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Title: Soap-Making Manual

A Practical Handbook on the Raw Materials, Their
Manipulation, Analysis and Control in the Modern Soap Plant.

Author: E. G. Thomssen

Release Date: October 22, 2010 [EBook #34114]

Language: English

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Soap-Making Manual
A practical handbook on the raw materials, their manipulation, analysis
and control in the modern soap plant.

By

E. G. Thomssen, Ph. D.
ILLUSTRATED

NEW YORK

D. VAN NOSTRAND COMPANY

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Eight Warren Street

1922

Copyright 1922

By

D. VAN NOSTRAND COMPANY

Printed in the United States of America

[Pg iii]

PREFATORY NOTE.
The material contained in this work appeared several years ago in serial form in the
American Perfumer and Essential Oil Review. Owing to the numerous requests received,
it has been decided to now place before those interested, these articles in book form.
While it is true that the works pertaining to the soapmaking industry are reasonably
plentiful, books are quite rare, however, which, in a brief volume, will clearly outline the
processes employed together with the necessary methods of analyses from a purely
practical standpoint. In the work presented the author has attempted to briefly, clearly,
and fully explain the manufacture of soap in such language that it might be understood by
all those interested in this industry. In many cases the smaller plants find it necessary to
dispense with the services of a chemist, so that it is necessary for the soapmaker to make
his own tests. The tests outlined, therefore, are given as simple as possible to meet this
condition. The formulae submitted are authentic, and in many cases are now being used
in soapmaking.
In taking up the industry for survey it has been thought desirable to first mention and
describe the raw materials used; second, to outline the processes of manufacture; third, to
classify the methods and illustrate by formulae the composition of various soaps together
with their mode of manufacture; fourth, to enumerate the various methods of glycerine
recovery, including the processes of saponification, and, fifth, to give the most important
analytical methods which are of value to control the process of manufacture and to [Pg iv]
determine the purity and fitness of the raw material entering into it.
It is not the intention of the author to go into great detail in this work, nor to outline to
any great extent the theoretical side of the subject, but rather to make the work as brief as
possible, keeping the practical side of the subject before him and not going into concise
descriptions of machinery as is very usual in works on this subject. Illustrations are
merely added to show typical kinds of machinery used.
The author wishes to take this opportunity of thanking Messrs. L. S. Levy and E. W.
Drew for the reading of proof, and Mr. C. W. Aiken of the Houchin-Aiken Co., for his aid
in making the illustrations a success, as well as others who have contributed in the
compiling of the formulae for various soaps. He trusts that this work may prove of value
to those engaged in soap manufacture.
E. G. T.
January, 1922

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Transcriber's note: This is a series of articles collected into a book.

There are differences in spelling and punctuation in the different
chapters (e.g. cocoanut in one chapter and coconut in another). These
differences were left in the text as they appeared.

TABLE OF CONTENTS. [Pg v]

CHAPTER I. Page.

Raw Materials Used in Soap Making 1-30

1. Soap Defined 1

2. Oils and Fats 1-2

3. Saponification Defined 2-3

4. Fats and Oils Used in Soap Manufacture 3-4

Fullers' Earth Process for Bleaching Tallow 4-6
Method for Further Improvement of Color in Tallow 6
Vegetable Oils 6-9
Chrome Bleaching of Palm Oil 9-12
Air Bleaching of Palm Oil 12-16

5. Rancidity of Oils and Fats 16-18

Prevention of Rancidity 18

6. Chemical Constants of Oils and Fats 18-19

7. Oil Hardening or Hydrogenating 19-21

8. Grease 21-22

9. Rosin (Colophony, Yellow Rosin, Resina) 22-23

10. Rosin Saponification 23-24

11. Naphthenic Acids 24-25

12. Alkalis 25-26

Caustic Soda 26
Caustic Potash 26-28
Sodium Carbonate (Soda Ash) 28-29
Potassium Carbonate 29

13. Additional Material Used in Soap Making 29-30

CHAPTER II.

Construction and Equipment of a Soap Plant 31-34

CHAPTER III.
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Classification of Soap Making Methods 35-46

1. Full Boiled Soaps 36-42

2. Cold Process 43-44

3. Carbonate Saponification 45-46

CHAPTER IV.

