — The degree of final pulverization which the cement re-
ceives at the place of manufacture is ascertained by measuring the
residue retained on certain sieves. Those known as the No. 100
and No. 200 sieves are recommended for this purpose.
18. — Apparatus. — The sieves should be circular, about 20 cm.
(7.87 in.) in diameter, 6 cm. (2.36 in.) high, and provided with a
pan, 5 cm. (1.97 in.) deep, and a cover.
120 APPENDIX
19. — The wire cloth should be of brass wire having the following
diameters:
No. 100, 0.0045 m-5 No. 200, 0.0024 in.
20. — This cloth should be mounted on the frames without dis-
tortion; the mesh should be regular in spacing and be within the
following limits:
No. 100, 96 to 100 meshes to the linear inch.
No. 200, 188 to 200 meshes to the linear inch.
21. — Fifty grams (1.76 oz.) or 100 g. (3.52 oz.) should be used
for the test, and dried at a temperature of 100° Cent. (2i2°Fahr.)
prior to sieving, tj
22. — Method. — The thoroughly dried and coarsely screened
sample is weighed and placed on the No. 200 sieve, which, with pan
and cover attached, is held in one hand in a slightly inclined posi-
tion, and moved forward and backward, at the same time striking
the side gently with the palm of the other hand, at the rate of about
200 strokes per minute. The operation is continued until not more
than one-tenth of i per cent passes through after one minute of con-
tinuous sieving. The residue is weighed, then placed on the No. 100
sieve and the operation repeated. The work may be expedited by
placing in the sieve a small quantity of large steel shot. The results
should be reported to the nearest tenth of i per cent.
NORMAL CONSISTENCY.
23. — Significance. — The use of a proper percentage of water in
making the pastes * from which pats, tests of setting, and briquettes
are made, is exceedingly important, and affects vitally the results
obtained.
24. — The determination consists in measuring the amount of
water required to reduce the cement to a given state of plasticity,
or to what is usually, designated the normal consistency.
25. — The Committee recommends the following method for
determining normal consistency.
*The term "paste" is used in this report to designate a mixture of
cement and water, and the word "mortar" a mixture of cement, sand and
water.
APPENDIX
121
26. — Method, Vicat Needle Apparatus. — This consists of a
frame (1C), Fig. 2, bearing a movable rod (£,), with the cap (A) at
one end, and at the other the cylinder (B), i cm. (0.39 in.) in diam-
eter, the cap, rod, and cylinder weighing 300 gms. (10.58 oz.). The
rod, which can be held in any desired position by a screw (F), car-
ries an indicator, which moves over a scale (graduated to centi-
meters) attached to the frame (K). The paste is held by a conical,
hard-rubber ring (7), 7 cm. (2.76 in.) in diameter at the base, 4 cm.
(1.57 in.) high, resting on a glass plate (7), about 10 cm. (3.94 in.)
square.
D D
ma
A
VICAT NEEDLE.
FlG. 2.
27. — In making the determination, the same quantity of cement
as will be subsequently used for each batch in making the briquettes,
but not less than 500 gms., is kneaded into a paste, as described in
Paragraph 52, and quickly formed into a ball with the hands, com-
pleting the operation by tossing it six times from one hand to the
other, maintained 6 in. apart; the ball is then pressed into the rubber
ring, through the larger opening, smoothed off, and placed (on its
large end) on a glass plate and the smaller end smoothed off with
a trowel; the paste, confined in the ring, resting on the plate, is
placed under the rod bearing the cylinder, which is brought in con-
tact with the surface and quickly released.
122
APPENDIX
28. — The paste is of normal consistency when the cylinder in
one minute from the time it is released penetrates to a point in the
mass 10 mm. (0.39 in.) below the top of the ring. Great care must
be taken to fill the ring exactly to the top. The apparatus must be
free from all vibrations during the test.
29. — The trial pastes are made with varying percentages of
water until the correct consistency is obtained.
30. — The Committee has recommended, as normal, a paste, the
consistency of which is rather wet, because it believes that variations
in the amount of compression to which the briquette is subjected in
moulding are likely to be less with such a paste.
31. — Having determined in this manner the proper percentage
of water required to produce a paste of normal consistency, the
proper percentage required for the mortars is obtained from the
table below.
