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Full text of "Practical flavoring extract maker, a treatise on the manufacture of the principal flavoring extracts, in accordance with the reqiurements of the food laws of the United States"

Practical 

Flavoring Extract 
Maker 



By 

E. J. JCESSLER 

A TREATISE ON THE MANU- 
FACTURE OF THE PRIN- 
CIPAL FLAVORING EX- 
TRACTS, IN ACCORDANCE 
WITH THE REQUIREMENTS 
OF THE FOOD LAWS OF 
THE UNITED STATES ; 
WRITTEN BY A PRACTI- 
CAL MANUFACTURER WHO 
SETS DOWN THE FULL 
KNOWLEDGE OF HIS 5 SFE-' 
CIALTY ACQUIRED DURING 
MANY YEARS OF CONTIN- 
UOUS EXPERIENCES''"' 



1912 
The Spice Mill Publishing Co. 

NEW YORK 



COPYRIGHT, 1912 BY 
THE SPICE MILL PUBLISHING Co. 

NEW YORK 



Main Lib. 

AGRIC, 




DtPt. ^^ 



Table of Contents 



GENERAL OBSERVATIONS .... 6 

QUALIFICATIONS OF A MANUFACTURER . . 7 

WHAT CONSTITUTES A FLAVORING EXTRACT . 8 

MANUFACTURE OF VANILLA EXTRACTS 

Description of Varieties of Vanilla Beans 
Resins Selecting Beans Bean Storage Cut- 
ting Beans Exhaustion of the Vanilla Bean 
Tonka Extract Imitation Vanilla Extracts 
Non-Alcoholic Extracts Testing Vanilla 
Extracts ...... 10-31 

MANUFACTURE OF LEMON EXTRACTS 

Terpeneless Extract of Lemon Lemon 

Flavor, Imitation Extract of Orange . 32-41 

VARIOUS EXTRACTS 

Extracts of Almond, Wintergreen, Pepper- 
mint, Ginger, Rose, Allspice (Pimento), 
Anise, Celery, Cinnamon, Cassia, Cloves, 
Mint (Spearmint), Chocolate, Sarsaparilla 
(imitation), Pistachio (imitation) Ethereal 
imitation Flavors ..... 42-51 

LABORATORY NOTES 

Menstruums (solvents) Rules for Testing 
Alcohol, Oils, etc. Filtration Double Pres- 
sure Filter and Percolator Testing Methods 
Estimation of Small Quantities of Essential 
Oils To Determine per cent, of gas in Aqua- 
Ammonia, and per cent, of Acidity of Vinegar 
To Purify Essential Oils . . . 52-66 

MISCELLANEOUS RECEIPTS .... 67-69 

ADHESIVES 70 

WEIGHTS AND MEASURES, TABLES ... 71 

HOUSEHOLD AMMONIA .... 72 

BOTTLES AND CORKS . . . . . 73-76 

FIGURING COSTS 76-79 

INDEX 80-83 

443166 



General Observations 

PRIOR to the enactment of the State and Federal 
pure food laws, few classes of food products 
were so grossly adulterated as flavoring ex- 
tracts. Some of the compounds termed "ex- 
tract of vanilla" were manufactured at a cost 
of from 40 to 60 cents per gallon. This con- 
dition undoubtedly resulted from the ease with which 
substitutes that readily deceive the purchaser are pre- 
pared. The average manufacturer was by no means in- 
spired by the desire to adulterate ; in the majority of in- 
stances the causes of the decline in the quality of the 
extracts offered can be traced directly to the door of 
either the dealer or consumer, or both. In justice to the 
manufacturer, it may be stated that the rule of price 
regulating quality was generally observed. This rule, al- 
though holding good in the main, has its exceptions. 
The discussion, while not having a direct bearing on the 
manufacture of flavoring extracts, is of sufficient impor- 
tance, especially when the manufacturer is called upon to 
match goods offered by competitors; and in order to 
properly decide such problems, he should have a fair 
knowledge of the non-technical processes for conducting 
tests. 



QUALIFICATIONS OF A MANUFACTURER. 

The primary qualifications of an extract manufac- 
turer are embraced in an ordinary education, plus a 
liberal display of effort. One need not be a graduate 
chemist, although a knowledge of the fundamental prin- 
ciples of chemistry will prove a valuable aid. For the be- 
ginner, in the absence of a better opportunity, the writer 
will suggest that he study a chemical text book such as 
"Steele's Popular Chemistry." Too much importance 
cannot be attached to the necessity of familiarizing one's 
self with both the Federal and State food laws, and the 
author would suggest that one request from the Secre- 
tary of the United States Department of Agriculture the 
mailing to him of all printed matter having reference to 
the Federal Food Law requirements, including circular 
No. 19, "Standards of Purity for Food Products," and 
also to place his firm name on the mailing list for "No- 
tices of Judgment," the latest rulings, etc., and adhere 
to the Department's teachings religiously. The same 
course should be followed in respect to the State or 
States in which one's products are offered for sale. In 
the event of his inability to interpret the laws, it will be 
best to employ the services of a competent attorney. 

One should never entertain the idea that his particu- 
lar process or system is perfect and he should not forget 
that perfection is an impossibility and that true progress 
is from the less to the greater. It requires energy and 
push to make headway in the world, and since work is 
ordinarily the measure of success, an active, energetic 
and persevering man is sure to succeed. 



8 What Constitutes a Flavoring Extract 

WHAT CONSTITUTES A FLAVORING 
EXTRACT? 

The best definition is contained in Circular No. 19, of 
the United States Department of Agriculture, as follows : 

"A flavoring extract is a solution in ethly alcohol of 
proper strength of the sapid and odorous principles de- 
rived from an aromatic plant, or parts of the plant, with 
or without its coloring matter, and conforms in name to 
the plant used in its preparation." 

This definition excludes all preparations which are 
not solutions in alcohol and eliminates the various forms 
of flavored sugars which are quite extensively used 
abroad. 

Extracts are divided into four classes, as follows : 

1. Those obtained by maceration and percolation of 
beans, seeds, roots, leaves and fruit of the plants. 

2. Those obtained by soltuion of essential oils. 

3. Those obtained by solution of synthetics (imita- 
tions), such as vanillin, and coumerin tinctures. 

4. Those obtained by solution of compound esters 
(a compound ether derived from an oxygenated acid). 

First Class. The following extracts are included un- 
der the first class : Vanilla, Tonka, Ginger, Celery, etc. 

Second Class. Lemon extract ; Terpeneless lemon ex- 
tract; Orange extract; Terpeneless orange extract; Cin- 
namon extract ; Cassia extract ; Almond extract ; Pepper- 
mint extract; Wintergreen extract; Nutmeg extract; 
Rose extract ; Anise extract ; Celery extract ; and Thyme 
extract. 

Third Class. Under the third class are included ex- 
tracts as follows : Vanillin extract, the synthetic prin- 
ciple of the vanilla bean ; coumarin extract, the synthetic 
principle of the tonka bean ; imitation wintergreen ex- 



What Constitutes a Flavoring E^tiact _ o 

tract, methyl salicylate, the synthetic principle of oil of 
wintergreen; imitation almond, benzaldehyde, the syn- 
thetic principle of oil of bitter almonds ; imitation sassa- 
fras, safrol, the synthetic principle of oil of sassafras. 

Fourth Class. Under this class are included extracts 
as follows : Imitation pineapple, strawberry, banana, 
raspberry, apple, cherry and peach all ethereal products 
representing ethyl butyrate, amyl butyrate, ethyl for- 
mate, amyl acetate, ethyl acetate, and amyl valerinate, all 
blended in proportions to represent the various flavors 
desired. 



io ' .Manufacture of Vanilla Extracts 



VANILLA EXTRACTS 



VANILLA BEANS. 

The vanilla bean, being the source of the most im- 
portant and popular flavoring on the market, will first 
be considered. The bean-producing plant is a climbing 
parasite (the Vanilla planifolia of Andrews). It was 
first described by a Franciscan Friar in 1575, and at that 
time was supposed to be of great medicinal value. The 
bean is a native of Mexico, the West Indies, South Amer- 
ica, the Bourbon Isles (chiefly the Comores group), Re- 
union, Seychelle, Madagascar, and the East Indies. 

Vanilla beans on the market are of various kinds as 
to name and quality. We have the Mexican, Bourbon, 
imitation Mexican, Tahiti, Guatemala, Java, and'Vanillon 
or Wild Vanilla. In quality we find quoted: ordinary; 
fair; good; extra; split; cuts; broken lots of mixed 
lengths ; and powdered with 50 per cent, of sugar. Thus 
we have various grades, from which no one can fail to 
find his Jiking, either in price or quality. In England 
manufacturers use the Bourbon Beans almost exclusively, 
using the Seychelle variety, Seychelle being an English 
province. France naturally is very partial to the Bour- 
bons and Mexicans, while Germany is very partial to the 
Tahiti. The Germans do not make extract, but sell va- 
nilla beans by the piece, these pieces being boiled with the 
pudding, etc. ; the consequence is that the Germans want 
as many beans as possible for the price per pound, and 
they naturally purchase the Tahiti grade. 

The United States, among the nations, is by far the 



Description of Varieties of Vanilla Beans n 



largest consumer of vanilla beans, the two most popular 
grades being the Mexicans and Bourbons, although of 
late the Tahiti is being more extensively used in various 
blends. 



DESCRIPTION OF VARIETIES OF VANILLA 
BEANS. 

The first quality of Mexican beans occurs in pods of 
from 8 to 10 inches long, flattened, ^ to ^ inches in 
diameter, with the lower end slightly tapered, the upper 
end gradually tapering for about a quarter the length of 
the pod, and is usually curved and slightly twisted near 
the point. The color is dark brown, the pods plump, the 
surface rigid longitudinally and frequently containing an 
incrustation of fine crystals beginning at the ends, grad- 
ually extending ; when fresh, somewhat viscid, but always 
roughish to the touch. 

The Bourbon vanilla resembles the Mexican, but is 
scarcely so long in the tapering portions; is of a dark 
brown, almost black color; is not as firm as the Mexi- 
can ; has a smooth and waxy surface and frequently be- 
comes covered with a coating of needle-shaped crystals 
(vanillin) known as "frost." 

The Seychelles and Mauritius vanilla has the pods 
6 inches in length, not over % inch in width, and is 
characterized by the pale color, the faint odor and a 
smooth but not waxy surface. 

Guadeloupe vanilla is usually recognizable, when the 
bean is entire, by it being broad arid flattened, usually 
y 2 inch or more wide, slightly tapering at the lower end 
and, at the upper, sharply tapering an inch or so at the 
point. It has a reddish brown color and possesses an 



12 Manufacture of Vanilla Extracts 



inferior pungent odor. It is very pulpy, with a surface 
intermediate between the Bourbon and the Mexican, and 
has but few crystals. One variety of this vanilla, sold 
under the name of "Vanillons," possesses the odor of 
heliotrope and is used principally by perfumers and to- 
bacco manufacturers. 

Java vanilla, which is almost exclusively consumed 
in Holland, has a pod from 4 to 6 inches long, and has 
a flavor almost as fine as that of the Mexican bean and 
a much stronger odor. 

Tahiti vanilla (transplanted Mexicans) has its pods 
from 4 to 7 inches long, is flat, from ^ to l /2 inch 
wide, and has a slightly reddish brown color. Owing to 
the insufficient attention of the vanilla planters (mostly 
Chinese) of the Society Islands (Tahiti being the ship- 
ping port) to the curing of the beans and the indiscrim- 
inate sale of their entire crop without regard to maturity, 
the value of the Tahitian vanilla has been depreciating 
in the world's markets; however, since the vanilla laws, 
which went into effect April i, 1911, providing means 
for licensing the curers and a rigid inspection of the 
beans prior to shipment, the character of this grade of 
vanilla has been very materially improved and is being 
extensively employed in this country. Nearly all of the 
Tahiti vanilla is received at the port of San Francisco, 
Cal. 

An interesting incident in the growth of vanilla beans 
is the artificial pollenization of the flower. Originally 
the cultivators depended solely upon insects to transmit 
the pollen from blossom to blossom, the results being 
anything but satisfactory, since some of the vines were 
made to bear too many pods, while others too few, re- 
sulting in a loss in both quality and quantity of the fruit 
produced. 



Description of Varieties of Vanilla Beans 13 

To overcome this difficulty the planter pollenizes by 
hand, the operation being a simple one and accomplished 
by removing the pollen from the male flowers by means 
of a splinter of wood, about the size of a tooth pick, and 
placing small portions of the pollen in the female flowers. 
Since the flowers open during the night and close before 
midday, the work is performed in the early morning and 
is most successful if performed on the first day on which 
the flower blossoms. Flowers not successfully pollinated 
soon wither and fall. With this method the number of 
pods which each vine is maturing can be ascertained 
and controlled, according to its age and physical struc- 
ture. 

The fruit, as first picked, has no aroma, the vanillin 
during the process of curing being developed from the 
glucoside conferin in the interior of the fruit. When 
vanilla beans are left to ripen too long, the pods will 
split and deteriorate, and the beans are then either sold 
as "splits" or are mixed with other inferior goods and 
sold as "cuts." The sale of cuts permits of considerable 
sophistication, in that, frequently, such beans as Tahiti 
are found among the mixture. Beans that have been 
picked too early are likewise distinctly inferior. 

If vanilla beans, finely divided, be distilled with water, 
a turbid liquid passes, which becomes clear by agitation 
with sulphuric ether, which ether on evaporation yields 
crystals of vanillin. 

Vanilla beans, from which the vanillin has been re- 
moved by means of a solvent, are sometimes offered to 
the trade. The fraud is to be detected by the absence 
of the flavor and odor. Such beans, also beans of an 
inferior quality, are sometimes "improved" in appear- 
ance and in odor by the use of benzoic acid. 

For the detection of this fraud, the operator should 



14 Manufacture of Vanilla Extracts 



avail himself of the fact that while benzoic acid crystals 
are flattened and rhomboidal and generally lie upon the 
bean, those of vanillin are usually needle-shaped and 
stand out almost at right angles from the surface of the 
fruit. These indications are not always infallible, since 
the crystalline structure is influenced considerably by 
the temperature, humidity of the surrounding air, etc. 
To more accurately determine the character of the flat 
crystals, detach them with the aid of a knife point, place 
in a test tube, heat over a Bunsen burner, and, if com- 
posed of benzoic acid, the unmistakable irritating odor 
of benzoic acid may be detected. 