Classification of Soaps 47-104

1. Laundry Soap 48
Semi-Boiled Laundry Soap 49-50
Settled Rosin Soap 50-54

2. Chip Soap 54-55 [Pg vi]

Cold Made Chip Soap 55-56
Unfilled Chip Soap 56

3. Soap Powders 56-59

Light Powders 60-61

4. Scouring Powders 61

5. Scouring Soap 61-62

6. Floating Soap 62-65

7. Toilet Soap 65-68

Cheaper Toilet Soaps 68-69
Run and Glued-up Soaps 69-71
Curd Soap 71-72
Cold Made Toilet Soaps 72-73
Perfuming and Coloring Toilet Soaps 73-75
Coloring Soap 75-76

8. Medicinal Soaps 76-77

Sulphur Soaps 77
Tar Soap 77
Soaps Containing Phenols 77-78
Peroxide Soap 78
Mercury Soaps 78
Less Important Medicinal Soaps 78-79

9. Castile Soap 79-81

10. Eschweger Soap 81-82

11. Transparent Soap 82-84

Cold Made Transparent Soap 84-87

12. Shaving Soaps 87-90

Shaving Powder 90
Shaving Cream 90-93

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13. Pumice or Sand Soaps 93-94

14. Liquid Soaps 94-95

15. Use of Hardened Oils in Toilet Soaps 96-98

16. Textile Soaps 98

Scouring and Fulling Soaps for Wool 98-100
Wool Thrower's Soap 100-101
Worsted Finishing Soaps 101
Soaps Used in the Silk Industry 101-103
Soaps Used for Cotton Goods 103-104

17. Sulphonated Oils 104-105

CHAPTER V.

Glycerine Recovery 105-126

1. Methods of Saponification 105-106 [Pg vii]

Recovery of Glycerine from Spent Lye 106-113
Twitchell Process 113-118
Autoclave Saponification 118
Lime Saponification 118-120
Acid Saponification 120-121
Aqueous Saponification 121
Splitting Fats with Ferments 121-123
Krebitz Process 123-125

2. Distillation of Fatty Acids 125-126

CHAPTER VI.

Analytical Methods 127-164

1. Analysis of Oils and Fats 128

Free Fatty Acids 128-130
Moisture 130
Titer 130-132
Determination of Unsaponifiable Matter 132-133
Test for Color of Soap 133-134
Testing of Alkalis Used in Soap Making 134-137

2. Soap Analysis 137-138

Moisture 138-139
Free Alkali or Acid 139-142
Insoluble Matter 143
Starch and Gelatine 143-144
Total Fatty and Resin Acids 144
Determination of Rosin 144-147
Total Alkali 147-148
Unsaponifiable Matter 148
Silica and Silicates 148-149
Glycerine in Soap 149-150
Sugar in Soap 150

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3. Glycerine Analysis 150-151

Sampling 151
Analysis 151-154
Acetin Process for the Determination of Glycerol 155-156
The Method 156-159
Ways of Calculating Actual Glycerol Contents 159-160
Bichromate Process for Glycerol Determination
Reagents Required 160-161
The Method 161-162
Sampling Crude Glycerine 162-164 [Pg viii]

CHAPTER VII

Standard Methods for the Sampling and Analysis of Commercial Fats165-195

and Oils

1. Scope, Applicability and Limitations of the Methods 165-166

Scope 165
Applicability 166
Limitations 166
Sampling 166-169
Tank Cars 166-167
Barrels, Tierces, Casks, Drums, and Other Packages 168

2. Analysis 169-183
Sample 169
Moisture and Volatile Matter 170-172
Insoluble Impurities 172-173
Soluble Mineral Matter 173
Free Fatty Acids 174
Titer 174-175
Unsaponifiable Matter 176-177
Iodine Number-Wijs Method 177-181
Saponification Number (Koettstorfer Number) 181
Melting Point 181-182
Cloud Test 182-184

3. Notes of the Above Methods 184-196

Sampling 183
Moisture and Volatile Matter 184-187
Insoluble Impurities 187
Soluble Mineral Matter 187-188
Free Fatty Acid 188-189
Titer 189
Unsaponified Matter 190-193
Melting Point 193-196

Plant and Machinery 198-219

Illustrations of Machinery and Layouts of the Plant of a Modern Soap Making
Establishment 198-219

Appendix 219-237

Useful Tables

Index 239

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CHAPTER I [Pg 1]

Raw Materials Used in Soap Making.

Soap is ordinarily thought of as the common cleansing agent well known to everyone. In
a general and strictly chemical sense this term is applied to the salts of the non-volatile
fatty acids. These salts are not only those formed by the alkali metals, sodium and
potassium, but also those formed by the heavy metals and alkaline earths. Thus we have
the insoluble soaps of lime and magnesia formed when we attempt to wash in "hard
water"; again aluminum soaps are used extensively in polishing materials and to thicken
lubricating oils; ammonia or "benzine" soaps are employed among the dry cleaners.
Commonly, however, when we speak of soap we limit it to the sodium or potassium salt
of a higher fatty acid.
It is very generally known that soap is made by combining a fat or oil with a water
solution of sodium hydroxide (caustic soda lye), or potassium hydroxide (caustic potash).
Sodium soaps are always harder than potassium soaps, provided the same fat or oil is
used in both cases.
The detergent properties of soap are due to the fact that it acts as an alkali regulator, that
is, when water comes into contact with soap, it undergoes what is called hydrolytic
dissociation. This means that it is broken down by water into other substances. Just what
these substances are is subject to controversy, though it is presumed caustic alkali and the
acid alkali salt of the fatty acids are formed.