PERCENTAGE OF WATER FOR STANDARD MORTARS
One cement,
One cement,
One cement,
Neat.
three standard
Neat.
three standard
Neat.
three standard
Ottawa sand.
Ottawa sand.
Ottawa sand.
is
8.0
23
9-3
31
10.7
16
8.2
24
9-5
32
10.8
17
8.3
25
9-7
33
II .0
18
8.5
26
9.8
34
II .2
iQ
8.7
27
10. O
35
"•5
20
8.8
28
10. 2
36
n-5
21
9.0
29
10.3
37
ii. 7
22
9.2
30
io-5
38
ii. 8
TIME OF SETTING.
32. — Significance. — The object of this test is to determine the
time which elapses from the moment water is added until the paste
ceases to be fluid and plastic (called the "initial set"), and also the
time required for it to acquire a certain degree of hardness (called
the "final" or "hard set"). The former of these is the more im-
portant, since, with the commencement of setting, the process of
crystallization or hardening is said to begin. As a disturbance of
this process may produce a loss of strength, it is desirable to com-
APPENDIX 123
plete the operation of mixing and moulding or incorporating the
mortar into the work before the cement begins to set.
33. — It is usual to measure arbitrarily the beginning and end
of the setting by the penetration of weighted wires of given di-
ameters.
34. — Method. — For this purpose the Vicat Needle, which has
already been described in Paragraph 26, should be used.
35. — In making the test, a paste of normal consistency is
molded and placed under the rod (Z,), Fig. 2, as described in Para-
graph 27; this rod, bearing the cap (D) at one end and the needle
(H), i mm. (0.039 mO m diameter, at the other, weighing 300 gms.
(10.58 oz.). The needle is then carefully brought in contact with
the surface of the paste and quickly released.
36. — The setting is said to have commenced when the needle
ceases to pass a point 5 mm. (0.20 in.) above the upper surface of
the glass plate, and is said to have terminated the moment the needle
does not sink visibly into the mass.
37. — The test pieces should be stored in moist air during the
test; this is accomplished by placing them on a rack over water con-
tained in a pan and covered with a damp cloth, the cloth to be kept
away from them by means of a wire screen; or they may be stored
in a moist box or closet.
38. — Care should be taken to keep the needle clean, as the collec-
tion of cement on the sides of the needle retards the penetration,
while cement on the point reduces the area and tends to increase the
penetration.
39. — The determination of the time of setting is only approxi-
mate, being materially affected by the temperature of the mixing
water, the temperature and humidity of the air during the test, the
percentage of water used, and the amount of kneading the paste
receives.
STANDARD SAND.
40. — The Committee recommends the natural sand from Ottawa,
111., screened to pass a sieve having 20 meshes per linear inch and
retained on a sieve having 30 meshes per linear inch; the wires to
have diameters of 0.0165 and 0.0112 in., respectively, i.e., half the
width of the opening in each case. Sand having passed the No. 20
124
APPENDIX
sieve shall be considered standard when not more than i per cent
passes a No. 30 sieve after one minute's continuous sifting of a 5oo-g
sample.*
FORM OF TEST PIECES.
41. — For tension tests the Committee recommends the form of
test piece shown in Fig. 3.
DETAILS FOR BRIQUETTE.
FlG. 3.
42. — For compression tests a 2-in. cube is recommended.
MOLDS.
43. — The molds should be made of brass, bronze, or some equally
non-corrodible material, having sufficient metal in the sides to pre-
vent spreading during molding.
44. — Gang molds, which permit molding a number of briquettes
at one time, are preferred by many to single molds; since the
*This sand may be obtained from the Ottawa Silica Company at a
cost of two cents per pound, f. o. b. cars, Ottawa, Illinois.
APPENDIX 125
greater quantity of mortar that can be mixed tends to produce
greater uniformity in the results. The type shown in Fig. 4 is
recommended.
DETAILS FOR GANG MOULD.
FIG. 4.
45. — The molds should be wiped with an oily cloth before using.
MIXING.
46. — All proportions should be stated by weight; the quantity of
water to be used should be stated as a percentage of the dry material.