The absence of the crystalline coating on the vanilla 
beans is not necessarily an indication of inferiority, since 
high grade vanilla beans very frequently manifest an op- 
posite condition. The most important fragrant principle 
of the vanilla bean and true vanilla extract is vanillin 
(Methyprotocatechuic aldehyde), a crystalline compound, 
the beans containing from i to about 2^4 per cent. The 
practical value of a vanilla bean is not, by any means, to 
be determined by the per cent, of vanillin content, since 
it frequently occurs that the very finest beans will show 
the smallest vanillin content. Busse found the following 
percentages of vanillan : 

Mexican vanilla beans 1.69 to 1.86 

Bourbon vanilla beans 1.91 to 2.48 

Tahiti vanilla beans 2.00 

German African vanilla beans... 2.16 
Java vanilla beans 2.75 

RESINS. 

While vanillin is a most important constituent of 
vanilla beans, there are other substances, such as resins, 



Resins Selecting Vanilla Beans 15 



gums, etc., soluble in dilute alcohol, that contribute to 
the fragrance and value of the extract. It is from these 
resins and gums that the vanilla extract derives the 
greater portion of the dark brown color. Practically 
nothing at this time is known of the chemical constitu- 
ents of vanilla resins. Experience has amply proven that 
to extract these resins thoroughly, a menstruum of at 
least 50 per cent, by volume of alcohol is necessary. 

Vanilla resins are a valuable analytical index, demon- 
strating approximately if the correct portion of beans to 
menstruum has been employed, likewise if the latter was 
of sufficient strength and if the extracting process was 
thorough. 

According to Brooks, the amount of resin present in 
different beans is as follows : 

Per Cent. 

Mexican (whole) 1.47 

Mexican (cuts) 1.96 

Seychelle (Bourbon cured) 1.93 

Comoros (Nossi Bey) 1.96 

Comoros (short) 1.90 

Mexican and South American, equal parts . 2.56 

SELECTING BEANS. 

In purchasing vanilla beans it is almost a necessity 
to take them on trust as to quality. The question of 
length as an element of value appears now to be ignored 
by some of the larger buyers, on the principle that the 
mere length of the bean has no more to do with its flavor 
or flavoring qualities than the length or breadth of a 
man decides his mental or moral qualities ; but as station, 
culture and education all play their part in the forma- 
tion of character, so soil, climate and cultivation estab- 



16 Manufacture of Vanilla Extracts 



lish the quality of the fruit under consideration. To be 
candid, and speaking as a manufacturer, we need more 
knowledge on the relative value of this valuable fruit, 
since all that the average buyers are sure of in pur- 
chasing are the price, aroma and physical structure ; 
therefore, in buying vanilla beans one should try to deal 
with the most reliable concern of whom he has knowl- 
edge. 

The most practical method to pursue in purchasing 
beans would be as follows : When in the market for 
beans, request from your dealer or dealers quotations 
with samples, and on receipt of samples proceed to make 
up test batches with the aid of small test percolators, or 
by maceration with frequent agitation, being careful to 
employ the same relative quantity of beans and mens- 
truum strength and treatment in all tests under operation. 
A test of this character can be successfully conducted 
within a period of forty-eight hours. When completed, 
first carefully note the density of color ; next dealco- 
holize in a porcelain evaporating dish over a water bath ; 
remove, and when almost cool, determine character of 
aroma by the sense of smell, and when thoroughly cool, 
by the sense of taste. In this manner you will be in a 
position to determine the .relative values of the samples 
submitted. 

BEAN STORAGE. 

Beans that are not required for immediate use should 
be stored in a cool, dry store room and should be ex- 
amined from time to time to guard against the forma- 
tion of mold or other infection. Beans can be success- 
fully stored in their reduced (cut) state, provided they 
are incorporated with sufficient dilute alcohol (equal 
parts) or glycerin +o cover them, and kept in an air- 



Exhaustion of the Vanilla Bean 17 



tight container in a cool place ; but do not forget to note 
on the package the exact weight of the beans, also the 
amount of dilute alcohol or glycerin used, as then you 
will be enabled to determine your formula more correctly. 

CUTTING BEANS. 

Vanilla beans should always be cut, not ground, for 
the following reasons : Grinding, in every instance, is 
accompanied with a rise of temperature, and it is a 
proven fact that the heating of vanilla beans results in 
the decomposition of the greater portion of the highly 
flavored aldehydes. The several forms of "meat cutters" 
that are sometimes used rip and shred the beans, and, 
through friction, generate considerable heat, always at 
the expense of the loss of some of the active principles ; 
whereas, with the use of a suitable knife chopper, the 
beans can be and should be reduced to a fine powder 
the finer the better the extraction, minus the heat. Too 
much importance cannot be attached to this branch of the 
subject. There are on the market a number of machines 
adapted for this purpose, and they can be had in either 
hand or belted power drives from $12.00 (the American 
chopper, hotel size) upward. 

EXHAUSTION OF THE VANILLA BEAN. 

EXTRACTION. 

The process for the rapid and thorough exhaustion 
of the vanilla bean constitutes the principal feature in the 
successful operation on this popular and costly fruit, 
since the vanilla bean is generally conceded as ranking 
among the most difficult substances from which to ex- 
tract its soluble or active principles, especially by perco- 
lation alone. The formula to be fallowed or the partic- 



1 8 Manufacture of Vanilla Extracts 



ular process to be adopted does not appear to be of such 
importance as that the complete exhaustion of the bean 
be secured, the work be well done, whether by percola- 
tion, maceration, digestion or a combination of the three. 
The proper menstruum, of course, will be the one 
that intelligent experiment has amply demonstrated as 
the most perfect in exhausting and preserving the im- 
portant principles. Vanilla extract differs from most of 
the other important extracts in its source, being made 
direct from the aromatic substance in its crude or natural 
condition; also in that it does not depend on a volatile 
oil for its virtue. 

PERCOLATION. 

Percolation is the process whereby a finely divided 
fruit or drug is deprived of its soluble constituents by 
the descent of a liquid (menstruum) through it, the oper- 
ation also embracing the process of straining and filtra- 
tion. Percolation is admirably adapted to a large number 




Exhaustion of the Vanilla Bean 19 



of drugs, but is not suitable in the manufacture of vanilla 
extract, for the following reasons: Slow operation, 
which must not exceed fifty drops per minute ; excessive 
losses in alcoholic evaporation, ranging from 10 to 15 
per cent.; incomplete exhaustion of the beans, since any 
irregular particles will tend to form an heterogeneous 
mass, offering a higher resistance to the flow of the 
menstruum than the coarser particles ; and the beans, 
being of a semi-soft character, when placed in the per- 
colator, have the tendency of conforming into packed 
masses of unequal resistances, resulting in the flow fol- 
lowing the course of least resistance, with the consequent 
losses from incomplete exhaustion. See Fig. on opposite 
page (glass percolator.) 

MACERATION. 

The process of maceration consists of exposing the 
finely reduced beans in the menstruum until they are 
thoroughly penetrated and the soluble or active princi- 
ples are dissolved. The usual method is to introduce the 
beans into an air-tight container ; agitate frequently dur- 
ing four to six months, decant the clear liquid; express 
the residue ; filter and mix the liquids. 

According to Remington's practice of pharmacy, 
"maceration is the process directed by the German Phar- 
macopoeia exclusively in preparing tinctures," and under 
the heading of percolation, he adds : "In Great Britain, 
France and Germany the process (percolation) is well 
known and is practiced to some extent, but maceration 
still holds in these countries the chief place as a means 
of extracting the soluble principles of drugs"; further, 
"No attempt should ever be made to produce fluid ex- 
tracts on the small scale without previous maceration," 
and "the intelligent practice of the process of percola- 



20 Manufacture of Vanilla Extracts 



tion, therefore, requires an accurate knowledge of the 
constituents and physical properties of medicinal sub- 
stances." 

DIGESTION. 

The use of heat for extraction is an old and dis- 
credited method and should never be practiced, since the 
effect of heat on the beans has the tendency of decom- 
posing the highly flavored aldehydes, with consequent 
loss of character. 

Exhausting the beans in vacuo would prove practical 
were it not for the fact that a large portion of the vanillin 
ethers and esters are carried over into the pump, which, 
of course, represents an irreparable loss. 

The most rapid, economical and thorough process 
for exhausting the active principles of the vanilla bean 
consists of mechanical maceration, the beans and mens- 
truum being placed in a suitable machine designed for 
the purpose (see figure on page 21). This machine is 
fitted with an air-tight cover for receiving and discharg- 
ing the content, and is absolutely air-tight, thoroughly 
eliminating all possibility of alcoholic evaporation. The 
effect of the violent, protracted surge of the menstruum 
in the machine is to force it through the cellular structure 
of the beans many thousand times during each day's 
operation, resulting in a rapid and thorough exhaustion 
by the combined mechanical and solvent power of the 
menstruum, with the certainty that all of the available 
vanillin, resins and color content of the beans are in solu- 
tion; whereas, in percolation, the menstruum comes in 
contact with the beans but once. 

PERCOLATING PROCESS. 

Select a percolator (conical preferred) with a capa- 



Exhaustion of the Vanilla Bean 



21 




22 Manufacture of Vanilla Extracts 

city double the amount required to hold the beans, and 
place at the bottom a small quantity of washed excelsior ; 
then place a layer of beans (cut fine) about three inches 
deep, then another layer of excelsior, then another of 
vanilla, until you have the entire quantity of the beans 
in the percolator. The beans should be packed, using 
a packing stick for the operation. Considerable care and 
experience are required so that the packing will be as 
uniform as possible throughout the entire mass. Also 
guard against packing too tight, since in that event the 
menstruum will refuse to flow; on the other hand, un- 
less sufficient resistance is offered to the menstruum, the 
net results will be far from satisfactory. 

Now add the menstruum, slowly, until the beans are 
covered ; open the spigot, and, when the percolate ap- 
pears, close the spigot, and, after covering the percolator, 
allow it to stand twenty-four hours to macerate; then 
open the spigot and permit the percolate to proceed, add- 
ing the menstruum until completed, which should be in 
from four to five days. 

Place the dregs into a cotton bag, put into a power- 
ful screw press and express, filter and add to the perco- 
late ; next add the sugar, completing the operation. The 
dregs should be saved for making a second quality of 
extract, but the resultant liquid would not pass as a legal 
vanilla and would have to be labeled "imitation." 

MECHANICAL MACERATION-PROCESS. 

Place the menstruum into the container of the ma- 
chine; next, add the finely cut (not ground) beans, screw 
down the air-tight cover and start the machine. From 
two to three days are sufficient to complete the exhaus- 
tion, since the beans and menstruum are brought into a 
surging contact, 26,000 times per day. 



Formula for Making Vanilla Extract 23 

The entire mass can now be transferred to a perco- 
lator for clarifying, although the use of the double pres- 
sure filter and percolator, described on page 21, will be 
found the most rapid and satisfactory. After the extract 
has ceased to flow from the dregs, ascertain the amount 
necessary for completing the volume of finished product 
and add that amount of water in the filter (water dis- 
placement) ; pour the water very carefully, letting it fall 
on a glass plate so that the position of the beans may 
not be disturbed. If you use sugar in your vanilla, do 
not fail to allow for the volume increase (see sugar table 
page 71). Always add the sugar to the finished product. 

We will suppose that the batch completed represented 
25 gallons, and that the menstruum used is what is known 
as dilute alcohol, viz., equal parts by volume; next add 
sufficient water in the filter until i2 l / 2 gallons of water 
washings has been obtained. The use of this water will 
be found under the heading of menstruum (solvent). 

FORMULA. 

The Federal "Standards of Purity for Food Prod- 
ucts" defines vanilla extract as follows : 

Vanilla extract is the flavoring extract pre- 
pared from vanilla bean, with or without sugar 
or glycerin, and contains in one hundred (100) 
cubic centimeters the soluble matters from not 
less than ten (10) grams of the vanilla bean." 
"Vanilla bean is the dried, cured fruit of 
Vanilla planifolia, Andrews." 

The foot-note on page 13 of Circular No. 19, issued 
by the Department of Agriculture, contains the follow- 
ing: 

"The flavoring extracts herein described are 
intended solely for food purposes and are not 



24 Manufacture of Vanilla Extracts 

to be confounded with similar preparations de- 
scribed in the Pharmacopoeia for medicinal pur- 
poses." 

Since 10 per cent., or 12 4/5 ounces, of beans to the 
gallon is the minimum allowed by law, the necessity of 
extracting all of the soluble principles is at once appar- 
ent. However, as a matter of precaution, it is much more 
advisable to employ 13 or 14 ounces to the gallon, as per 
the following formula: 

Vanilla beans, cut very fine. . . . 14 ounces 
Cologne spirits (190 proof) .... ^ gallon 

Pure water y 2 gallon 

Cane sugar to suit (5 to 10 per cent.). 
(Sugar vs. Glycerin.) 

The philosophy of adding glycerin to vanilla was 
based on the theory that glycerin acts as a binder during 
baking operations. While it is true that vanillin is sol- 
uble in glycerin, and glycerin is a non-volatile or fixed 
body, various baking tests failed to substantiate the the- 
ory. The use of glycerin has many supporters, while 
others, including such eminent authorities as Dr. C. P. 
Nicholls ("Monograph on Flavoring Extracts," by Har- 
rop), writes as follows: "A mixture of cologne spirits, 
water and glycerin has been tried, but I have not found 
the addition of glycerin an improvement." 

The use of sugar is to be recommended, since it will 
increase the body and help to bring out the flavor. 

AGEING. 

The principal virtue in storing vanilla in wood for a 
long period consists of dealcoholization. This can be 
demonstrated by dealcoholizing a sample in an evaporat- 
ing dish at room temperature, and comparing with sample 



Manufacture of Tonka Extract 25 

not so treated. Ageing practically amounts to concen- 
trating, since alcohol is not an active principle, and al- 
though at least 50 per cent, by volume of alcohol is neces- 
sary to extract the vanillin, resins and other active prin- 
ciples after once being dissolved, they will remain in solu- 
tion even when the alcolohic content of the extract has 
been reduced 15 per cent. 

The lowering of the alcoholic strength by the direct 
addition of water will precipitate the greater portion of 
the resins, and resins once thrown out of solution in this 
manner do not dissolve again by simply adding a little 
more alcohol. 

TONKA EXTRACT. 

"Tonka extract is the flavoring extract pre- 
pared from tonka bean, with or without sugar 
or glycerin, and contains not less than one-tenth 
(o.i) per cent, by weight of coumarin extracted 
from the tonka bean, together with a corre- 
sponding proportion of the other soluble matters 
thereof." 

The tonka bean is the odoriferous seed of Wilding- 
ham (Dipteryx odorata), a large tree growing in Guiana. 
Two varieties commonly found in the market are Angos- 
tura and Para, the former being held at a much higher 
price than the latter. Another kind, Surinam, is also 
known to the trade. 