OILS AND FATS.

There is no sharp distinction between fat and oil. By "oil" the layman has the impression
of a liquid which at warm temperature will flow as a slippery, lubricating, viscous fluid; [Pg 2]
by "fat" he understands a greasy, solid substance unctuous to the touch. It thus becomes
necessary to differentiate the oils and fats used in the manufacture of soap.
Inasmuch as a soap is the alkali salt of a fatty acid, the oil or fat from which soap is made
must have as a constituent part, these fatty acids. Hydrocarbon oils or paraffines,
included in the term "oil," are thus useless in the process of soap-making, as far as
entering into chemical combination with the caustic alkalis is concerned. The oils and
fats which form soap are those which are a combination of fatty acids and glycerine, the
glycerine being obtained as a by-product to the soap-making industry.

NATURE OF A FAT OR OIL USED IN SOAP MANUFACTURE.

Glycerine, being a trihydric alcohol, has three atoms of hydrogen which are replaceable
by three univalent radicals of the higher members of the fatty acids, e. g.,

OH OR
C3 H5 OH + 3 ROH = C3 H5 OR + 3 H2O
OH OR

Glycerine plus 3 Fatty Alcohols equals Fat or Oil plus 3 Water.

Thus three fatty acid radicals combine with one glycerine to form a true neutral oil or fat
which are called triglycerides. The fatty acids which most commonly enter into
combination of fats and oils are lauric, myristic, palmitic, stearic and oleic acids and form
the neutral oils or triglycerides derived from these, e. g., stearin, palmatin, olein. Mono
and diglycerides are also present in fats.

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SAPONIFICATION DEFINED.

When a fat or oil enters into chemical combination with one of the caustic hydrates in the
presence of water, the process is called "saponification" and the new compounds formed [Pg 3]
are soap and glycerine, thus:

OR OH
C3H5 OR + 3 NaOH = C3H5 OH + 3 NaOR
OR OH

Fat or Oil plus 3 Sodium Hydrate equals Glycerine plus 3 Soap.

It is by this reaction almost all of the soap used today is made.
There are also other means of saponification, as, the hydrolysis of an oil or fat by the
action of hydrochloric or sulfuric acid, by autoclave and by ferments or enzymes. By
these latter processes the fatty acids and glycerine are obtained directly, no soap being
formed.

FATS AND OILS USED IN SOAP MANUFACTURE.

The various and most important oils and fats used in the manufacture of soap are, tallow,
cocoanut oil, palm oil, olive oil, poppy oil, sesame oil, soya bean oil, cotton-seed oil,
corn oil and the various greases. Besides these the fatty acids, stearic, red oil (oleic acid)
are more or less extensively used. These oils, fats and fatty acids, while they vary from
time to time and to some extent as to their color, odor and consistency, can readily be
distinguished by various physical and chemical constants.
Much can be learned by one, who through continued acquaintance with these oils has
thoroughly familiarized himself with the indications of a good or bad oil, by taste, smell,
feel and appearance. It is, however, not well for the manufacturer in purchasing to depend
entirely upon these simpler tests. Since he is interested in the yield of glycerine, the
largest possible yield of soap per pound of soap stock and the general body and
appearance of the finished product, the chemical tests upon which these depend should be [Pg 4]
made. Those especially important are the acid value, percentage unsaponifiable matter
and titer test.
A short description of the various oils and fats mentioned is sufficient for their use in the
soap industry.
Tallow is the name given to the fat extracted from the solid fat or "suet" of cattle, sheep
or horses. The quality varies greatly, depending upon the seasons of the year, the food
and age of the animal and the method of rendering. It comes to the market under the
distinction of edible and inedible, a further distinction being made in commerce as beef
tallow, mutton tallow or horse tallow. The better quality is white and bleaches whiter
upon exposure to air and light, though it usually has a yellowish tint, a well defined grain
and a clean odor. It consists chiefly of stearin, palmitin and olein. Tallow is by far the
most extensively used and important fat in the making of soap.
In the manufacture of soaps for toilet purposes, it is usually necessary to produce as white
a product as possible. In order to do this it often is necessary to bleach the tallow before
saponification. The method usually employed is the Fuller's Earth process.