47. — The metric system is recommended because of the con-
venient relation of the gram and the cubic centimeter.
48. — The temperature of the room and the mixing water should
be as near 21° Cent. (70° Fahr.) as it is practicable to maintain it.
49. — The sand and cement should be thoroughly mixed dry.
The mixing should be done on some non-absorbing surface, prefer-
ably plate glass. If the mixing must be done on an absorbing sur-
face it should be thoroughly dampened prior to use.
50. — The quantity of material to be mixed at one time de-
pends on the number of test pieces to be made; about 1,000 gms.
(35.28oz.) makes a convenient quantity to mix, especially by hand
methods.
51. — The Committee, after investigation of the various mechan-
ical mixing machines, has decided not to recommend any machine
that has thus far been devised, for the following reasons:
(i) The tendency of most cement is to "ball up" in the machine^
thereby preventing the working of it into a homogeneous paste;
(2) there is no means of ascertaining when the mixing is complete
without stopping the machine; and (3) the difficulty of keeping the
machine clean.
52. — Method. — The material is weighed and placed on the mix-
ing table, and a crater formed in the center, into which the proper
percentage of clean water is poured; the material on the outer edge
126 APPENDIX
is turned into the crater by the aid of a trowel. As soon as the
water has been absorbed, which should not require more than one
minute, the operation is completed by vigorously kneading with the
hands for an additional one minute, the process being similar to that
used in kneading dough. A sand-glass affords a convenient guide
for the time of kneading. During the operation of mixing, the
hands should be protected by gloves, preferably of rubber.
MOLDING.
53. — Having worked the paste or mortar to the proper consist-
ency, it is at once placed in the molds by hand.
54. — The Committee has been unable to secure satisfactory re-
sults with the present molding machines; the operation of machine
moulding is very slow, and the present types permit of molding
but one briquette at a time, and are not practicable with the pastes
or mortars herein recommended.
55. — Method. — The molds should be filled immediately after
the mixing is completed, the material pressed in firmly with the
fingers and smoothed off with a trowel without mechanical ramming;
the material should be heaped up on the upper surface of the mold,
and, in smoothing off, the trowel should be drawn over the mold
in such a manner as to exert a moderate pressure on the excess
material. The mold should be turned over and the operation
repeated.
56. — A check upon the uniformity of the mixing and molding
is afforded by weighing the briquettes just prior to immersion, or
upon removal from the moist closet. Briquettes which vary in
weight more than 3 per cent from the average should not be tested.
STORAGE or THE TEST PIECES.
57. — During the first 24 hours after molding, the test pieces
should be kept in moist air to prevent them from drying out.
58. — A moist closet or chamber is so easily devised that the use
of the damp cloth should be abandoned. Covering the test pieces
with a damp cloth is objectionable, as commonly used, because the
cloth may dry out unequally, and, in consequence, the test pieces are
not all maintained under the same condition. Where a moist closet
APPENDIX
127
is not available, a cloth may be used and kept uniformly wet by
immersing the ends in water. It should be kept from direct contact
with the test pieces by means of a wire screen or some similar
arrangement.
59. — A moist closet consists of a soapstone or slate box, or a
metal-lined wooden box — the metal lining being covered with felt
and this felt kept wet. The bottom of the box is so constructed as
to hold water, and the sides are provided with cleats for holding
glass shelves on which to place the briquettes. Care should be
taken to keep the air in the closet uniformly moist.
60. — After 24 hours in moist air, the test pieces for longer
periods of time should be immersed in water maintained as near
21° Cent. (70° Fahr.) as practicable; they may be stored in tanks or
pans, which should be of non-corrodible material.
TENSILE STRENGTH.
61. — The tests may be made on any machine. A solid metal
clip, as shown in Fig. 5, is recommended. This clip is to be used
without cushioning at the points of contact with
the test specimen. The bearing at each point of
contact should be | in. wide and the distance
between the center of contact on the same clip
should be i^ in.