The active or odorous principle of the tonka bean 
consists chiefly of coumarin, a rhomboidal, somewhat 
irregular crystalline compound (C 9 H 8 O 2 ), the anhydride 
of coumaric acid. It is prepared synthetically from sweet 
clover, melilot, and other plants. The tonka bean has a 
strong, agreeable, rather heavy, aromatic odor which, 
while not resembling the vanilla in flavor, is sometimes 



26 Manufacture of Imitation Vanilla Extracts 



used to "strengthen" vanilla, the proportion in which it 
may be mixed with vanilla being a matter of taste and 
cost. 

IMITATION VANILLA. 

The principal ingredients employed in the manufac- 
ture of imitation vanilla are synthetic vanillin and cou- 
marin. The characteristic features of coumarin is de- 
scribed under heading of "Tonka Extract." Synthetic 
vanillin is obtained from eugenol, the heavy oil of clove. 
The natural vanillin and the synthetic vanillin are chemi- 
cally identical, but in the flavoring there is a perceptible 
difference in favor of the natural. However, it is rather 
difficult to explain how and where the difference exists. 
Vanillin alone is too delicate for general results, and a 
slight proportion of coumarin is necessary to bring out 
its qualities, as per the following formula : 

Vanillin 7 ounces 

Coumarin I ounce 

Cane sugar 8 pounds 

Spirits 3 gallons 

Pure water to make 10 gallons 

Caramel color to suit. 

Dissolve the vanillin and coumarin in the alcohol; next 
dissolve the sugar in the water and mix ; filter, if neces- 
sary. 

A proportion of one part coumarin to four parts 
vanillin may perhaps please some customers, particularly 
for culinary purposes. A product of this character will 
be found much stronger and considerably cheaper, but 
of course it lacks the delicate character : 

Vanillin 4 ounces 

Coumarin I ounce 

Cane sugar 6 pounds 



Manufacture of Non-Alcoholic Extracts 27 

Spirits YZ gallon 

Pure water to make 7 gallons 

Caramel color to suit. 
Proceed as in first formula. 

WHITE VANILLA. 

There will be found an occasional demand for a 
"white vanilla." All that is necessary is to eliminate the 
color from the foregoing formulas. The only advantage 
it possesses is the absence of any tint when used in white 
work such as frostings, etc. It should be protected from 
strong light owing to its tendency to discolor. 

USES HOT AND COLD. 

Tests on syrups, cold custards, ice cream, cake and 
candy have amply demonstrated the relative value of 
true and synthetic flavors for usage in hot or cold work. 
On all cold work, the true flavor showed a distinct ad- 
vantage, while on hot work the synthetic proved the more 
lasting and valuable. This rule holds good with all 
flavors ; the vanilla lost most of its highly flavored esters 
by the action of heat, while vanillin seemed to hold its 
full power. 

NON-ALCOHOLIC EXTRACTS. 

Non-alcoholic flavors are prepared in two forms, viz. : 
Powder and paste. In the powder form the composition 
is usually the essential oil incorporated with cane sugar 
and glycerine in about the following proportions : 

Granulated cane sugar 65 pounds 

Oil of bitter almonds 3 pounds 

Glycerin, C. P 2 pounds 

The ingredients are thoroughly mixed and packed in 
paper-lined air-tight tin containers. 

In the paste form, the composition and proportions 
are about as follows: 



28 Manufacture of Non-Alcoholic Extracts 

Vanillin 2 ounces 

Coumarin J/2 ounce 

Glycerin, a sufficient quantity. 
Caramel color, a sufficient quantity. 

Glucose, quantity sufficient to make 14 pints. 
The vanillin and coumarin are thoroughly mixed with a 
sufficient quantity of glycerin until a smooth paste re- 
sults, then add the glucose, thoroughly mix, and lastly 
add the caramel color to the desired shade. These goods 
are packed in one and two-ounce collapsible tubes. 

The legal requirements having reference to the proper 
labeling of these preparations should be very carefully 
investigated before attempting to place them on the mar- 
ket, since they are not entitled to the term "flavoring ex- 
tracts," the Department of Agriculture specifying an 
extract as a solution in ethyl alcohol. 

MENSTRUUM. 

The subject, alcohol content of menstruums, is of vital 
interest for the following reasons : 

First Since alcohol does not contribute to the flavor- 
ing value of any extract, being entirely dissipated when 
used in baking, the per cent, necessary is the amount 
that will thoroughly extract the available active princi- 
ples and preserve them at the lowest temperature to 
which the extracts will be exposed after shipping; hence 
any surplus quantity employed will represent an actual 
waste. 

Second Vanilla being regarded as one of the most 
delicate flavors known, it is always desirable to put the 
finished product on the market with the lowest per cent, 
of alcohol possible, conditional that all of the available 
vanillin and resins have been extracted and held in solu- 
tion. The minimum per cent, is thirty, since in the event 



Alcoholic Content of Menstruums 29 

of the alcohol falling below this number, the Government 
chemists invariably go further and test for total solids. 

Third No manufacturer would knowingly add an 
unnecessary cost to any of his products. 

The most intelligent method for determining the per 
cent, of alcohol necessary is to prepare small test batches, 
using, as a minimum, 45 and proceeding up to 55 per 
cent, by volume. Fifty per cent, as a rule is ample with 
the average beans, and occasionally we find old crop dry 
Mexicans that will operate nicely on 45 and 40 per cent. 
The principal trouble to guard against is the question of 
clarification, due to the fact that all vanilla beans con- 
tain a mucilaginous (gummy) product. As this matter 
is insoluble in strong alcohol, it is necessary to employ 
sufficient alcohol to keep the gummy matter out of solu- 
tion. To overcome the necessity of employing a high 
per cent, of alcohol (above 50 by volume), several proc- 
esses have been tried out with more or less success. 

First By the removal of the mucilaginous principle 
with the use of boiling water. While this method cer- 
tainly does remove the gum, it also has the effect of de- 
composing some of the more volatile aldehydes and 
esters; there is also the loss by vaporizing of some of 
the vanillin. If the water used for this purpose was not 
used in the making up of the menstruum, there would 
be quite a loss of vanillin, since this product is soluble 
in hot water. 

Second By drying the beans after cutting, the beans 
being spread out in a thin layer and exposed to a tem- 
perature of not more than no degrees F. The process, 
if properly conducted, will harden the gum and in conse- 
quence permit the use of a weaker menstruum. It must 
not be forgotten that the effect of the heat on the beans 
has the tendency of vaporizing some of the more volatile 



30 Alcoholic Content of Menstruums 

constituents of the bean, with the consequent deteriora- 
tion of the finished product. 

Third By the use of a strong primary menstruum, 
as follows : 

Vanilla beans, finely cut I pound 

Cane sugar i pound 

Alcohol, 190 proof 5 pints 

Pure water 3 pints 

The alcohol and water must be mixed previous to pour- 
ing on the beans, this rule holding good in any process 
followed. 

The above produces an extract in the proportion of 
one part of beans to eight parts of extract. By adding 
two pints of water to each eight pints of finished ex- 
tract, you produce an extract in the proportion of one to 
ten, conforming with the National Food Laws, as well 
as all the State laws. The extra water is added after 
removing the extract from the beans and after the extract 
has stood a few days. 

There is one serious objection to this process in that 
it is impossible to add water to a finished extract with- 
out throwing out of solution a perceptible amount of the 
resin content; and since it is these resins that serve as 
an index to the analytical chemist in determining whether 
10 per cent, of beans was used, the process is not recom- 
mended. 

Fourth By the use of "water-washings" described 
under "Mechanical Maceration." The process produces 
the best results of all methods heretofore described and 
operates under the following principle : When the ex- 
hausted beans are treated with water, the resultant prod- 
uct is known as water- washings ; and since these gums 
are insoluble in alcohol and are freely soluble in water, 
the water-washings contain a very appreciable amount 



Testing Vanilla Extracts 31 

of the gum in solution ; and when about an equal amount 
of alcohol is added, the mucilage is thrown out of solu- 
tion (precipitation) and gradually settles to the bottom. 
In practice, the beans are placed in the container and the 
alcohol and water washings are mixed and added to the 
beans in the least possible time required. If, under ordi- 
nary conditions, the gum is dissolved with the use of the 
water-washings, the gum from the beans would unite 
with the gum thrown out of solution from the washings 
and both would settle to the bottom at one and the same 
time. This operation requires the least time and labor, 
while no loss of any of the active principles is possible. 

Other conditions being equal, well cured old crop 
beans are always to be preferred, for as a general rule 
they will produce a clear extract with a much less 
amount of alcohol. 

CARE OF FINISHED EXTRACTS. 

Finished extracts should be well protected from the 
decomposing chemical action of strong light, for if this 
is not heeded the extracts will eventually be ruined. 

DEMONSTRATION. 

The old habit of testing extracts, particularly vanilla, 
by eliminating the alcohol by way of friction between the 
hands, is decidedly impractical, since by this method the 
exudation from the pores of the skin of the hands adds 
an odor to the vanilla that certainly does not tend to im- 
prove it. The most satisfactory method is with the use 
of an atomizer, which should be operated up to within 
about three feet of the prospective buyer. The results 
in a demonstrative way are all that could be desired, as 
when vanilla is finely subdivided the alcohol seems to be 
entirely eliminated while traveling through space, and 
the buyer gets the full benefit of the vanilla character. 



32 Manufacture of Lemon Extracts 



LEMON EXTRACTS 



LEMON EXTRACT. 

The flavoring preparation next in importance to 
vanilla is lemon extract. The Federal ''Standards of 
Purity for Food Products" Circular No. 19 defines lemon 
extract as follows: 

"Lemon extract is the flavoring extract pre- 
pared from oil of lemon, or from lemon peel, or 
both, and contains not less than five (5) per 
cent, by volume of oil of lemon"; 

and further, 

"Oil of lemon is the volatile oil obtained, by 
expression or alcoholic solution, from the fresh 
peel of the lemon (Citrus limonum L.), has an 
optical rotation (25 C.) of not less than +60 
in a loo-millimeter tube, and contains not less 
than four (4) per cent, by weight of citral." 

Lemon oil is a veiy complex body, consisting of at 
least 15 constituents. Of these the terpenes compose 
about 90 per cent, of the oil, serving mainly as a vehicle 
for the essential ingredients, viz.: the aldehydes, includ- 
ing citral, 4 to 6 per cent., the alcohols and esters and 
other compounds 4 to \S per cent. The entire oil is read- 
ily soluble in strong akohol (80 per cent, or more) which 
constitutes the most expensive ingredient, since its cost 
is a trifle over 75 per cnt. of the total cost of the extract. 
Citral is the chief esseitial ingredient, but citral alone is 
not lemon, the remaining ingredients being necessary to 
fully develop the true lemon character. 



Oil of Lemon 33 



The terpenes are very prone to decomposition ; ex- 
posed to the action of light and heat with access of air, 
they quickly develop an odor and taste of turpentine. 

Oil of lemon should be kept in well stoppered con- 
tainers, in a cool place, protected from the chemical ac- 
tion of light. The contents of an original package, after 
having a portion removed, can be kept in a fragrant 
condition by adding to each pound of oil one ounce of 
alcohol ; shake well, and next add one ounce of water 
and again shake. The water withdraws the alcohol from 
the oil and collects as dilute alcohol at the bottom of the 
container, where it should be permitted to remain until 
the oil has been used, shaking each time the container has 
been opened. Oil of lemon so treated has been kept fresh 
and fragrant for fourteen months. 

Oil of orange may be treated in a similar manner 
with excellent results. 

Oil of lemon can be kept for an indefinite period un- 
der the most unfavorable conditions known if from I to 
2 per cent, of a fixed oil is incorporated with it. Such 
oils as cotton and olive are well adapted for this purpose. 
A test sample treated in this manner has been exposed 
to the action of heat and light for two years, and at the 
end of that time did not indicate any deterioration in the 
least. This method of preserving oil is well adapted to 
bakers' and confectioners' use, also oils intended for pre- 
paring terpeneless extract of lemon ; but it is not recom- 
mended for use in whole oil lemon, since the existence of 
the minute quantities of the fixed oil might be opposed 
by the pure food authorities. 

The manufacture of extract of lemon is a very simple 
process, the formula consisting of a solution of 5 per 
cent, of oil of lemon in strong alcohol as per the fol- 
lowing : 



34 Manufacture of Lemon Extracts 



Oil of lemon 6.4 ounces 

Grain alcohol 121. 6 ounces 

128 ounces=i gallon 
Mix thoroughly, let stand a few hours, and filter. 

Bear in mind that this formula contains the minimum 
allowed by the food laws, and the author would suggest 
the advisability of employing a larger per cent, of oil, 
since there is always a liability of error on the part of 
the manufacturer or analyst, which may result in a food 
law case. The habit of obeying the law in the letter, 
rather than in the spirit, is not to be commended. 

That this position has been adopted by some of the 
leading manufacturers is attested by an examination of 
seven of the most popular brands on the market. The 
per cent, of whole oil of lemon varied from 8 to 17 per 
cent., with the precipitation and centrifuge method. 

TERPENELESS EXTRACT OF LEMON. 

The Federal "Standards of Purity for Food Prod- 
ucts" Circular No. 19 defines terpeneless extract of lemon 
as follows: 

"Terpeneless extract of lemon is the flavoring 
extract prepared by shaking oil of lemon with 
dilute alcohol, or by dissolving terpeneless oil of 
lemon in dilute alcohol, and contains not less 
than two-tenths (0.2) per cent, by weight of 
citral derived from oil of lemon." "Terpeneless 
oil of lemon from which all or nearly all of the 
terpenes have been removed." 

Terpeneless oil of lemon is simply the natural oil freed 
from the terpenes by distillation under vacuum. These 
terpenes are bodies or chemical compounds which con- 



Terpeneless Extract of Lemon 35 



sist entirely of hydrogen and carbon, and while they are 
considered as inert and worthless as a flavoring medium, 
they require a strong alcohol for solution. Terpeneless 
oils of lemon are offered by the trade at prices ranging 
from $20 to $30 per pound, while the percentage of citral 
varies from between 40 to 65 per cent. The lower grade 
oils have been freed from only a portion of the terpenes 
and will not dissolve clear in a 50 per cent, by volume of 
a 190 proof alcohol. 

The words, "nearly all of the terpenes have been re- 
moved," no doubt account for the presence on our mar- 
kets of oil of various strengths and character. When 
purchasing a terpeneless lemon oil, the most logical 
method for the manufacturer to pursue would be as 
follows: Purchase a high-grade oil of a reliable house 
and request a statement in the form of a guarantee, hav- 
ing reference to the citral content, which should like- 
wise appear on the label ; then, and then only, will one be 
able to intelligently ascertain the amount of oil required. 
The amount of alcohol required should be sufficient to 
dissolve the oil (in a clear state) and hold it in solution 
at the lowest winter temperature to which these extracts 
would be subject in shipping to the trade, the amount in 
no instance being less than 50 per cent, by volume of 190 
proof. 