FULLER'S EARTH PROCESS FOR BLEACHING TALLOW.

From one to two tons of tallow are melted out into the bleaching tank. This tank is
jacketed, made of iron and provided with a good agitator designed to stir up sediment or
a coil provided with tangential downward opening perforations and a draw-off cock at the
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bottom. The coil is the far simpler arrangement, more cleanly and less likely to cause
trouble. By this arrangement compressed air which is really essential in the utilization of
the press (see later) is utilized for agitation. A dry steam coil in an ordinary tank may be
employed in place of a jacketed tank, which lessens the cost of installation. [Pg 5]

The tallow in the bleaching tank is heated to 180° F. (82° C.) and ten pounds of dry salt
per ton of fat used added and thoroughly mixed by agitation. This addition coagulates any
albumen and dehydrates the fat. The whole mass is allowed to settle over night where
possible, or for at least five hours. Any brine which has separated is drawn off from the
bottom and the temperature of the fat is then raised to 160° F. (71° C).
Five per cent. of the weight of the tallow operated upon, of dry Fuller's earth is now
added and the whole mass agitated from twenty to thirty minutes.
The new bleached fat, containing the Fuller's earth is pumped directly to a previously
heated filter press and the issuing clear oil run directly to the soap kettle.
One of the difficulties experienced in the process is the heating of the press to a
temperature sufficient to prevent solidification of the fat without raising the press to too
great a temperature. To overcome this the first plate is heated by wet steam. Air delivered
from a blower and heated by passage through a series of coils raised to a high
temperature by external application of heat (super-heated steam) is then substituted for
the steam. The moisture produced by the condensation of the steam is vaporized by the
hot air and carried on gradually to each succeeding plate where it again condenses and
vaporizes. In this way the small quantity of water is carried through the entire press,
raising its temperature to 80°-100° C. This temperature is subsequently maintained by the
passage of hot air. By this method of heating the poor conductivity of hot air is overcome
through the intermediary action of a liquid vapor and the latent heat of steam is utilized to
obtain the initial rise in temperature. To heat a small press economically where conditions
are such that a large output is not required the entire press may be encased in a small [Pg 6]
wooden house which can be heated by steam coils. The cake in the press is heated for
some time after the filtration is complete to assist drainage. After such treatment the cake
should contain approximately 15 per cent. fat and 25 per cent. water. The cake is now
removed from the press and transferred to a small tank where it is treated with sufficient
caustic soda to convert the fat content into soap.
Saturated brine is then added to salt out the soap, the Fuller's earth is allowed to settle to
the bottom of the tank and the soap which solidifies after a short time is skimmed off to
be used in a cheap soap where color is not important. The liquor underneath may also be
run off without disturbing the sediment to be used in graining a similar cheap soap. The
waste Fuller's earth contains about 0.1 to 0.3 per cent. of fat.

METHOD FOR FURTHER IMPROVEMENT OF COLOR.

A further improvement of the color of the tallow may be obtained by freeing it from a
portion of its free fatty acids, either with or without previous Fuller's earth bleaching.
To carry out this process the melted fat is allowed to settle and as much water as possible
taken off. The temperature is then raised to 160° F. with dry steam and enough saturated
solution of soda ash added to remove 0.5 per cent. of the free fatty acids, while agitating
the mass thoroughly mechanically or by air. The agitation is continued ten minutes, the
whole allowed to settle for two hours and the foots drawn off. The soap thus formed
entangles a large proportion of the impurities of the fat.

VEGETABLE OILS.