62. — Test pieces should be broken as soon as
they are removed from the water. Care should
be observed in centering the briquettes in the
testing machine, as cross-strains, produced by
improper centering, tend to lower the breaking
strength. The load should not be applied too
suddenly, as it may produce vibration, the shock
from which often breaks the briquettes before
the ultimate strength is reached. Care must
be taken that the clips and the sides of the
briquette be clean and free from grains of sand
or dirt, which would prevent a good bearing. The load should be
applied at the rate of 600 Ib. per min. The average of the bri-
quettes of each sample tested should be taken as the test, excluding
any results which are manifestly faulty.
3
FORM OF CLIR
FIG. 5.
128 APPENDIX
CONSTANCY OF VOLUME.
63. — Significance. — The object is to develop those qualities
which tend to destroy the strength and durability of a cement. As
it is highly essential to determine such qualities at once, tests of this
character are for the most part made in a very short time, and are
known, therefore, as accelerated tests. Failure is revealed by crack-
ing, checking, swelling, or disintegration, or all of these phenomena.
A cement which remains perfectly sound is said to be of constant
volume.
64. — Methods. — Tests for constancy of volume are divided into
two classes: (i) normal tests, or those made in either air or water
maintained at about 21° Cent. (70° Fahr.), and (2) accelerated tests,
or those made in air, steam, or water at a temperature of 45° Cent.
(113° Fahr.) and upward. The test pieces should be allowed to
remain 24 hours in moist air before immersion in water or steam,
or preservation in air.
65. — For these tests, pats, about 7^ cm. (2.95 in.) in diameter,
i£ cm. (0.49 in.) thick at the center, and tapering to a thin edge,
should be made, upon a clean glass plate [about 10 cm. (3.94 in.)
square], from cement paste of normal consistency.
66. — Normal Test. — A pat is immersed in water maintained as
near 21° Cent. (70° Fahr.) as possible for 28 days, and observed at
intervals. A similar pat, after 24 hours in moist air, is maintained
in air at ordinary temperature and observed at intervals.
67. — Accelerated Tests. — A pat is placed in an atmosphere of
steam upon a wire screen i in. above boiling water for five (5) hours.
The apparatus should be so constructed as to permit the free escape
of steam and maintain atmospheric pressure. Since the type of
apparatus used has a great influence on the uniformity of the results,
that shown in Fig. 8 is recommended.
68. — To pass these tests satisfactorily, the pats should remain firm
and hard, and show no signs of cracking, distortion or disintegration.
69. — Should the pat leave the plate, distortion may be detected
best with a straight-edge applied to the surface which was in contact
with the plate.
70. — In the present state of our knowledge it cannot be said
that cement should necessarily be condemmed simply for failure to
APPENDIX
129
330 APPENDIX
pass the accelerated tests; nor can a cement be considered entirely
satisfactory simply because it has passed these tests.
Submitted on behalf of the Committee,
GEORGE S. WEBSTER,
Chairman.
RICHARD L. HUMPHREY,
Secretary.
JANUARY iSxn, 1911.
Committee.
GEORGE S. WEBSTER,
RICHARD L. HUMPHREY,
GEORGE F. SWAIN,
ALFRED NOBLE,
Louis C. SABIN,
S. B. NEWBERRY,
CLIFFORD RICHARDSON,
W. B. W. HOWE,
F. H. LEWIS.
NEW YORK SECTION SOCIETY FOR CHEMICAL INDUSTRY
Method Suggested for the Analysis of Limestones, Raw Mixtures and
Portland Cements by the Committee on Uniformity in Techni-
cal Analysis with the Advice of W. F. Hillebrand.
SOLUTION.
One-half gram of the finely-powdered substance is to be weighed
out and, if a limestone or unburned mixture, strongly ignited in a
covered platinum crucible over a strong blast for fifteen minutes, or
longer if the blast is not powerful enough to effect complete conver-
sion to a cement in this time. It is then transferred to an evaporating
dish, preferably a platinum for the sake of celerity in evapora-
tion, moistened with enough water to prevent lumping, and 5 to
10 c.c. of strong HC1 added and digested with the aid of gentle heat
and agitation until solution is complete. Solution may be aided by
APPENDIX 131
light pressure with the flattened end of a glass rod.* The solution
is then evaporated to dryness, as far as this may be possible on the
bath.
SILICA (SiO2).