The use of carbonate of magnesia or any other filter- 
ing medium should be discouraged, since more or less of 
the citral is held back with the terpenes and magnesia, 
eliminating the element of certainty in computing the per 
cent, of citral in the finished product ; while with the use 
of the proper oil, no filtering is necessary. Whenever 
possible, soft or distilled water should be used. 

The advantages of terpeneless extract of lemon are 
as follows : They will not develop a rancid or turpen- 



36 Manufacture of Lemon Extracts 

tine flavor on exposure to heat or strong light, because 
the hydro-carbon that portion of the oil which readily 
decomposes is not present ; and, being soluble in water, 
they readily mix into ices, fountain syrups, etc. There 
is a saving of about 50 per cent, of alcohol, and they can 
be produced at the lowest possible cost for the strength, 
purity and permanence of flavor obtained. It is undoubt- 
edly true that this class of products is useful as a flavor- 
ing agent, but, as is true of all such products, they should 
be labeled exactly what they are. 

MANUFACTURE OF TERPENELESS LEMON EXTRACT. 

Various methods have been employed in the manufac- 
ture of terpeneless extract of lemon, the following being 
among the most popular : 

First What is known as the "shaking out" process 
consists of placing the oil and dilute alcohol into an air- 
tight container and churning for a considerable length 
of time ; then allowing the mixture to stand until the oily 
portion rises to the top, when the lower stratum is drawn 
off and filtered with the aid of magnesium carbonate or 
kieselguhr (an infusorial earth) to remove globules of 
oil held in suspension. The degree of citral removed 
depends, first, upon the alcoholic strength, and second, 
upon the thoroughness of the agitation, facilitating the 
extracting alcohol to come into close contact with the 
very minute globules of whole oil of lemon. The oily 
residue is generally subjected to a second churning proc- 
ess, in an effort to remove the entire amount of the deli- 
cate flavoring constituent, viz. : citral, which is the prin- 
cipal flavoring ingredient in oil of lemon. 

Second Place the lemon oil and alcohol into a suit- 
able container (an alcohol barrel free from glue) and 



Tcrpeneless Lemon Extracts 37 



agitate occasionally during a period of twenty- four 
hours; next add magnesium carbonate or kieselguhr 
(about 24 ounce to each gallon), shake thoroughly and 
add the water lukewarm, shaking thoroughly after each 
gallon addition, and, when complete, agitate or churn 
for at least one day; next place the barrel on a rack 
and allow the filtering medium to subside; next syphon 
off the almost clear liquid, being careful not to insert 
the hose too close to the filtering medium at the bottom 
of the barrel. In this manner the filtering operation will 
operate quite rapidly. Lastly, place the remaining por- 
tion of the mixture into the filter, using either heavy 
white paper or felt. A great deal of conscientious care 
and good judgment must be exercised in this process; 
otherwise a considerable waste of materials will result. 
The filtering medium will, in both cases, be found to con- 
tain the terpene product, together with considerable of 
the extract, and this can be recovered by placing the me- 
dium into a close-mesh cotton or linen bag and then put- 
ting the bag into a powerful screw press to express the 
products. Two distinctive layers will result; the lower, 
which is the extract and which can be syphoned off, and 
the upper, the objectionable terpene principle. 

The basis for computing the strength of a lemon ex- 
tract lies in the percentage of the citral it contains. An 
extract made from the whole oil will contain about .2 per 
cent, of citral in the finished extract, provided that 5 per 
cent, of oil has been used. Lemon oil usually contains 
about 4 per cent, of citral ; therefore, in the finished ex- 
tract there will be .O5X.O4=.OO2, or .2 per cent. Theo- 
retically, 5 per cent, of whole lemon oil, containing 4 per 
cent, of citral, should yield the required .2 per cent, of 
citral to a terpeneless lemon extract made by the shaking- 
out process. In practice, this is far from being correct, 



38 Manufacture of Lemon Extracts 

due mainly to the fact that more or less of the citral is 
withheld in the terpenes and filtering medium. The 
safest course to pursue would be the employment of at 
least 8 per cent, of oil as per the following formula : 

Spirits 190 proof ............. 59 ounces 

Water (lukewarm) ........... 59 ounces 

Oil, lemon ................... 10% ounces 



Third By simply dissolving terpeneless lemon oil in 
dilute alcohol. Processes No. i and No. 2 have been in 
use many years and are still quite extensively practiced. 
Practically all advantages as regards certainty of citral 
content and cost and labor are in favor of the simple 
method of dissolving terpeneless lemon oil in suitable 
strength alcohol, as per the following formula: 

Terpeneless oil of lemon (assaying 

66% citral) .................. 3^ drams 

Spirits 190 proof ................ j gallon 

Water (soft preferred) .......... ^2 gallon 

Add the oil to the spirits and shake well; next add the 
water, gradually shaking after each addition; then filter 
through paper, if necessary. To determine the citral 
content in the finished product, proceed as follows: 

8 drams=i ounce; 128 ounces= 

i gallon, or ................. 1024 drams 

add to the above the oil used. . . . 3^ drams 



and employ the total as the divisor; 1027) 3.125 (.00304 
for the dividend take the amount of oil used; the quo- 
tient represents the per cent, of oil employed ; next mul- 
tiply the per cent, of oil used by the per cent, of citral 
contained in the oil : 



Terpeneless Lemon Extracts 39 



.304 representing the per cent, of oil used 

.66 representing the per cent, of citral con- 
tent of the lemon oil 



1824 
1824 



0.20064 representing the per cent, of citral in the 
finished product, provided that no filter- 
ing medium has been employed. 

To ascertain the amount of terpeneless oil required 
to contain the necessary 2/10 per cent, citral in the fin- 
ished product, using an oil assaying 60 per cent, citral, 
proceed as follows : 

Per cent, of citral in the oil of lemon 

is the divisor 60) .002000 (.0034 

Per cent, of citral in finished prod- 
uct is the dividend 

Per cent, of oil required is the quo- 
tient 

Number of drams to the gallon 1024 

Times per cent, of oil required .0034 

3.4816 drams to the gal. 

The grated exterior rinds of fresh yellow lemons are 
a valuable addition to any lemon extract, adding charac- 
ter and piquancy, in fact, all that could be desired in a 
high-grade product. 

LEMON FLAVOR IMITATION. 

All grades of lemon extracts below the standards 
specified under "Lemon extract" and "Terpeneless lemon 
extract" must be labeled, sold and invoiced as imita- 



40 Manufacture of Lemon Flavor Imitation 

tions. All products labeled and sold as imitations do not 
require a specified standard of purity or strength ; hence, 
by varying the proportions of formulas submitted, ex- 
tracts of almost any desired strength and cost can be 
made. At this time, the Federal and most State laws 
permit the use of coloring, provided the colors used are 
plainly stated on the label and are of the "certified" type. 
The great advantage which the use of certified colors of- 
fers to the food products manufacturers is clearly set 
forth in F. I. D. (Food Inspection Decision) No. 117, 
as follows : 

"Food Inspection Decision No. 76, published 
July 13, 1907, gives a list of seven coal tar dyes 
which may, without objection from the Depart- 
ment of Agriculture, be used in foods until fur- 
ther notice. Food Inspection Decision No. 77, 
published September 25, 1907, provides for the 
certification of dyes. Certified dyes may be used 
in foods without objection by the Department 
of Agriculture, provided the use of the dye in 
food does not conceal damage or inferiority." 

Uncertified coal tar dyes are likely to contain arsenic 
and other poisonous elements which, when used in food, 
may render such food injurious to health, and, therefore, 
would be adulterated under the law. 

The active principle of imitation lemon is composed 
chiefly of citral or lemongrass. One ounce of citral is 
equivalent in flavoring power to one pound of oil of 
lemon, but is decidedly deficient in delicacy and charac- 
ter of the real lemon oil. Commercial citral is not a syn- 
thetic product, its common source being lemongrass, sepa- 
rated by distillation. The per cent, of citral content of 
lemongrass varies from 60 to 75 per cent. Citral occu- 



Manufacture of Lemon Flavor Imitation 41 



pies the same relation to lemon flavor as coumarin does 
to vanilla, but it does not blend nearly as well. In the 
following formulas the use of citral or lemongrass are 
optional. There are three grades of lemongrass on the 
market, viz. : Native, rectified and Java, their relative 
values being in the same order : 

Terpeneless oil of lemon ^2 dram 

Citral y* dram 

Oil of lemon 4 ounces 

Alcohol 3 pints 

Water (lukewarm) 5 pints 

Magnesia carbonate 2 ounces 

Dissolve the oils in the alcohol, mix the magnesia and 
water, and add slowly together, shaking thoroughly off 
and on for one day ; filter through paper. 

Lemongrass 4 drams 

Alcohol 32 ounces 

Water (lukewarm) 96 ounces 

Carbonate Magnesia I ounce 

Treat as above. 

EXTRACT OF ORANGE. 

The Federal standard of extract of orange and ter- 
peneless extract of orange corresponds in all respects to 
lemon extract. As in the case of the lemon, the use of 
the grated outer rind of the orange is a valuable addi- 
tion to orange extract. There are no substitutes for 
orange flavors, the cheapest practical formula consisting 
of the terpeneless. 



42 Manufacture of Various Extracts 



VARIOUS EXTRACTS 



EXTRACT OF ALMOND. 

"Almond extract is the flavoring extract pre- 
pared from oil of bitter almonds, free from hy- 
drocyanic acid, and contains not less than one 
(i) per cent, by volume of oil of bitter al- 
monds." 

Oil of bitter almonds, commercial, is the volatile oil 
obtained from the seed of the bitter almond (Amygdalus 
communis L.), the apricot (Prunus armenlaca L.), or the 
peach (Amygdalus persica L.). 

No. i. 

Oil of almond 3 ounces 

Spirits 5 pints 

Water 3 pints 

Dissolve the oil in the alcohol and add water gradually, 
shaking after each addition; filter if necessary. 

No. 2. 

Oil of almond i 3/10 ounces 

Spirits 52 ounces 

Water 76 ounces 

Proceed as in formula No. i. 

A very satisfactory imitation can be prepared by the 
use of "Benzaldehyde," but, like all other synthetic 
flavors, is inferior to the natural product when used in 
the cold, but it withstands heat better. 



Manufacture of Various Extracts 43 

No. 3. 

Benzaldehyde i% ounces 

Spirits 45 ounces 

Water 83 ounces 

Proceed as above. 

WINTERGREEN EXTRACT. 

"Wintergreen extract is the flavoring extract 
prepared from oil of wintergreen, and contains 
not less than three (3) per cent, by volume of 
oil of wintergreen." "Oil of wintergreen is the 
volatile oil distilled from the leaves of the Gaul- 
theria procumbens L." 

No. i. 

Oil of wintergreen 4 ounces 

Spirits 90 ounces 

Water 38 ounces 

Imitation wintergreen is prepared by the use of oil 
of sweet birch, or Methly salicylate. 

No. 2. 
Oil of sweet birch, or methyl 

salicylate 3^/2 ounces 

Spirits 76 ounces 

Water 52 ounces 

Mix, and filter if necessary. 

EXTRACT OF PEPPERMINT. 

"Peppermint extract is the flavoring extract 
prepared from oil of peppermint, or from pep- 
permint, or both, and contains not less than 
three (3) per cent, by volume of oil of pepper- 
mint." "Oil of peppermint is the volatile oil 



44 Manufacture of Various Extracts 

obtained from peppermint and contains not less 
than fifty (50) per cent, by weight of menthol." 

Substitutes for peppermint of a practical character 
are not known. 

No. i. 

Oil of peppermint 4 ounces 

Spirits i gallon 

Mix. This product can be colored with the use of pep- 
permint leaves to suit. 

In the event of a cheaper product being desired, pre- 
pare a terpeneless extract either by the use of terpene- 
less oil of peppermint or by the "shaking out" process, as 
prescribed for terpeneless extract of lemon. Since these 
products fall below the legal standard, they should be 
labeled, sold and invoiced as an imitation. 

EXTRACT OF GINGER. 

"Ginger extract is the flavoring extract pre- 
pared from ginger and contains in each one hun- 
dred (100) cubic centimeters the alcohol-soluble 
matters from not less than twenty (20) grams 
of ginger." 

No. i. 

Jamaica ginger (coarse powder) 2 pounds 

Spirits i gallon 

Place the ginger in a narrow percolator, using no force 
in packing, always providing sufficient washed-fine ex- 
celsior in the apex of the percolator to retain the ginger ; 
next pour on the alcohol, and when the entire mass is sub- 
merged, cork the delivery and cover the top and let stand 
for several days ; then percolate. 

Another method, in the absence of a percolator, is 
to place the ginger and spirits in a suitable air-tight con- 



Manufacture of Various Extracts 45 

tainer, such as a packing bottle or a keg, and shake fre- 
quently for a few days ; next place the mass on a coarse 
paper filter and finish. 

Jamaica ginger is always to be preferred to any of the 
lower grades, since the character is not only the finest, 
but the tendency of precipitates (sediment)' is reduced 
to a minimum. 
No. 2. 

Oleo-resin ginger ( i % ) 1 . 28 ounces 

Spirits 24 gallon 

Water (soft) }4 gallon 

Dissolve the oleo-resin in the spirits and gradually add 
the water lukewarm, shaking after each addition; let 
stand for a few days ; filter through paper, using a small 
amount of precipitated calcium carbonate as a medium if 
necessary. 

For a cheaper product the soluble essence is recom- 
mended, as follows: 
No. 3. Soluble. 
Jamaica ginger (coarse powder) .... 4 pounds 

Pumice stone (powdered) 4 ounces 

Lime (slacked) 4 ounces 

Spirits (dilute, equal parts) I gallon 

Rub the ginger with the pumice stone and lime until 
thoroughly mixed. Moisten with the dilute alcohol until 
saturated, and place in a narrow percolator, being care- 
ful not to use force in packing, simply placing it in to 
obtain the position of a powder to be percolated, so that 
the menstruum will flow through uniformly. Next add 
the dilute alcohol and percolate until one gallon of the 
percolate is obtained. Let stand twenty-four hours, and 
filter if necessary. The pumice should be repeatedly 
washed in water prior to using. 



46 Manufacture of Various Extracts 

No. 4. Soluble. 

Fluid extract of ginger (U. S. P.) . . 8 ounces 

Pumice, powdered and washed .... 2 ounces 

Water, quantity sufficient to make . . 24 ounces 

Pour the fluid extract of ginger into a bottle and add the 
pumice, shaking thoroughly; repeat the operation for 
several hours ; next add the water in the proportion of 
about two ounces at a time, shaking after each addition. 
When all is added, repeat the agitation occasionally dur- 
ing twenty-four hours, then filter, returning the filtrate 
until it comes through clear, and, if necessary, add suf- 
ficient water to produce the required 24 ounces of fin- 
ished product. 