Cocoanut Oil, as the name implies, is obtained from the fruit of the cocoanut palm. This
oil is a solid, white fat at ordinary temperature, having a bland taste and a characteristic [Pg 7]
odor. It is rarely adulterated and is very readily saponified. In recent years the price of
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this oil has increased materially because cocoanut oil is now being used extensively for
edible purposes, especially in the making of oleomargarine. Present indications are that
shortly very little high grade oil will be employed for soap manufacture since the demand
for oleomargarine is constantly increasing and since new methods of refining the oil for
this purpose are constantly being devised.
The oil is found in the market under three different grades: (1) Cochin cocoanut oil, the
choicest oil comes from Cochin (Malabar). This product, being more carefully cultivated
and refined than the other grades, is whiter, cleaner and contains a smaller percentage of
free acid. (2) Ceylon cocoanut oil, coming chiefly from Ceylon, is usually of a yellowish
tint and more acrid in odor than Cochin oil. (3) Continental cocoanut oil (Copra,
Freudenberg) is obtained from the dried kernels, the copra, which are shipped to Europe
in large quantities, where the oil is extracted. These dried kernels yield 60 to 70 per cent
oil. This product is generally superior to the Ceylon oil and may be used as a very
satisfactory substitute for Cochin oil, in soap manufacture, provided it is low in free acid
and of good color. The writer has employed it satisfactorily in the whitest and finest of
toilet soaps without being able to distinguish any disadvantage to the Cochin oil. Since
continental oil is usually cheaper than Cochin oil, it is advisable to use it, as occasion
permits.
Cocoanut oil is used extensively in toilet soap making, usually in connection with tallow.
When used alone the soap made from this oil forms a lather, which comes up rapidly but
which is fluffy and dries quickly. A pure tallow soap lathers very much slower but
produces a more lasting lather. Thus the advantage of using cocoanut oil in soap is seen. [Pg 8]
It is further used in making a cocoanut oil soap by the cold process also for "fake" or
filled soaps. The fatty acid content readily starts the saponification which takes place
easily with a strong lye (25°-35° B.). Where large quantities of the oil are saponified care
must be exercised as the soap formed suddenly rises or puffs up and may boil over.
Cocoanut oil soap takes up large quantities of water, cases having been cited where a 500
per cent. yield has been obtained. This water of course dries out again upon exposure to
the air. The soap is harsh to the skin, develops rancidity and darkens readily.
Palm Kernel Oil, which is obtained from the kernels of the palm tree of West Africa, is
used in soap making to replace cocoanut oil where the lower price warrants its use. It
resembles cocoanut oil in respect to saponification and in forming a very similar soap.
Kernel oil is white in color, has a pleasant nutty odor when fresh, but rapidly develops
free acid, which runs to a high percentage.
Palm Oil is produced from the fruit of the several species of the palm tree on the western
coast of Africa generally, but also in the Philippines. The fresh oil has a deep orange
yellow tint not destroyed by saponification, a sweetish taste and an odor of orris root or
violet which is also imparted to soap made from it. The methods by which the natives
obtain the oil are crude and depend upon a fermentation, or putrefaction. Large quantities
are said to be wasted because of this fact. The oil contains impurities in the form of
fermentable fibre and albuminous matter, and consequently develops free fatty acid
rapidly. Samples tested for free acid have been found to have hydrolized completely and
one seldom obtains an oil with low acid content. Because of this high percentage of free
fatty acid, the glycerine yield is small, though the neutral oil should produce
approximately 12 per cent. glycerine. Some writers claim that glycerine exists in the free [Pg 9]
state in palm oil. The writer has washed large quantities of the oil and analyzed the wash
water for glycerine. The results showed that the amount present did not merit its
recovery. Most soap makers do not attempt to recover the glycerine from this oil, when
used alone for soap manufacture.
There are several grades of palm oil in commerce, but in toilet soap making it is
advisable to utilize only Lagos palm oil, which is the best grade. Where it is desired to
maintain the color of the soap this oil produces, a small quantity of the lower or "brass"
grade of palm oil may be used, as the soap made from the better grades of oil gradually
bleaches and loses its orange yellow color.

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Palm oil produces a crumbly soap which cannot readily be milled and is termed "short."
When used with tallow and cocoanut oil, or 20 to 25 per cent. cocoanut oil, it produces a
very satisfactory toilet soap. In the saponification of palm oil it is not advisable to
combine it with tallow in the kettle, as the two do not readily mix.
Since the finished soap has conveyed to it the orange color of the oil, the oil is bleached
before saponification. Oxidation readily destroys the coloring matter, while heat and light
assist materially. The methods generally employed are by the use of oxygen developed by
bichromates and hydrochloric acid and the direct bleaching through the agency of the
oxygen of the air.

CHROME BLEACHING OF PALM OIL.

The chrome process of bleaching palm oil is more rapid and the oxygen thus derived
being more active will bleach oils which air alone cannot. It depends upon the reaction:
Na2Cr2O7 + 8HCl = Cr2Cl6 + 2NaCl + 7O.

in which the oxygen is the active principle. In practice it is found necessary to use an
excess of acid over that theoretically indicated. [Pg 10]