The residue without further heating is treated at first with 5 to
10 c.c. of strong HC1, which is then diluted to half strength or less,
or upon the residue may be poured at once a larger volume of acid
of half strength. The dish is then covered and digestion allowed to
go on for 10 minutes on the bath, after which the solution is filtered
and the separated silica washed thoroughly with water. The filtrate
is again evaporated to dryness, the residue without further heating
taken up with acid and water and the small amount of silica it con-
tains separated on another filter paper. The papers containing the
residue are transferred wet to a weighed platinum crucible, dried,
ignited, first over a Bunsen burner until the carbon of the filter is
completely consumed, and finally over the blast for 15 minutes and
checked by a further blasting for 10 minutes or to constant weight.
The silica, if great accuracy is desired, is treated in the crucible with
about 10 c.c. of HF and four drops of H2SO4 and evaporated over
a low flame to complete dryness. The small residue is finally blasted,
for a minute or two, cooled and weighed. The difference between
this weight and the weight previously obtained gives the amount
of silica.f
ALUMINA AND IRON (A12O3 AND Fe2O3).
The filtrate, about 250 c.c., from the second evaporation for
Si02, is made alkaline with NH4OH after adding HC1, if need be,
to insure a total of 10 to 15 c.c. strong acid, and boiled to expel
excess of NH3, or until there is but a faint odor of it, and the pre-
cipitated iron and aluminum hydrates, after settling, are washed once
by decantatkm and slightly on the filter. Setting aside the filtrate,
* If anything remains undecomposed it should be separated, fused with
a little Na2CO3, dissolved and added to the original solution. Of course a
small amount of separated non-gelatinous silica is not to be mistaken for
undecomposed matter.
t For ordinary control in the plant laboratory this correction may,
perhaps, be neglected; the double evaporation never.
132 APPENDIX
the precipitate is dissolved in hot dilute HC1, the solution passing
into the beaker in which the precipitation was made. The-aluminum
and iron are then reprecipitated by NH4OH, boiled and the second
precipitate collected and washed on the same filter used in the first
instance. The filter paper, with the precipitate, is then placed in a
weighed platinum crucible, the paper burned off and the precipitate
ignited and finally blasted 5 minutes, with care to prevent reduction,
cooled and weighed as A12C>3 + Fe2C>3.*
IRON (Fe203).
The combined iron and aluminum oxides are fused in a platinum
crucible at a very low temperature with about 3 to 4 grams of
KHSO4, or, better, NaHSO4, the melt taken up with so much dilute
H2SO4 that there shall be no less than 5 grams absolute acid and
enough water to effect solution on heating. The solution is then
evaporated and eventually heated till acid fumes come off copiously.
After cooling and redissolving in water the small amount of silica is
filtered out, weighed and corrected by HF and H2SO4.f The filtrate
is reduced by zinc, or preferably by hydrogen sulphide, boiling out
the excess of the latter afterwards while passing CO2 through the
flask, and titrated with permanganate. J The strength of the per-
manganate solution should not be greater than .0040 grm. Fe2Os
per c.c.
LIME (CaO).
To the combined filtrate from the A12O3 -f Fe2O3 precipitate a
few drops of NH4OH are added, and the solution brought to boil-
ing. To the boiling solution 20 c.c. of a saturated solution of
ammonium oxalate are added, and the boiling continued until the
precipitated CaC2O4 assumes a well-defined granular form. It is
then allowed to stand for 20 minutes, or until the precipitate has
* This precipitate contains TiO2, P2Os, Mn3O4.
t This correction of A12O3 Fe2O3 for silica should not be made when the
HF correction of the main silica has been omitted, unless that silica was
obtained by only one evaporation and filtration. After two evaporations
and nitrations i to 2 mg. of SiO2 are still to be found with the A^Os Fe2Oa.
| In this way only is the influence of titanium to be avoided and a cor-
rect result obtained for iron.
APPENDIX 133
settled, and then filtered and washed. The precipitate and filter are
placed wet in a platinum crucible, and the paper burned off over a
small flame of a Bunsen burner. It is then ignited, redissolved in
HC1, and the solution made up to 100 c.c. with water. Ammonia
is added in slight excess, and the liquid is boiled. If a small amount
of A12O3 separates, this is filtered out, weighed, and the amount
added to that found in the first determination, when greater accu-
racy is desired. The lime is then reprecipitated by ammonium oxa-
late, allowed to stand until settled, filtered, and washed,* weighed as
oxide by ignition and blasted in a covered crucible to constant
weight, or determined with dilute standard permanganate.!