EXTRACT OF ROSE. 

"Rose extract is the flavoring extract prepared 
from otto of roses, with or without red rose 
petals, and contains not less than four-tenths 
(0.4) per cent, by volume of otto of roses." 

Otto of roses is the volatile oil obtained from the 
petals of Rosa damascena Mill., R. moschata Herrm. 

No. i. 

Oil of rose (otto) y 2 ounce 

Spirits i gallon 

Mix and filter if necessary. 

There are a number of desirable artificial rose oils 
on the market, soluble in dilute 3 to i spirits, suitable for 
imitation products, costing but 25 per cent, of that of the 
genuine oil. To increase the tone or piquancy of this 
product, use rose geranium of the very best quality, as 
per the following: 



Manufacture of Various Extracts 47 

No. 2. 

Oil of rose (artificial) 2 drams 

Oil rose geranium (best quality) ... ]/?. dram 

Oil of clove (amboyna) 24 minims 

Spirits 3 quarts 

Water I quart 

Filter with carbonate of magnesia if necessary. Label 

an imitation. 

EXTRACT OF ALLSPICE. 

The Government standards do not include allspice. 

Oil of allspice (pimento) 2 drams 

Allspice (coarse powder) 3 ounces 

Spirits (dilute) 2 pints 

Mix, macerate for several days, and filter. 

ANISE EXTRACT. 

"Anise extract is the flavoring extract pre- 
pared from oil of anise, and contains not less 
than three (3) per cent, by volume of oil of 
anise." 

"Oil of anise is the volatile oil obtained from the anise 

seed." 

Oil of anise 4 ounces 

Spirits I gallon 

Mix and filter if necessary. 

CELERY EXTRACT. 

"Celery seed extract is the flavoring extract 
prepared from celery seed or the oil of celery 
seed, or both, and contains not less than three- 
tenths (0.3) per cent, by volume of oil of celery 
seed." 



48 Manufacture of Various Extracts 

"Oil of celery seed is the volatile oil obtained from 
celery seed." 

Oil of celery seed 3^ drams 

Spirits 3 quarts 

Water i quart 

Mix and filter if necessary. 

EXTRACT OF CINNAMON. 

"Cinnamon extract is the flavoring extract 
prepared from oil of cinnamon, and contains 
not less than two (2) per cent, by volume of oil 
of cinnamon." 

"Oil of cinnamon is the lead-free volatile oil obtained 
from the bark of the Ceylon cinnamon (Cinnamomum 
zeylanicum Breyne), and contains not less than sixty- 
five (65) per cent, by weight of cinnamic aldehyde and 
not more than ten (10) per cent, by weight of eugenol." 

Oil of cinnamon 2 . 56 ounces 

Spirits 90 ounces 

Water 38 ounces 

Thoroughly shake the oil with the alcohol and add the 
water gradually, shaking after each addition; filter if 
necessary. 

The standard for cassia extract is the same as that 
for cinnamon, but the oil specification is somewhat dif- 
ferent, as follows : 

"Oil of cassia is the lead-free volatile oil ob- 
tained from the leaves or bark of the Cina- 
momum cassia BL, and contains not less than 
seventy-five (75) per cent, by weight of cin- 
namic aldehyde." 



Manufacture of Various Extracts 49 



EXTRACT OF CLOVES. 

"Clove extract is the flavoring extract pre- 
pared from oil of cloves, and contains not less 
than two (2) per cent, by volume of oil of 
cloves." 
Formula is the same as that for cinnamon extract. 

EXTRACT OF MINT (SPEARMINT). 

"Spearmint extract is the flavoring extract 
prepared from oil of spearmint, or from spear- 
mint, or both, and contains not less than three 
(3) P er cent, by volume of oil of spearmint." 
Formula same as for anise extract. 

EXTRACT OF CHOCOLATE. 

(No Government Standard.) 

Curacao cocoa i J/2 pounds 

Dilute spirits (equal parts) I gallon 

Mix thoroughly and macerate for from five to ten days, 
shaking occasionally, and filter or percolate ; addition of 
extract of vanilla is an improvement. 

EXTRACT SARSAPARILLA SOLUBLE AN IMITATION. 

Oil of wintergreen I ounce 

Oil of sassafras */2 ounce 

Oil of cassia (or cinnamon) I dram 

Oil of fennel I dram 

Oil of caraway I dram 

Oil of anise 4 drams 

Alcohol and water of each y 2 gallon 

Caramel color to suit. 



50 Ethereal Imitation Flavors 

Dissolve the various oils in the alcohol and rub with three 
ounces of carbonate of magnesia in a mortar. Transfer 
the mixture into a bottle and add the water, shaking after 
each addition ; allow to macerate for a few days, and ni- 
ter through paper, adding sufficient water through the 
paper to make one gallon. 

EXTRACT PISTACHIO IMITATION. 
NO. I. 

Extract of almond 2 ounces 

Extract of vanilla 4 ounces 

Oil of neroli I drop 

Mix. 

No. 2. 

Oil of orange 4 drams 

Oil of cassia or cinnamon i dram 

Oil of nutmeg 1^2 drams 

Oil of bitter almonds 15 minims 

Oil of calamus 15 minims 

Oil of cloves 30 minims 

Spirits 12 ounces 

Water 4 ounces 

Magnesia, carbonate 3 drams 

Dissolve the various oils in the alcohol and rub with the 
magnesia; add the water with agitation; let stand a few 
hours, and filter. 

ETHEREAL IMITATION FLAVORS. 

Such flavors as pineapple, strawberry, banana, rasp- 
berry, cherry, etc., are prepared from concentrated fruit 
ethers. Owing to the large number of individual ethers 
required to compound the various flavors, considering the 



Ethereal Imitation Flavors 51 

small demand in general and the variations of formula, 
it is more economical, as well as more satisfactory, to 
purchase from a reliable essential oil house the mixed 
ethers representing the flavors desired. These ethers 
were formerly known as "Fruit Oils/' but under the 
Federal Food and Drugs Act this term has gone into 
disuse. 

As to the status of these ethereal flavors under the 
food laws, there is pending at present under the Penn- 
sylvania State law litigation as to whether Amyl Acetate 
and, possibly, one or two other ethers may be used in 
food products. Undoubtedly the general disposition of 
food officials is against such substitute materials. They 
have never been very popular, but certain sections of the 
country enjoy a fair demand. It is necessary so to label 
them that no complaint can be made of misbranding un- 
der the food laws. 

They are made into the ordinary strength by a simple 
reduction with alcohol and water in the following pro- 
portions : 

Concentrated pineapple ether 3 ounces 

Spirits J/ gallon 

Water J^ gallon 

Dissolve the ether in the alcohol, and gradually add the 
water and filter. 



52 Laboratory Notes 



Laboratory Notes 

Menstruums (Solvents). 

Alcohol, being the most extensively employed, will be 
considered first. Alcohol is a volatile, inflammable, color- 
less liquid (C 2 H 5 OH) of a penetrating odor and burning 
taste. In commerce the alcohol produced from maize or 
other grain is known as ethyl or grain alcohol. It should 
be kept in well stoppered containers, and in a cool place, 
remote from fire. When alcohol and water are mixed to- 
gether, a rise in temperature and contraction in volume 
take place. In small operations the contraction is gen- 
erally disregarded; in larger operations the loss is very 
apparent. If fifty-five gallons of alcohol be mixed with 
forty-five gallons of water, the total will not be 100 gal- 
lons of dilute alcohol, but only 96% gallons, showing a 
loss of 3^4 gallons. 

One gallon of 190 proof alcohol, temperature 15.6 C. 
(60 F.), specific gravity 0.816, weighs 6 pounds 12 
ounces and 339 grains. 

Proof Spirit is a term used by the Revenue Depart- 
ment in assessing the tax on alcoholic liquors. It means 
a liquid in which there is 50 per cent, (by volume) of 
absolute alcohol. As it is the actual alcohol in the 
whiskey, brandy, dilute alcohol, etc., which is taxed, and 
as this varies widely, it is necessary that the actual wine 
gallons be converted into proof gallons before the tax 
rate can be fixed. A sample that is half alcohol and half 
water is "100 proof." A sample that is three-quarters 
alcohol and one-quarter water is 150 proof, and the tax 
on every gallon of it is one and a half times the regular 
Government rate per proof gallon. Absolute alcohol is 



Alcohol S3 

200 proof and is required to pay a double tax. The legal 
definition of proof spirit is : "That alcoholic liquor 
which contains one-half its volume of alcohol of a specific 
gravity of 0.7939 at 60 F." 

Rule for Diluting Alcohol (Pile's). 

To reduce alcohol to any desired strength: To as 
many parts of the given alcohol as are indicated by the 
percentage required, add sufficient water to make the 
number of parts of the mixture equal to the percentage 
of the given alcohol. 

Example: If it is desired to make an alcohol of 30 
per cent, from one of 95 per cent., take 30 fluid ounces 
of the alcohol and add a sufficient amount of water to 
make 95 fluid ounces. 

The alcohol best suited for the manufacture of flavor- 
ing extracts is what is known as true deodorized or Co- 
logne spirit, or alcohol free from fusel oil. A mixture 
of 10 cubic centimeters of alcohol and 0.2 cubic centi- 
meter of potash lye evaporated down to one cubic centi- 
meter should not give any odor of fusel oil after super- 
saturation with dilute sulphuric acid. Deodorized alco- 
hol should not possess a foreign odor and should mix 
with water without becoming turbid. 

Water as a solvent in flavoring extracts is next in 
importance. Ordinary water always contains solid mat- 
ter, and traces of various salts in solution or suspension ; 
while this solid matter and salts do not ordinarily unfit 
it for drinking purposes, they do, in many instances, 
seriously interfere with the preparation of flavoring ex- 
tracts. In some sections of the country, the drinking 
water might be pure enough for the processes, or, at 
least, it does not contain serious impurities ; in other sec- 
tions, the water would be totally unfit for the preparation 



54 Laboratory Notes 

of flavoring extracts. Soft or distilled waters are always 
to be perferred. 

Brief Rules for Qualitative Tests of Water. 

No. i. If the water reddens blue litmus paper be- 
for boiling but not afterward, and the color of reddened 
paper is restored upon warming, it is carbonated. 

No. 2. If it possesses a nauseous odor and gives a 
black precipitate with acetate of lead, it is sulphurous. 

No. 3. If it restores blue color to litmus paper after 
boiling, or develops a red color on the addition of a 
phenolphthalein test solution, it is alkaline. 

No. 4. If it possesses neither of the above proper- 
ties in a marked degree and leaves a large residue upon 
evaporation, it is a saline water. 

When water is pure, it will not become turbid or pro- 
duce a precipitate with any of the following reagents : 

Baryta water, if a precipitate or opaqueness appears, 
carbonic acid is present. 

Chloride of barium indicates sulphates. 

Nitrate of silver indicates chlorides. 

Oxalate of ammonia indicates lime salts. 

Boiling for five minutes and filtering when cool will, 
in many instances, make objectionable water suitable for 
extract purposes. 

FILTRATION. 

Filtration is the process of separating liquids from 
solids, with the object of obtaining a liquid in a trans- 
parent condition. The intervention of porous substances, 
termed filters, to intercept solid particles is necessary in 
performing this process. They are usually made from 
paper, paper pulp, linen, felt, etc. Paper filters are the 



Filtration Methods 55 

most useful of all kinds and are employed in general 
operations requiring fine filtration, since the solid par- 
ticles are much more completely separated by paper than 
by strainers, owing to the pores of the paper being 
smaller and more numerous. 

When folding a filter, care should be observed not to 
extend the creases entirely to the apex, but to terminate 
them at a distance of about J^ inch from it, since the 
point at which all creases converge would thereby be so 
weakened that the weight of the liquid would rupture the 
filter. When pouring the liquid in the filter, the stream 
should never be delivered upon the apex, but upon the 
sides, feeding in a circular motion, so that the force of 
the fall will be broken before the weakest point is reached. 
In filtering liquids composed mostly of water the paper 
is very liable to be broken, since the water tends to soften 
it (while alcohol has a reverse action) ; the use of a small 
tuft of absorbent cotton in the apex of the filter will, in 
a large measure, overcome this trouble. The filter paper 
should be entirely within the funnel, since, if the edge 
of the paper projects above the funnel, waste ensues 
from evaporation of volatile liquids, as well as from the 
increased and unnecessary absorption due to the excess 
of the filtering paper ; in addition, an untidy and careless 
habit is formed. 

The filtering papers in the market are of three 
weights : light, medium and heavy ; and of two colors : 
white and gray. For general purposes the French filters 
are almost universally used, the "Prat Dumas" brand be- 
ing the most common. The gray filters are made from 
a mixture of cotton, flax, wool, etc., and are well adapted 
for filtering colored liquids or tinctures, but, owing to 
the coloring matter they contain, they are not practicable 
for liquids containing free alkali. Ribbed-glass funnels 



56 Laboratory Notes 



are always to be preferred, as they operate more rapidly 
than the plain. Felt filters are made bag-shaped and are 
admirably adapted in operations where a large amount 
of liquid is to be filtered and in cases where a filtering 
medium is employed. They are made in sizes ranging 
from one to five gallons' capacity, and operate very 
rapidly. When using such a filter on volatile liquids it 
should be enclosed in a tight-fitting filtering cabinet, pro- 
vided with a glass door ; for, if this is not done, the evapo- 
rative loss due to the large surface exposed to the atmos- 
phere will be quite large. Filtering mediums are finely 
powdered substances used to facilitate the operation of 
filtering. They operate on the principle of adhering to 
or entangling the objectionable suspended matter, thereby 
preventing it from rapidly obstructing the pores of the 
filter. 

The following substances are generally used for this 
purpose : Magnesium carbonate, purified talcum, washed 
pumice, precipitated calcium carbonate, precipitated cal- 
cium phosphate and kieselguhr (an infusorial earth). 
For operations on liquids containing acids, talcum and 
pumice are recommended, since the employment of the 
carbonates results in a chemical change. 

Filtering liquids of a volatile character should be con- 
ducted in the least possible time, and, to facilitate this 
condition, the filter must constantly be kept full, so that 
the maximum benefit of the filter surface can be utilized. 
For this purpose the automatic feeding or continuous fil- 
tration principle is recommended (see figure). The use 
of the containers termed skeleton demijohns is especially 
recommended. The bottles are clear glass, affording op- 
portunity for minute and intelligent inspection of the 
contents. The protection against breakage at the bottom 
is perfect, while the four upright canes or standards af- 



Filtration Methods 



57 




ford security for the sides and serve as substantial han- 
dles. These bottles are made in three sizes : two, three, 
and five gallons' capacity, respectively. 