For the best results an oil should be chosen containing under 2 per cent. impurities and a
low percentage of free fatty acids. Lagos oil is best adapted to these requirements. The oil
is melted by open steam from a jet introduced through the bung, the melted oil and
condensed water running to the store tank through two sieves (about 1/8 inch mesh) to
remove the fibrous material and gross impurities. The oil thus obtained contains fine
earthy and fibrous material and vegetable albuminous matter which should be removed,
as far as possible, since chemicals are wasted in their oxidation and they retard the
bleaching. This is best done by boiling the oil for one hour with wet steam and 10 per
cent. solution of common salt (2 per cent. dry salt on weight of oil used) in a lead-lined or
wooden tank. After settling over night the brine and impurities are removed by running
from a cock at the bottom of the vat and the oil is run out into the bleaching tank through
an oil cock, situated about seven inches from the bottom.
The bleaching tank is a lead-lined iron tank of the approximate dimensions of 4 feet deep,
4 feet long and 3-1/2 feet wide, holding about 1-1/2 tons. The charge is one ton. A leaden
outlet pipe is fixed at the bottom, to which is attached a rubber tube closed by a screw
clip. A plug also is fitted into the lead outlet pipe from above. Seven inches above the
lower outlet is affixed another tap through which the oil is drawn off.
The tank is further equipped with a wet steam coil and a coil arranged to allow thorough
air agitation, both coils being of lead. A good arrangement is to use one coil to deliver
either air or steam. These coils should extend as nearly as possible over the entire bottom
of the tank and have a number of small downward perforations, so as to spread the
agitation throughout the mass.
The temperature of the oil is reduced by passing in air to 110° F. and 40 pounds of fine [Pg 11]
common salt per ton added through a sieve. About one-half of the acid (40 pounds of
concentrated commercial hydrochloric acid) is now poured in and this is followed by the
sodium bichromate in concentrated solution, previously prepared in a small lead vat or
earthen vessel by dissolving 17 pounds of bichromate in 45 pounds commercial
hydrochloric acid. This solution should be added slowly and should occupy three hours,
the whole mass being thoroughly agitated with air during the addition and for one hour
after the last of the bleaching mixture has been introduced. The whole mixture is now
allowed to settle for one hour and the exhausted chrome liquors are then run off from the
lower pipe to a waste tank. About 40 gallons of water are now run into the bleached oil
and the temperature raised by open steam to 150° to 160° F. The mass is then allowed to
settle over night.

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One such wash is sufficient to remove the spent chrome liquor completely, provided
ample time is allowed for settling. A number of washings given successively with short
periods of settling do not remove the chrome liquors effectually. The success of the
operation depends entirely upon the completeness of settling.
The wash water is drawn off as before and the clear oil run to storage tanks or to the soap
kettle through the upper oil cock.
The waste liquors are boiled with wet steam and the oil skimmed from the surface, after
which the liquors are run out through an oil trap.
By following the above instructions carefully it is possible to bleach one ton of palm oil
with 17 pounds of bichromate of soda and 85 pounds hydrochloric acid.
The spent liquors should be a bright green color. Should they be of a yellow or brownish
shade insufficient acid has been allowed and more must be added to render the whole of [Pg 12]
the oxygen available.
If low grade oils are being treated more chrome will be necessary, the amount being best
judged by conducting the operation as usual and after the addition of the bichromate,
removing a sample of the oil, washing the sample and noting the color of a rapidly cooled
sample.
A little practice will enable the operator to judge the correspondence between the color to
be removed and the amount of bleaching mixture to be added.
To obtain success with this process the method of working given must be adhered to even
in the smallest detail. This applies to the temperature at which each operation is carried
out particularly.

AIR BLEACHING OF PALM OIL.

The method of conducting this process is identical with the chrome process to the point
where the hydrochloric acid is to be added to the oil. In this method no acid or chrome is
necessary, as the active bleaching agent is the oxygen of the air.
The equipment is similar to that of the former process, except that a wooden tank in
which no iron is exposed will suffice to bleach the oil in. The process depends in rapidity
upon the amount of air blown through the oil and its even distribution. Iron should not be
present or exposed to the oil during bleaching, as it retards the process considerably.
After the impurities have been removed, as outlined under the chrome process, the
temperature of the oil is raised by open steam to boiling. The steam is then shut off and
air allowed to blow through the oil until it is completely bleached, the temperature being
maintained above 150° F. by occasionally passing in steam. Usually a ton of oil is readily
and completely bleached after the air has been passed through it for 18 to 20 hours, [Pg 13]
provided the oil is thoroughly agitated by a sufficient flow of air.
If the oil has been allowed to settle over night, it is advisable to run off the condensed
water and impurities by the lower cock before agitating again the second day.
When the oil has been bleached to the desired color, which can be determined by
removing a sample and cooling, the mass is allowed to settle, the water run off to a waste
tank from which any oil carried along may be skimmed off and the supernatant clear oil
run to the storage or soap kettle.
In bleaching by this process, while the process consumes more time and is not as efficient
in bleaching the lower grade oils, the cost of bleaching is less and with a good oil success
is more probable, as there is no possibility of any of the chrome liquors being present in
the oil. These give the bleached oil a green tint when the chrome method is improperly
conducted and they are not removed.