MAGNESIA (MgO).
The combined filtrates from the calcium precipitates are acidi-
fied with HC1 and concentrated on the steam bath to about 150 c.c.,
10 c.c. of saturated solution of Na(NH4)HPO4 are added, and the
solution boiled for several minutes. It is then removed from the
flame and cooled by placing the beaker in ice water. After cooling,
NH4OH is added drop by drop with constant stirring until the crys-
talline ammonium-magnesium ortho-phosphate begins to form, and
then in moderate excess, the stirring being continued for several
minutes. It is then set aside for several hours in a cool atmosphere
and filtered. The precipitate is redissolved in hot dilute HC1, the
solution made up to about 100 c.c., i c.c. of a saturated solution of
Na(NH4)HP04 added, and ammonia drop by drop, with constant
stirring, until the precipitate is again formed as described and the
ammonia is in moderate excess. It is then allowed to stand for
about 2 hours, when it is filtered on a paper or a Gooch crucible,
ignited, cooled and weighed as Mg2P2O7.
ALKALIES (K2O AND Na20).
For the determination of the alkalies, the well-known method
of Prof. J. Lawrence Smith is to be followed, either with or without
the addition of CaCO3 with NI^Cl.
* The volume of wash- water should not be too large; vide Hillebrand.
t The accuracy of this method admits of criticism, but its convenience
and rapidity demand its insertion.
134 APPENDIX
ANHYDROUS SULPHURIC ACID (S03).
One gram of the substance is dissolved in 15 c.c. of HC1, filtered
and residue washed thoroughly.*
The solution is made up, to 250 c.c. in a beaker and boiled. To
the boiling solution 10 c.c. of a saturated solution of BaQ2 is added
slowly drop by drop from a pipette and the boiling continued until
the precipitate is well formed, or digestion on the steam bath may
be substituted for the boiling. It is then set aside over night, or for
a few hours, filtered, ignited and weighed as BaS04.
TOTAL SULPHUR.
One gram of the material is weighed out in a large platinum cru-
cible and fused with Na2C03 and a little KNO3, being careful to
avoid contamination from sulphur in the gases from source of heat.
This may be done by fitting the crucible in a hole in an asbestos
board. The melt is treated in the crucible with boiling water and
the liquid poured into a tall narrow beaker and more hot water
added until the mass is disintegrated. The solution is then filtered.
The filtrate contained in a No. 4 beaker is to be acidulated with
HC1 and made up to 250 c.c. with distilled water, boiled, the sul-
phur precipitated as BaSO4 and allowed to stand over night or for
a few hours.
Loss ON IGNITION.
Half a gram of cement is to be weighed out in a platinum cru-
cible, placed in a hole in an asbestos board so that about | of the
crucible projects below, and blasted 15 minutes, preferably with an
inclined flame. The loss by weight, which is checked by a second
blasting of 5 minutes, is the loss on ignition.
May, 1903: Recent investigations have shown that large errors
in results are often due to the use of impure distilled water and
reagents. The analyst should, therefore, test his distilled water by
evaporation and his reagents by appropriate tests before proceeding
with his work.
* Evaporation to dryness is unnecessary, unless gelatinous silica should
have separated, and should never be performed on a bath heated by gas;
vide Hillebrand.
INDEX.
Aging, 33.
Alkalies, 4.
determination of, 97.
Alkali waste, 5.
Alumina, 3.
determination of, 91.
Analyses of cements, typical, 5.
chemical, 80.
Appendix, in.
Beam molds, 43, 78.
Beams, breaking of, 44.
Boiling test apparatus, 75.
Briquette molds, 34, 78.
Briquettes, breaking of, 37.
mortar, 36.
Burette, 78.
Lesley, 78.
Carbonic acid, 4.
Carbon dioxide, direct method for
determination of, 103.
indirect method for determination
of, 101.
Cement, chemical analysis of, 84.
classification of, i.
definition of, i.
rock, 5.
specific gravity of, 14.
typical analyses of, 5.