The capacity of the container does not affect the prin- 
ciple involved, but in all cases both bottles should be of 
the same capacity, since, under such conditions, the oper- 
ations can be conducted over night and on Sunday, with- 
out the danger of overflowing the receiver. This process 
is adapted equally for use with the felt or other forms of 
filters. In principle, when the apparatus is in action, the 
liquid cannot escape from the upper container after the 
funnel is full as high as the mouth of that container, for 
the simple reason that the liquid in the funnel regulates 
the ingress of air. After the liquid escapes through the 
filter, receding from the mouth of the inverted container, 
air rushes in, more liquid runs out, and the supply in the 
funnel is thus kept up automatically until all the liquid 
has run from the upper bottle or demijohn. 



Laboratory Notes 




PRESSURE FII/TER AND PERCOLATOR 



Double Pressure Filter and Percolator 59 



DOUBLE PRESSURE FILTER AND PER- 
COLATOR. 

(See Fig., page 58.) 

In all filtering operations of 15 gallons or more, the 
most satisfactory results are obtained with the use of 
the Double Pressure Filter and Percolator, operating on 
the following principle : Cocks "E" and "G" are closed 
while vent valve "C" is opened ; the material to be filtered 
or percolated is next placed on perforated disc (clothed 
with felt or paper) "A," drawing off samples at cock "G" 
and returning until the filtrate or percolate runs perfectly 
clear. At this stage, close cock "G" and when the liquid 
in space "B" reaches about 10 inches in height, close 
valve "C" and open cock "E." A portion of the liquid 
will rapidly flow into receiver "H," but in the absence of 
sufficient vent, a partial vacuum is formed in space "B" 
and henceforth the flow into the receiver is in ratio to the 
flow through the perforated disc "A." Thus we have a 
double pressure, viz. : the weight of the liquid on top of 
the disc, plus the partial vacuum, or, as it is ordinarily 
understood, the suction of the lower column of liquid, 
the operation thus producing a finer filtrate in a shorter 
period. The cock "G" is designed for use in determining 
the character of the filtrate at the beginning of the opera- 
tion, as before stated; also as an exit for waste water 
when washing out the apparatus. The glass gauge "D," 
while not a necessity, will be found a convenience. All 
fittings should be of brass, preferably tinned. 

To construct a filter of this type, proceed as follows : 
Select an alcohol barrel in good condition; carefully re- 
move the head; next thoroughly remove all of the glue, 
if any. Next bore a ^2-inch hole in the bottom and se- 



6o Laboratory Notes 



curely fasten a J^-inch flange coupling and insert a brass 
nipple so that the end will come up flush on the inside, 
providing means for thoroughly draining; on this nipple 
fasten the cock. Insert a nipple at "E" and use lock 
nuts on both sides to thoroughly secure it, and screw 
on the cock. In a like manner, insert a nipple for vent 
pipe "C," bring up to top of barrel and end with valve. 

Should you decide to use a glass gauge, it will be 
necessary to place it at this time. The wood disc should 
be made of ^-inch oak and securely fastened at the cen- 
ter of the barrel; it should be made in two sections to 
facilitate placing it in position. This disc should contain 
a very liberal amount of perforations of about %-inch 
diameter; the more perforations the better. After this 
is completed, the entire disc should be clothed with a 
piece of thick felt or paper, securely fastened around the 
entire circle ; the filter is then ready for use. A filter of 
this design can be constructed of metal, but oak is much 
preferable on extract work, particularly vanilla. 

When through with the filter, always clean it at once 
in the following manner: Remove all of the magma 
(solids) from the filtering disc, next add hot water and 
operate as in filtering, with the exception of drawing off 
at cock "G," and, when through, leave all portions of 
the filter open to the air, including valves and cocks, 
thereby eliminating the tendency of the formation of 
must and foreign odors. A filter of this class will operate 
with the minimum evaporative loss, since the liquids at 
no time are exposed to the atmosphere, and can be fed 
automatically from an exterior source (an inverted con- 
tainer or syphon). The labor for results obtained is the 
minimum and the filter will last for years. The receiver 
should, in all cases, be of the same capacity as the amount 
operated on, thus eliminating any danger of overflowing. 



Simple Methods of Testing 61 



SIMPLE METHODS OF TESTING. 

The presence of fixed (fatty) oils, such as poppy- 
seed, castor and other bland resinous oils, can readily be 
determined by placing a few drops on clean white blot- 
ting paper and exposing the paper to a mild heat ; if the 
oil is pure, the spot on the blotter disappears immediately. 
To fully substantiate this test the blotter should be held 
up to the light, and if no permanent stain is visible, the 
oil can be accepted as free from fixed oils. 

Alcohol is sometimes added to essential oils of high 
value. To detect, add a small portion in a graduated test 
tube and carefully drop in a small amount of water; if 
alcohol is present, the drops will be surrounded with a 
milky (turbid) circle; next, add more water and shake, 
and after the liquids have separated, the approximate per 
cent, of alcohol present can be computed by the increased 
volume of the upper layer. Another method consists of 
agitating with the oil in a test tube a few small pieces of 
dried chloride of calcium. These will remain unchanged 
if the oil is pure, but they will dissolve in an oil contain- 
ing alcohol, and the resulting solution will form a dis- 
tinctive layer on the bottom of the container. 

A more accurate test of the presence of alcohol in an 
essential oil is accomplished by the use of metallic sodium 
or potassium. Place fourteen drops of the oil on a per- 
fectly dry watch glass, and put a piece of sodium or po- 
tassium, the size of a pin's head, in the center of it. If 
the alkali remains unchanged for twenty minutes, no al- 
cohol is present, but if it disappears after five minutes, 
the oil contains at least 4 per cent, of alcohol; if it dis- 
appears in less than one minute, it indicates the presence 
of not less than 20 per cent, of alcohol. 



62 Laboratory Notes 



To Test Oil of Lemon. The presence of purified 
turpentine in oil of lemon is not so easily detected on 
account of its similar composition and specific gravity. 
By adding three volumes of strong alcohol with one vol- 
ume of the oil, the turpentine, if present, will remain un- 
dissolved, and by evaporating a small quantity on a blot- 
ting paper and shaking the paper in the air, the presence 
of this adulterant- will be indicated by the terebinthinate 
(turpentine) odor, using a similar test for comparison 
with an oil of known purity. 

The most dangerous adulterant in oil of lemon is 
citrene, the terpene principle obtained as a by-product in 
the extraction of citral from oil of lemon, while prepar- 
ing terpeneless oil. 

To Test the Purity of Oil of Cloves. Oil of cloves, 
when pure, will manifest the following reaction : When 
shaken with pure liquor of ammonia, it coagulates and 
crystallizes after fusion by a gentle heat ; treated with an 
alcoholic solution of potassa, it congeals into a crystalline 
mass with total loss of its odor. A solution of potassium 
chromate transforms it into brown flakes, while the yel- 
low color of the salt is dissipated. A negative result in- 
dicates an addition of inferior oils. 

To Test the Purity of Oil of Bitter Almonds. Oil of 
bitter almonds is sometimes adulterated with nitro-ben- 
zole, and this may be detected by the use of a solution of 
potassa. The liquid has a green color if nitrate-benzole 
is present, and upon dilution three layers are formed, the 
lower yellow, the upper green ; over night, the green color 
changes to red. 

To Test the Purity of Otto of Roses. The principal 
adulterants to be found in otto of roses are the oils of 
rhodium, geranium, sandalwood and camphor, and occa- 
sionally spermaceti, which is added to contribute the crys- 



Simple Methods of Testing 63 



talline appearance. Otto of rose, when pure, has a bland, 
sweet taste; if it is bitter, this indicates the presence of 
rhodium or sandalwood ; if it is pungent or biting to the 
palate, it contains either oil of geranium or camphor, or 
both ; if it imparts an unctuous sensation to the palate, or 
if it responds to the blotter paper test for fixed oils, it 
contains spermaceti. A single drop of otto, placed on a 
watch glass with one drop of concentrated sulphuric acid 
(C. P.) and stirred with a glass rod, will retain its purity 
and color, but a sample adulterated with other oils is ren- 
dered more or less brown and develops peculiar odors, 
i. e., from oil of geranium, strong and disagreeable ; from 
oil of rhodium, increased and rendered unctuous and re- 
sembling cubeb; from camphor, characteristic and com- 
bined with acidity ; from spermaceti, unctuous and clearly 
perceptible. 

The specific gravity of an essential oil is not an in- 
fallible indicator, and this method should be employed 
only after all other known methods of detection have 
been resorted to. 



64 Laboratory Notes 



ESTIMATION OF SMALL QUANTITIES OF 
ESSENTIAL OILS. 

To determine the per cent, of essential oil in flavor- 
ing extracts, proceed as follows : 

Howard Method. Twenty c.c. of the extract are 
diluted with 50 c.c. of water and one drop of hydrochloric 
acid (except in case of clove and cinnamon extracts, 
when the acid is unnecessary). The liquid is then ex- 
tracted in a separator with three successive portions of 
15 c.c., 10 c.c. and 5 c.c. of ether. The mixed ethereal 
extracts are washed with 10 c.c. of water that has been 
previously saturated with ether, so as to remove prac- 
tically all of the alcohol. The ether solution is now trans- 
ferred to a Babcock milk bottle, which is immersed in 
warm water and the ether driven off. Water is now 
added and the bottle is placed in the centrifugal ap- 
paratus, and the essential oil read off in the bottle in the 
same way as with milk fat. The author claims that this 
process renders very accurate results, as the essential oil 
is scarcely exposed to heat, and there is, therefore, little 
risk of loss by evaporation. 

TO DETERMINE THE PER CENT. OF GAS IN 
AQUA-AMMONIA. 

The "Baume" hydrometer for ammonia renders fairly 
good results, provided no alkaline salts to any appreciable 
extent are present; this condition cj,n be determined by 
evaporation over a steam bath. For comparative testing 
the use of the burette will be found more accurate, using 
a standard acid solution in the burette and 15 c.c. of am- 
monia with a drop of phenolphthalein indicator added to 
it, and continuing the flow until exactly neutralized. 



Determining Acidity of Vinegar 65 



TO DETERMINE THE PER CENT. OF ACIDITY 
(AS ACETIC ACID) OF VINEGAR. 

Fill a 50 c.c. burette to zero point with "standard al- 
kali solution." Fill pipette by suction with vinegar to be 
tested ; cover mouth end with finger and allow the vinegar 
to fall exactly to 6 c.c. mark and place the vinegar in a 
porcelain dish until exactly at zero mark. Add a little 
pure water to the vinegar (distilled preferable) until 
nearly colorless; next add a drop of indicator, and by 
opening the pinch-cock add standard alkali solution from 
the burette until a permanent faint pink color appears, 
stirring with glass rod meanwhile. With a 45-grain 
(4.5%) vinegar, about 40 c.c. of alkali solution may be 
quickly added to the vinegar; then it should be added, 
drop by drop, until a faint pink color is permanent. The 
number of c.c. of alkali solution used indicates the acid 
strength in grains, which, divided by ten, gives per cent, 
of acidity (as acetic acid). For a strong vinegar (over 
50 grains) fill the pipette to 3 c.c. mark only and multiply 
the burette reading by two. 

The "standard alkali solution" used for the above 
test can be obtained from any reliable consulting chemist 
or dealer in chemical supplies, and is known as a tenth- 
normal alkali solution, being a 0.4 per cent, solution of 
sodium hydrate, very exactly standardized, against tenth- 
normal acid which has, in turn, been exactly standardized 
by calcite or other scientific means. 

The indicator solution is prepared by dissolving about 
2 per cent, of the phenolphthalein in strongest alcohol 
and diluting with an equal volume of distilled water. 



66 Laboratory Notes 



TO PURIFY ESSENTIAL OILS DETERI- 
ORATED FROM AGE. 

There are several oils that by absorption of oxygen 
from the air and from the chemical effect of light rays 
will become camphorated, grow turbid, deposit a residue 
(generally called stearopten) and lose more or less of 
their natural flavor, and, in the case of lemon oil, will 
acquire the odor of crude turpentine. Such oils as are 
free from oxygen are chiefly subject to these changes. 
Oils that have deteriorated in the manner indicated may 
be improved, but they can never be fully restored to 
their original condition. 

There are various methods employed: The most 
practicable is redistillation, mixing the oils first with 
water and incorporating a small amount of alkali ; or by 
agitation for thirty minutes with a thick paste consisting 
of powdered borax, animal charcoal and water, and fil- 
tering. The latter process renders excellent results with 
almost all essential oil restorations. Another method is 
to add 10 per cent, of warm water, shake well for fifteen 
minutes, let settle, draw off by means of a syphon, and 
filter through paper. Another process is the use of a 
potassium permanganate solution as follows: Dissolve 
one ounce of the salt in seven ounces of water and 
thoroughly agitate with four pounds of the oil, decant, 
mix with fresh water, and heat gently until the oil as- 
sumes a clear condition ; then separate and filter. 



Miscellaneous Receipts 67 

MISCELLANEOUS RECEIPTS. 

PLAIN OR SIMPLE SYRUP. 

Granulated cane sugar 30 pounds 

Water (boiling) 7 quarts 

Pour the sugar into the water gradually, stirring mean- 
while, and when dissolved, strain through coarse cotton 
cloth. Do not cover container until thoroughly cooled. 
This will produce four gallons of syrup. The relative 
proportions of sugar and water are very important since, 
if a smaller amount of sugar is employed, fermentation 
sooner or later will ensue. If too much sugar is used, 
crystallization will surely follow, resulting in a liquid too 
thin to keep under ordinary temperature. 

SODA FOAM. 

Soap bark, chips or coarse ground . 1 24 pounds 

Alcohol, 190 proof 2 pints 

Water, quantity sufficient to make. I gallon 

Mix the bark with 6 pints of water, boil for 10 minutes 
and strain. Add enough water (hot) through the strainer 
to make 6 pints of tincture and when cool add the alco- 
hol. Let stand over night and filter. One fluid ounce of 
this tincture is sufficient for one gallon of syrup. 

FRUIT ACID SOLUTION. 

Citric acid in crystals 2 pounds 

Alcohol, 190 proof I pint 

Water (distilled preferred) to make. I gallon 

Dissolve the acid in the water, add the alcohol, set aside 
for a few hours, and filter through paper. One ounce of 
this is sufficient for one gallon of syrup. 



68 Laboratory Notes 

For soda-fountain syrups, add from 2 to 4 ounces of 
flavor and color to suit. 

SEALING OR BOTTLE-TOPPING WAX. 

No. i. Elastic Enamel Wax. 