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Instead of blowing the air through it, the heater oil may be brought into contact with the
air, either by a paddle wheel arrangement, which, in constantly turning, brings the oil into
contact with the air, or by pumping the heated oil into an elevated vessel, pierced with
numerous fine holes from which the oil continuously flows back into the vessel from
which the oil is pumped. While in these methods air, light and heat act simultaneously in
the bleaching of the oil, the equipment required is too cumbersome to be practical.

Recent investigations[1] in bleaching palm oil by oxygen have shown that not only the
coloring matter but the oil itself was affected. In bleaching palm oil for 30 hours with air
the free fatty acid content rose and titer decreased considerably. [Pg 14]

Olive Oil, which comes from the fruit of the olive trees, varies greatly in quality,
according to the method by which it is obtained and according to the tree bearing the
fruit. Three hundred varieties are known in Italy alone. Since the larger portion of olive
oil is used for edible purposes, a lower grade, denatured oil, denatured because of the
tariff, is used for soap manufacture in this country. The oil varies in color from pale green
to golden yellow. The percentage of free acid in this oil varies greatly, though the oil does
not turn rancid easily. It is used mainly in the manufacture of white castile soap.
Olive oil foots, which is the oil extracted by solvents after the better oil is expressed,
finds its use in soap making mostly in textile soaps for washing and dyeing silks and in
the production of green castile soaps.
Other oils, as poppy seed oil, sesame oil, cottonseed oil, rape oil, peanut (arachis) oil, are
used as adulterants for olive oil, also as substitutes in the manufacture of castile soap,
since they are cheaper than olive oil.
Cottonseed Oil is largely used in the manufacture of floating and laundry soaps. It may
be used for toilet soaps where a white color is not desired, as yellow spots appear on a
finished soap in which it has been used after having been in stock a short time.
Corn Oil and Soya Bean Oil are also used to a slight extent in the manufacture of toilet
soaps, although the oils form a soap of very little body. Their soaps also spot yellow on
aging.
Corn oil finds its greatest use in the manufacture of soap for washing automobiles. It is
further employed for the manufacture of cheap liquid soaps.
Fatty Acids are also used extensively in soap manufacture. While the soap manufacturer
prefers to use a neutral oil or fat, since from these the by-product glycerine is obtained, [Pg 15]
circumstances arise where it is an advantage to use the free fatty acids. Red oil (oleic
acid, elaine) and stearic acid are the two fatty acids most generally bought for soap
making. In plants using the Twitchell process, which consists in splitting the neutral fats
and oils into fatty acids and glycerine by dilute sulphuric acid and producing their final
separation by the use of so-called aromatic sulphonic acids, these fatty acids consisting of
a mixture of oleic, stearic, palmitic acids, etc., are used directly after having been purified
by distillation, the glycerine being obtained from evaporating the wash water.
Oleic acid (red oil) and stearic acid are obtained usually by the saponification of oils, fats
and greases by acid, lime or water under pressure or Twitchelling. The fatty acids thus are
freed from their combination with glycerine and solidify upon cooling, after which they
are separated from the water and pressed at a higher or lower temperature. The oleic acid,
being liquid at ordinary temperature, together with some stearic and palmitic acid, is thus
pressed out. These latter acids are usually separated by distillation, combined with the
press cake further purified and sold as stearic acid.
The red oil, sometimes called saponified red oil, is often semi-solid, resembling a soft
tallow, due to the presence of stearic acid. The distilled oils are usually clear, varying in
color from light to a deep brown. Stearic acid, which reaches the trade in slab form,
varies in quality from a soft brown, greasy, crumbly solid of unpleasant odor to a snow
white, wax-like, hard, odorless mass. The quality of stearic acid is best judged by the
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melting point, since the presence of any oleic acid lowers this. The melting point of the
varieties used in soap manufacture usually ranges from 128° to 132° F. Red oil is used in
the manufacture of textile soaps, replacing olive oil foots soap for this purpose, [Pg 16]
chlorophyll being used to color the soap green. Stearic acid, being the hard firm fatty
acid, may be used in small quantities to give a better grade of soap body and finish. In
adding this substance it should always be done in the crutcher, as it will not mix in the
kettle. It finds its largest use for soap, however, in the manufacture of shaving soaps and
shaving creams, since it produces the non-drying creamy lather so greatly desired for this
purpose. Both red oil and stearic acid being fatty acids, readily unite with the alkali
carbonates, carbon dioxide being formed in the reaction and this method is extensively
used in the formation of soap from them.

RANCIDITY OF OILS AND FATS.