Chalk, 6.
Chemical analysis, 80.
factors influencing, 82.
sample for, 83.
Classification of -cements, i.
•Clay, 5.
analysis of, 107.
Clips, 70.
Composition of cement, i, 33.
Compression tool, 70.
Compressive strength, 41.
determination of, 42.
report blanks, 46, 47.
Constancy of volume, 28.
determination of, 29.
report blank, 32.
Constant level apparatus, 75.
Cube molds, 42, 78.
Cubes, breaking of, 43.
D
Definition of cement, i.
Effective size of sand, 52.
Fairbanks machine, 63.
operation of, 64.
Falkenau-Sinclair machine, 64.
operation of, 66.
Fineness, 9, 34.
determination of, n.
importance of, 9.
report blank, 13.
Inspection, 7.
Iron and Alumina, determination
of, 87.
135
i36
INDEX
Iron, determination of, 88.
reduction of, by H^S, 91.
reduction of, by zinc, 89, 90.
Iron oxide, 3.
J
Jones reductor, 90.
Laboratory equipment, 63.
Le Chatelier flask, 15.
Lesley burette, 78.
storage tank, 77.
Lime, 3.
determination of, 92.
Limestone, 6.
analysis of, 106.
Loam in sand, determination of, 49.
Loss on ignition, determination of,
84.
M
Machines, for compression tests, 72.
for tension tests, 63.
Magnesia, 4.
determination of, 93.
Manufacture of cement, 5.
Marl, 5.
analysis of, 107.
Mechanical analysis, of sand, 50.
of stone, 54.
Mixed cement, 2.
Mixing, 21.
Modulus of rupture, calculation of,
44-
determination of, 43.
report blank, 48.
Moist closet, 76.
Moisture, determination of, 96.
Molds, beam, 43, 78.
briquette, 34, 78.
cube, 42, 78.
Mortar briquettes, 36.
N
Natural cement, i, 4.
Normal consistency, 20.
determination of, 22.
report blank, 26.
O
Olsen briquette machine, 63, 64.
operation of, 66.
Olsen hydraulic compression ma-
chine, 72.
Pats, preparation of, 29.
Portland cement, i.
Potash, determination of, 99.
Pozzuolana cement, 2, 4.
R
Raw material, 5.
Riehle machine, 63, 64.
operation of, 66.
Sampling, 7, 83.
auger, 8.
Sand, 49.
determination of loam in, 49.
mechanical analysis of, 50.
report blank, 60.
percentage of loam report blank,
59-
sifter, 74.
specific gravity of, report blank,
61.
standard, 49.
weight per cubic foot of, report
blank, 61.
Scales, n, 75.
Set, time of, 23.
Shot machines, 63.
Sieves, 10.
INDEX
137
Sifter, sand, 74.
Silica, 3.
determination of, 85.
Slag, analysis of, 107.
Soda, determination of, 100.
Specific gravity of cement, 14.
determination of, 16.
report blank, 19.
significance of, 14.
Standard specifications, in.
Stone, 54.
mechanical analysis of, 54.
specific gravity of, 55.
report blank, 61.
weight per cubic foot of, report
' blank, 62.
Storage, 7.
tanks, 76.
Lesley, 77.
Sulphur, 4.
as sulphide, 96.
determination of, 94.
Sulphuric acid, 4.
determination of, 93.
Sulphur trioxide, 4.
Table, 77.
Tensile strength, 33.
determination of, mortar, 36.
determination of, neat cement, 34.
Tensile strength, factors affecting.
33-
report blanks, 39, 40.
Testing machines, 63.
Tests, accelerated, 29.
normal, 28.
transverse, 43.
Time of set, 23.
determination of, 24.
factors affecting, 24.
report blank, 27.
significance of, 23.
Tool, compression, 70.
Transverse test attachment, 70.
U
Uniformity coefficient, 52.
Universal testing machine, 72.
Unsoundness, causes of, 28.
Vicat apparatus, 20.
Voids in sand, 52.
determination of, 52.
Voids in stone, 55.
determination of, 56, 57.
W
Weight per cubic foot of sand, 54.
of stone, 56.
Work table, 77.
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