Good white glue i pound 

Oxide of zinc i ounce 

Precipitated chalk i ounce 

Dry white lead J/2 ounce 

Glycerine 3 ounces 

Color to suit. 

Make a paste of zinc, chalk and glycerine by rubbing 
them up into a cream ; then stir them into the liquid glue 
while hot and to about the consistency of syrup, and stir 
thoroughly ; it is then ready for use in the white and can 
be colored any shade desired by using aniline to suit. 
Antique bronze color can be obtained first by adding a 
little dry bronze powder and then adding aniline of the 
shade desired. To be used warm over water bath, and 
can be used any number of times. 

No. 2. 

Rosin 40 pounds 

Silicate of magnesia 25 pounds 

Paraffine 2 pounds 

Color to suit. 

Dissolve the rosin and paraffine with the aid of heat ; stir 
in the silicate of magnesia, stirring until thoroughly in- 
corporated; next add the color. 

No. 3. Take ordinary hard paraffine and, when 
melted, stir in sufficient oil soluble and aniline to suit. 

GRADUATING CONTAINERS. 

Graduated containers will be found very convenient 



Miscellaneous Receipts 69 

when used as receivers in filtration or percolation opera- 
tions, or for use in compounding. Plain containers may 
be graduated by placing them in a perfectly level position 
and carefully measuring out the exact quantity of water 
at 60 degrees F., next pasting a strip of bright-red-colored 
paper on the four quarter points, being careful to allow 
for the capillary curves ; and, when dry, shellacking the 
surface of the paper. 

DEODORIZING CONTAINERS. 

Place in the container some mashed raw potatoes with 
warm water, and shake occasionally for one hour; then 
empty the contents and wash with cold water. The odor 
will then have entirely disappeared. Such obstinate odors 
as peppermint readily yield to this treatment. To clean 
containers from the dry, hard film frequently encoun- 
tered, use a solution of potash with fine shot. This is also 
useful in removing fixed oils, etc. 



70 Laboratory Notes 



ADHESIVES. 

As a matter of convenience it is always desirable to 
employ an adhesive that can be used in the cold and, at 
the same time, that will dry in the shortest possible time. 
The best article for use on carton work is "silicate of 
soda"; it is inexpensive, does not ferment or decompose 
and will render very satisfactory results. Another good 
preparation is powdered corn starch digested with the 
aid of an alkali ; however, considerable care is necessary 
in its preparation, since it is highly important that the 
minimum possible amount of alkali should be employed 
as per the following : 

Into a suitable receptacle place one-half gallon of cold 
water; next stir in one pound of powdered corn starch 
and follow with one-half gallon of boiling-hot water into 
which has been added three fluid ounces of alkali solu- 
tion; stir until the mass becomes clear and transparent 
and immediately reduce to the consistency desired with 
hot water. For carton work it should be used consider- 
ably heavier than for labeling. This paste will not fer- 
ment or decompose, and is very economical, but, as be- 
fore stated, requires considerable care in its preparation. 

ALKALI SOLUTION (FOR PASTE). 

Dissolve Red Seal i can 

Lye in water i quart 



Weights and Tables 



TABLES. 

AVOIRDUPOIS WEIGHT. 
Pounds. Ounces. Drachms. Grains (Troy). 

i = 16 = 256 = 7,000 
i = 16 = 437.5 
i = 27.34 



Grams. 
453-60 

28.35 
1.77 



FLUID MEASURE. 
Gallons. Pints. Ounces. Drams. Minims. 

i = 8 = 128 = 1,024 
i = 16 = 128 






Cubic Centimeters. 
= 6l,440 = 3,785.435 
473-179 



= 7,680 = 



480 
60 



29-574 
3.697 



Sixteen ounces, or one pint, is sometimes termed a 
fluid pound. The above table is the one usually adopted 



in formulas. 

Pounds of Sugar. 
Added to 
One Gci lion of 


Quantity 


SYRUP TABLE. 

of Syrup Actually 


Obtained. 


Pounds of 
Sugar in 


Cold Water. 


Gallons. 


Pints. Fluid Ounces. 


of Syrup. 


I 


I 




10 


93 


2 


I 


I 


4 


i-73 


3 


I 


I 


14 


2-43 


4 


I 


2 


3 


3-05 


5 


I 


3 


2 


3-6 


6 


I 


3 


12 


4.09 


7 


I 


4 


6 


4-52 


8 


I 


5 


. . 


4.92 


9 


I 


5 


10 


5-28 


10 


I 


6 


4 


5-62 


ii 


I 


6 


14 


5-92 


12 


I 


7 


8 


6.18 


13 


2 




2 


6.38 


14 


2 




12 


6.7 


15 


2 


i 


6 


6.91 



72 Laboratory Notes 



AQUA (HOUSEHOLD) AMMONIA. 

Ammonia is a colorless, pungent, suffocating gas 
(NH 3 ), and the commercial article is obtained from gas 
liquor. Water is capable of absorbing 670 times its vol- 
ume of ammonia gas at 50 degrees F., increasing in bulk 
about two-thirds. Keep the tanks in a cool place and the 
plug secure, since heat rapidly expands the gas, with 
consequent loss and danger when drawing off. It is 
safer, if the ammonia has been kept in a warm room, to 
cool it off with ice water before attempting to withdraw 
the plug, as the liberated gas, when warm, frequently is 
forced out with extreme violence, and accidents which 
have resulted in injury to the sight of the operator are 
on record. The best antidote is the exposure or inhala- 
tion of vinegar or acetic acid. 

Table Showing the Percentage of Gas contained at 60 
Degrees Fahrenheit. 



20 degrees Beaume 17 per cent. 

19 " " 15 " " 

18 " " 13.5 " " 

17 " " 12 " " 

16 " " 10 " " 

15 " " 8 " " 

14 " " 6.6 " " 

j -2 a - 

12 " " 3.2 " " 

ii " " 1.6 " " 

One gallon of 26 degrees weighs 7^2 pounds. 



Bottles 73 



BOTTLES AND CORKS. 

BOTTLES CAPACITY, BREAKAGE, ETC. 

The question of over-capacities and breakage of ex- 
tract bottles is of sufficient importance in that it seriously 
affects the cost of production. It is a well-known fact 
that it is next to impossible to purchase bottles accurately 
graduated, since the workman or blower is compelled to 
guess at the quantity of glass he gathers for each bottle. 
He can do nothing else, as it is impossible to weigh or 
measure the molten mass. This is why it is impossible to 
guarantee the absolute accuracy of a bottle. However, 
some manufacturers are able to balance the variation to 
within about 2 per cent, either way, and this is about the 
best condition we can look to until the time when such a 
glass-blowing machine as the "Owens" will be adapted to 
the making of extract bottles. 

Breakage of bottles is due to several causes : Im- 
proper combination of raw materials, an excess of silica, 
a deficiency of alkali, insufficient heat in furnace, uneven 
distribution, and improper annealing, since carelessness 
on the part of the lehr tender in not keeping his lehr at 
the correct temperature will cause breakage. A large 
amount of breakage is due to rough handling in transit 
by the transportation companies, draymen and receiving 
departments. The writer would suggest ordering bottles 
shipped in the open crate with paper packing, in place 
of the closed box with hay for packing, since in the for- 
mer the men can see what they are handling and are more 
careful than they would be with the old-style package. 
The receiving department should be very careful before 
signing for bottle shipments to ascertain that the crates, 
cases and contents are in good condition. If not, they 



74 Bottles 

should make a notation on the receipt that the goods were 
received "in damaged conditions, subject to claim." 

Bottles should always be well washed prior to filling, 
irrespective of their clean appearance when taken from 
the packing case, for we must not forget that they are 
intended to contain a food product, and, since glass is a 
product resulting from a fusion at a high temperature of 
silica and alkali, very frequently traces of the alkali are 
found in the bottles, and these traces would have the ten- 
dency to deteriorate some of the more delicate flavors. 

FILLING BOTTLES. 

Bottle-filling machines are a valuable adjunct to con- 
cerns handling a large quantity of given size bottles at 
one time. In cases of frequent changing of containers 
and material, a cheap method consists of the use of a 
large, portable tray made of well-seasoned wood, of suit- 
able length and depth to accommodate the tallest bottles. 
The tray should be lined with sheet copper, although zinc 
will answer the purpose, but will not last as long. It 
should be fitted with standards of four by four, and in- 
clined to one of the corners, so that any liquid spilled by 
overflow or broken bottle can be quickly recovered 
through the drain. The standards should be fitted with 
roller-bearing castors of at least three inches diameter. 
This portable tray can be run to the bottle dryer and 
filled and next run to the source of supply and the bot- 
tles filled and corked with the aid of a rubber mallet. 
They can then be run to the labeling table and either 
labeled from the tray, or transferred to the tables, the 
latter being the better method, since all bottles ought to 
be permitted to lie flat on the table for a short time in 
order to ascertain that there are no leaky corks in the lot. 



Filling Bottles Corks 75 

When filling bottles, the supply should be elevated on 
a superstructure at least forty inches higher than the 
portable tray. If the stock can be contained in a barrel, 
a suitable-sized rubber tube may be connected with the 
faucet; but in the event of the container being of glass, 
the syphon system will have to be employed, with the 
aid of a semi-circular rubber-tube supporter to obviate 
the kinking of the tube. A certain percentage of the bot- 
tles will be found to contain a surplus quantity, and these 
can rapidly be corrected with the aid of a wood displace- 
ment stick. This stick should be cut or dressed with a 
handle about J^ inch diameter and iJ/2 inches long; at 
this point a shoulder should be provided and the rest 
should be of a diameter sufficiently small to enter the 
bottle readily and of a length to displace the required 
amount; this will necessarily have to be determined by 
experiment. 

CORKS. 

Use a good three or 4 "X" extra long taper cork. 
Corks should be stored in a dry room, as, in a damp room, 
the corks attract moisture and, in consequence, molds 
attach themselves to them and they acquire not only an 
unpleasant, musty odor, but a bad taste, easily communi- 
cated to the contents of the bottles stoppered with them. 
Before using, immerse them in cold water, never hot 
water. Very frequently when removing a cork it will 
break, hence the advisability of placing in the carton an 
extra cork. 



76 Figuring Costs 



FIGURING COSTS. 

The common error of computing costs of finished 
products wholly on formulas and costs of raw materials 
is practised by quite a number of concerns. Shrinkage 
losses, both visible and otherwise, are inevitable and must 
be carefully considered. For example, when equal quan- 
tities of water and alcohol are mixed, a curious phenom- 
enon occurs, since they occupy less space than when sepa- 
rate, the shrinkage amounting to about 3 J4 P er cent. 
This shrinkage, being controlled entirely by nature, can- 
not, of course, be eliminated. There are other losses that 
develop in the manufacture of flavoring extracts, and 
the total content should be determined in each batch pro- 
duced. This can be readily ascertained by the use of a 
card-recording system, as follows : 



Figuring Costs 77 



Extract Department. 
Date, February 12, 1912. 
Batch No. i. 

Character of stock produced, Tuxedo brand vanilla 
Operation started, February 12. 
Operation finished, February 20. 

Total gallons required from formula, 22. 
Per cent, of beans used, 10. 
Character of beans used, Bourbon, 75 per cent. 
Character of beans used, Mexican, 25 per cent. 
Total amount of beans used, 17.6 pounds. 
Cost of beans per pound, Bourbons, $3.00. 
Cost of beans per pound, Mexicans, $3.50. 
Per cent, of alcohol used in menstruum, 50. 
Amount of finished product obtained, 21.25 gallons. 
Amount of added menstruum required to complete, 

.75 gallon. 

Cost of same $i .00 

Total cost of beans 55-O 

Amount and cost of alcohol used, n gallons 

@ $2.68 29.48 

Amount and cost of sugar used, 20 pounds 

@ .05 i.oo 

Total labor required, 5 hours @ .40 2.00 

Total cost for 22 gallons $88.48 

Total cost per gallon 4.03 

Remarks . 



78 Figuring Costs 



Extract Packing Department. 

Date, March 5, 1912. 

Character of stock packed, 2 oz. Tuxedo vanilla. 

Amount of stock supplied, 14 gallons @ 

$4-03 

Less 23/100 gallons remaining 93 

Total cost of vanilla $5549 

Bottles supplied, 6 gross @ $2.15 12.90 

Bottles broken, 18 27 

Over-capacity, 2 per cent. =34.56 ounces. ... 1.02 

Six gross of cartons @ $3.80 per 1,000 3.28 

Corks and labels i .60 

Time required washing bottles, i girl, 2 40/60 

hours, @ . 10 27 

Time required rilling bottles, I girl, 3 20/60 

hours, .11 37 

Time required labeling and completing, i girl, 

12 15/60 hours, @.ii 1.35 



$76.55 
Total cost per gross 12.76 



To the above should be added a certain per cent, to 
cover supervision and general expenses. 



Figuring Costs 79 



The essential advantages of the recording system con- 
sist of providing ready means for determining the yearly 
output, including exact costs, of all grades of goods 
manufactured. It serves as a check on raw materials, 
including the shrinkage of alcohol, vanilla beans, etc., in 
original packages, and as an incentive to encourage em- 
ployees to provide means for reducing leaks and waste 
to their lowest terms. It standardizes time requirements 
for various operations and provides means for deter- 
mining the relative values of the employees. Again, since 
the capacities of stock bottles vary to an appreciable ex- 
tent, this system will continually keep one in touch with 
the same. 

Count, Weigh and Measure All Items on Receipt of 
Shipment. As an illustration: On receipt of a barrel 
of 95 per cent, alcohol or 190 proof, if the barrel has on 
it the Government stamp, one is reasonably certain of 
its purity. Weigh the barrel at once and note if the 
weight agrees with the Government gauger's weight 
stamped near the bung; if it does not, notify the distiller 
or dealer at once. If the weight is correct, open the 
barrel, and with the aid of a hydrometer (alcoholometer) 
determine the proof. After the barrel is empty, weigh 
it and note if the tare as stamped on the barrel is cor- 
rect, and if so, divide the net pounds by 6.7963, represent- 
ing the weight of one gallon of 95 per cent, alcohol. The 
author would suggest that the alcohol be shipped in glue- 
coated barrels, as this prevents any solution from the 
wood of the barrel, which, in some instances, affects the 
color and solvent properties of the alcohol. 



8o 



Index 



Index 



Acidity in Vinegar 65 

Adhesives 76 

African Vanilla Beans 14 

Age, Deteriorated Essential 

Oils 66 

Ageing Vanilla 24 

Alcohol.. 14, 27, 28, 29, 52, 

53, 61 
Alcoholic Content of Men- 

struums 29, 30 

Allspice (Pimento) Ext... 47 

Almond Extract 8,42 

Almond Extract, : |Fede/ral 

Standard 42 

Ammonia 64, 72 

Anise Extract 8, 47 

Apple Extract, Imitation . . 9 

Aqua-Ammonia 64, 72 

Avoirdupois Weight 71 

Bottle Breakage 73,74 

Bottle Capacity 73 

Bottle Filling 74, 75 

Bottles 73-75 

Bottle Topping Wax For- 
mulas 68, 69 

Bourbon Vanilla Beans n 

Brooks on Resins 15 

Care of Finished Extracts. 31 

Carton Adhesives 70 

Cassia Extract 8, 48 

Celery Extract 8, 47, 48 

Cherry Extract, Imitation. 9 

Chocolate Extract 49 

Cinnamon Extract 8, 48 

Circular No. 19, U. S. 

Dept. of Agriculture 8 

Classes of Extracts 8 

Clove Extract 49 

Cold Work in Extract 

Making 27 

Coloring, Use of 40 

Comoros, Vanilla Beans... 15 
Containers, Deodorizing... 69 
Containers, Graduating 69 



Corks 75, 76 

Cost Record, Extract De- 
partment 77 

Cost Record, Extract Pack- 
ing Department 78 

Costs of Extract Depart- 
ment 76, 77, 78, 79 

Coumarin 8, 25, 26, 28 

Coumarin Extract 8,26 

Cultivation of Vanilla Beans 12 
Cutting Vanilla Beans 17 

Definition of Flavoring Ex- 
tract 8 

Deodorizing Containers 69 

Digestion in Vanilla Bean 

Exhaustion 20 

Dilutirig Alcohol, Rule for. 53 
Double Pressure Filter and 
Percolator 59, 60 

Essential Oil Extracts ... 8, 48 
Essential Oils. 8, 32-36, 48, 61, 
62, 63, 64, 66 
Essential Oils Deteriorated 

by Age 66 

Esters Extracts, Estimate, 

ing Small Quantities of.. 8 
Ethereal, Imitation Fla- 
vors 50, 51 

Ethereal Extracts 8, 9, 50 

Exhaustion of the Vanilla 

Bean 4 17 

Extract of Allspice (Pi- 
mento) 47 

Extract of Almond 8, 42 

Extract of Anise 47 

Extract of Cassia 48 

Extract of Celery 47, 48 

Extract of Chocolate 49 

Extract of Cinnamon 48 

Extract of Cloves 49 

Extract, Flavoring, What 

Constitutes a 8 

Extract of Ginger 44 

Extract of Lemon 32-36 



Index 



81 



Extract of Mint (Spear- 
mint) 49 

Extract of Orange 8, 41 

Extract of Peppermint 43 

Extract of Pistachio, Imi- 
tation 59 

Extract of Rose 46 

Extract of Sarsaparilla ... 49 

Extract of Vanilla 10-25 

Extract of Wintergreen ... 43 
Extraction of Vanilla Beans 17 
Extracts by Maceration and 

Percolation 8 

Extracts from Essential 

Oils 8 

Extracts from Esters 8 

Extracts from Synthetics . . 8 
Extracts, Non- Alcoholic. 27, 28 

Federal Standard for Al- 
mond Extract 42 

Federal Standard for Ex- 
tract of Anise 47 

Federal Standard for Cas- 
sia Extract 48 

Federal Standard for Cel- 
ery Extract 47 

Federal Standard for Clove 
Extract 49 

Federal Standard for Cin- 
namon Extract 48 

Federal Standard for Gin- 
ger Extract 44 

Federal Standard for Lem- 
on Extract 32 

Federal Standard of Oil of 
Lemon 32 

Federal Standard' for Pep- 
permint Extract 43 

Federal Standard for Rose 
Extract 46 

Federal Standard for Spear- 
mint Extract 49 

Federal Standard for Tonka 
Extract 25 

Federal Standard for Ter- 
peneless Lemon Extract. 34 

Federal Standard for Va- 
nilla Extract 23 

Federal Standard for Win- 
tergreen Extract 43 

Figuring Costs of Extract 
Department 76, 77, 78, 79 



Filling Bottles 74, 5 

Filter and Percolator, 

Double Pressure 59, 60 

Filtering Liquids 56, 57 

Filtering Papers 55, 56 

Filters 55-60 

Filtration 54-60 

Filtration Methods 54-60 

Finished Extracts, Care of. 31 
Flavoring Extract, What 

It Is 8 

Fluid Measure 71 

Formula for Allspice (Pi- 
mento) Extract 47 

Formula for Celery Ext. ... 48 
Formula for Chocolate Ex- 
tract 49 

Formula for Clove Ext 49 

Formula for Making Va- 
nilla Extract 22, 23 

Formula for Peppermint 

Extract 44 

Formula for Almond Ex- 
tract 42, 43 

Formula for Anise Extract 47 
Formulas for Cinnamon 

Extract 48 

Formulas for Ginger Ex- 
tract ; .. : .44, 45, 46 

Formula for Imitation Sar- 
saparilla Extract 49, 50 

Formulas for Lemon Fla- 
vor, Imitation 41 

Formulas for Imitation Pis- 
tachio Extract 50 

Formulas for Rose Ex- 
tract 46, 47 

Formulas for Terpeneless 

Lemon Extract 38, 39 

Formulas for Wintergreen 

Extract 43 

Fruit Acid Solution 68 

Fruit Oils 51 

Gas in Aqua-Ammonia 64 

Ginger Extract 8, 44, 45, 46 

Graduating Containers 69 

Grinding Vanilla Beans 17 

Guadeloupe Vanilla Beans. II 

Harrop on Flavoring Ext. 24 
Hot Work in Extract 
Making 27 



82 



Index 



Household Ammonia 72 

Howard Method for Essen- 
tial Oils 64 

Imitation Extracts 8, 9, 26 

Imitation Lemon Flavor... 40 

Imitation Pistachio Ext 50 

Imitation Sarsaparilla Ext. 49 
Imitation Vanilla Extract.. 26 

Java Vanilla Beans 12 

Labeling Imitation Ext 28 

Laboratory Notes 52-56 

Lemon Extract 8, 32-36 

Lemon Ext., Fed. Standard 32 

Lemon Extract, Mfg 32-36 

Lemon Flavor, Imitation. . . 40 
Lemon Flavor, Imitation, 

Formulas 41 

Lemon Oil 32, 33 

Maceration in Vanilla Bean 
Exhaustion 19 

Machines for Cutting Va- 
nilla Beans 17 

Machine for Mechanical 
Maceration of Vanilla 
Beans 20, 21 

Manufacture of Lemon Ex- 
tract 32-36 

Manufacture of Terpene- 
less Extract of Lemon. 34-39 

Manufacture of Vanilla Ex- 
tract 10-25 

Manufacture of Various 
Extracts 42-49 

Mauritius Vanilla Beans... n 

Meat Cutters for Vanilla 
Beans 17 

Mechan. Maceration Proc- 
ess for Vanilla Beans ... 22 

Menstruums for Vanilla 
Bean Exhaustion 18 

Methods for Testing Oils, 

61, 62, 63 

Mexican Vanilla Beans n 

Mint Extract 49 

Miscellaneous Extracts.. .42-49 

Miscellaneous Recipes 67-69 

Non-Alcoholic Extracts. 27, 28 
Nutmeg Extract 8 



Oil of Lemon 32, 33 

Oil of Lemon, Federal 

Standard of 32 

Oil of Orange 32 

Oil Testing 61, 62, 63 

Orange Extract 8, 41 

Orange Oil 33 

Peach Extract, Imitation . . 9 

Peppermint Extract 8, 43 

Percolating Process in Va- 
nilla Bean Exhaustion. 20, 22 
Percolation in Vanilla Bean 

Exhaustion 18, 19 

Percolators for Testing Va- 
nilla Beans '. . 16 

Pimento (Allspice) Ext... 47 
Pineapple Ext, Imitation.. 9 
Pistachio Ext, Imitation... 50 

Plain or Simple Syrup 67 

Proof Spirit 52 

Purchasing Vanilla Beans. 16 
Purifying Essential Oils... 66 

Qualifications of a Manu- 
facturer 7 

Qualitative Tests for 
Water 54 

Raspberry Ext., Imitation. 9 
Record of Costs, Extract 

Department 77, 78 

Remington on Maceration. 19 
Remington on Percolation. 19 

Resins 14 

Rose Extract i, 8, 46, 47 

Rule for Diluting Alcohol. 53 

Sarsaparilla Extract 49 

Sassafras Ext, Imitation.. 9 
Sealing Wax Formulas. .68, 69 

Selecting Vanilla Beans 15 

Seychelles Vanilla Beans. .. li 

Soda Foam, Formula 67 

Solution, Fruit Acid 68 

Spearmint Extract 49 

Standard, Federal, Extract 

of Almond 42 

Standard, Federal, for An- 
ise Extract 47 

Standard, Federal, for Cas- 
sia Extract 48 

Standard, Federal, for Cel- 
ery Extract 47 



Index 



Standard, Federal, for Cin- 
namon Extract 48 

Standard, Federal, for Clove 
Extract 49 

Standard, Federal, for Gin- 
ger Extract 44 

Standard, Federal, for 
Lemon Extract 32 

Standard, Federal, Oil of 
Lemon 32 

Standard, Federal, for Pep- 
permint Extract 43 

Standard, Federal, for Rose 
Extract 46 

Standard, Federal, for 
Spearmint Extract 49 

Standard, Federal, for Ter- 
peneless Lemon Extract. 34 

Standard, Federal, for 
Tonka Extract 25 

Standard, Federal, for Va- 
nilla Extract 23 

Standard, Federal, for 
Wintergreen Extract 43 

Storaging of Vanilla Beans 16 

Strawberry Extract, Imita- 
tion of 9 

Synthetical Extracts 8 

Syrup Formula 67 

Syrup Table 71 

Tables of Weights and 
Measures 71 

Tahiti Vanilla Beans 12 

Terpeneless Extract of 
Lemon 8, 34-39 

Terpeneless Lemon Ext, 
Federal Standard 34 

Terpeneless Lemon Ext., 
Formulas 38, 39 

Terpeneless Orange Ext... 8 

Test Percolators for Va- 
nilla Beans 16 

Testing Oil of Lemon 62 



Testing Oil of Cloves 62 

Testing Oil of Almond ... 62 

Testing Methods 61, 62, 63 

Testing Otto of Roses 63 

Testing Vanilla Extract... 31 

Tests for Water, Rules 54 

Thyme Extract 8 

Tonka Extract 8, 25 

Tonka Extract, Federal 
Standard 25 

U. S. Definition of Flavor- 
ing Extracts 8 

Use of Coloring 40 

Vanilla Beans 10, n, 15 

Vanilla Bean Exhaustion.. 17 

Vanilla Bean Storage 16 

Vanilla Beans, Varieties 

10, n, 12, 13 

Vanilla Beans, Where Cul- 
tivated 10 

Vanilla Extract 8, 10, 25 

Vanilla Extract, Federal 

Standard 23 

Vanilla Ext, Formula.. 22, 23 
Vanilla Extract, Manufac- 
ture 10-25 

Vanilla Extract, Testing... 31 

Vanilla Resins 15 

Vanillin 8, 13, 14, 25, 26, 28 

Vanilla Extract 8, 26 

Varieties of Vanilla Beans 10 

Various Extracts 42-49 

Vinegar 65 

Water Tests 54 

Weights and Measures, 

Tables 71 

What Constitutes a Flavor- 
ing Extract 8 

White Vanilla 27 

Wintergreen Extract 8,43 



84 Practical Flavoring Extract Maker 



VANILLA 
-BEANS- 



Not merely VANILLAS but 
a comprehensive stock thor- 
oughly representative of every 
producing district: MEXICO, 
THE BOURBON IS- 
LANDS, TAHITA, GUA- 
DELOUPE, and worthy of 
serious consideration on the 
part of every buyer of round 
lots entire, as received from 
primary sources. Samples for 
inspection cheerfully sent, ex- 
press prepaid. 

TONKA BEANS, VAN- 
ILLIN, COUMARIN, 
ESSENTIAL OILS 



M. L. Barrett & Co. 

223 West Lake Street 
Importers CHICAGO 



Practical Flavoring Extract Maker 



85 



HEADQUARTERS FOR 
MAPLE FLAVOR 



We offer : TRI-MAPLE FLAVOR, a flavor suitable 
for making syrup or to put up in bottles as a general 
household flavoring. A vegetable flavor, pure and 
wholesome. C.CONCENTRATED MAPLE FLA- 
VOR, of very intense MAPLE AROMA. Soluble 
in 50 per cent, alcohol Suitable for making flavor- 
ing extracts. C.We SPECIALIZE ON MAPLE 
FLAVOR and are the ONLY HOUSE making 
Maple Flavor EXCLUSIVELY. C. WRITE US 
about anything you want in Maple Flavor. 

THOMAS HENDERSON 

Manufacturing Chemist 
86 FULTON STREET NEW YORK 



Williamson's Burnt Sugar 
Coloring (Caramel) 

BRILLIANT, SOLUBLE AND UNIFORM. JSuit- 
able for COLORING FLAVORING EXTRACTS 
and ALCOHOLIC PREPARATIONS. QA BRIL- 
LIANT SUGAR COLORING will add to the ap- 
pearance of your extracts, while a poor SUGAR 
COLORING will give your products a "muddy" 
appearance. J The name "WILLIAMSON " stands 
for the best in SUGAR COLORING. CJ Write for 
sample and price. 

D. D. WILLIAMSON & CO. 

Manufacturing Chemists 

86 Fulton St., New York. Works at Long Island City 
The Largest Makers of Burnt Sugar Coloring (Caramel) 



86 Practical Flavoring Extract Maker 



World Labeler Improved 



The machine that does the world's 
labeling. Body labels only or body 
and neck labels at one operation. 
Equipped with special mechanism 
adapted to your own class of work. 
Let us tell you how much World 
Labeler will save you. Send labeled 
samples for quotation to day. 



Economic Machinery Co, 

WORCESTER, MASS., U. S. A. 
Largest makers of labeling machines in the world 



Ungerer & Co/s Vanillin 

Electro-Chemical Process 

Our Vanillin is not an imitation of nature, but an absolute repro- 
duction of the natural aromatic principles of the vanilla bean by 
the combination of the very same elements which have hitherto 
been found only as blended in nature's own laboratory, ^j The 
method of manufacture is an improvement upon approved methods, 
so that we obtain a snow-white and absolutely pure vanillin 
by a harmless electro- chemical process. (|Our vanillin is the 
most perfect product yet obtained and of the highest possible 
strength and aroma. No matter what you have heard or what 
your experience has been with other brands of vanillin, we know 
for a certainty and can prove to you that our Vanillin is superior 
to that produced by all other methods or processes. 

Ungerer & Company 

New York San Francisco Chicago Philadelphia 



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