Rancidity in neutral oils and fats is one of the problems the soap manufacturer has to
contend with. The mere saying that an oil is rancid is no indication of its being high in
free acid. The two terms rancidity and acidity are usually allied. Formerly, the acidity of a
fat was looked upon as the direct measure of its rancidity. This idea is still prevalent in
practice and cannot be too often stated as incorrect. Fats and oils may be acid, or rancid,
or acid and rancid. In an acid fat there has been a hydrolysis of the fat and it has
developed a rather high percentage of free acid. A rancid fat is one in which have been
developed compounds of an odoriferous nature. An acid and rancid fat is one in which
both free acid and organic compounds of the well known disagreeable odors have been
produced.
It cannot be definitely stated just how this rancidity takes place, any more than just what
are the chemical products causing rancidity. The only conclusion that one may draw is
that the fats are first hydrolyzed or split up into glycerine and free fatty acids. This is
followed by an oxidation of the products thus formed. [Pg 17]

Moisture, air, light, enzymes (organized ferments) and bacteria are all given as causes of
rancidity.
It seems very probable that the initial splitting of the fats is caused by enzymes, which
are present in the seeds and fruits of the vegetable oils and tissue of animal fats, in the
presence of moisture. Lewkowitsch strongly emphasizes this point and he is substantiated
in his idea by other authorities. Others hold that bacteria or micro-organisms are the
cause of this hydrolysis, citing the fact that they have isolated various micro-organisms
from various fats and oils. The acceptance of the bacterial action would explain the
various methods of preservation of oils and fats by the use of antiseptic preparations. It
cannot, however, be accepted as a certainty that bacteria cause the rancidity of fats.
The action of enzymes is a more probable explanation.
The hydrolysis of fats and oils is accelerated when they are allowed to remain for some
time in the presence of organic non-fats. Thus, palm oil, lower grades of olive oil, and
tallow, which has been in contact with the animal tissue for a long time, all contain other
nitrogenous matter and exhibit a larger percentage of free fatty acid than the oils and fats
not containing such impurities.
Granting this initial splitting of the fat into free fatty acids and glycerine, this is not a
sufficient explanation. The products thus formed must be acted upon by air and light. It is
by the action of these agents that there is a further action upon the products, and from this
oxidation we ascertain by taste and smell (chemical means are still unable to define
rancidity) whether or not a fat is rancid. While some authorities have presumed to isolate
some of these products causing rancidity, we can only assume the presence of the various
possible compounds produced by the action of air and light which include oxy fatty [Pg 18]
acids, lactones, alcohols, esters, aldehydes and other products.

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The soap manufacturer is interested in rancidity to the extent of the effect upon the
finished soap. Rancid fats form darker soaps than fats in the neutral state, and very often
carry with them the disagreeable odor of a rancid oil. Further, a rancid fat or oil is usually
high in free acid. It is by no means true, however, that rancidity is a measure for acidity,
for as has already been pointed out, an oil may be rancid and not high in free acid.
The percentage of free fatty acid is of even greater importance in the soap industry. The
amount of glycerine yield is dependent upon the percentage of free fatty acid and is one
of the criterions of a good fat or oil for soap stock.

PREVENTION OF RANCIDITY.
Since moisture, air, light and enzymes, produced by the presence of organic impurities,
are necessary for the rancidity of a fat or oil, the methods of preventing rancidity are
given. Complete dryness, complete purification of fats and oils and storage without
access of air or light are desirable. Simple as these means may seem, they can only be
approximated in practice. The most difficult problem is the removal of the last trace of
moisture. Impurities may be lessened very often by the use of greater care. In storing it is
well to store in closed barrels or closed iron tanks away from light, as it has been
observed that oils and fats in closed receptacles become rancid less rapidly than those in
open ones, even though this method of storing is only partially attained. Preservatives are
also used, but only in edible products, where their effectiveness is an open question.

CHEMICAL CONSTANTS OF OILS AND FATS.

Besides the various physical properties of oils and fats, such as color, specific gravity, [Pg 19]
melting point, solubility, etc., they may be distinguished chemically by a number of
chemical constants. These are the iodine number, the acetyl value, saponification number,
Reichert-Meissl number for volatile acids, Hehner number for insoluble acids. These
constants, while they vary somewhat with any particular oil or fat, are more applicable to
the edible products and are criterions where any adulteration of fat or oil is suspected.
The methods of carrying out the analyses of oils and fats to obtain these constants are
given in the various texts[2] on oils and fats, and inasmuch as they are not of great
importance to the soap industry they are merely mentioned here.

OIL HARDENING OR HYDROGENATING.

It is very well known that oils and fats vary in consistency and hardness, depending upon
the glycerides forming same. Olein, a combination of oleic acid and glycerine, as well as
oleic acid itself largely forms the liquid portion of oils and fats. Oleic acid (C18H34O2) is
an unsaturated acid and differs from stearic acid (C18H36O2), the acid forming the hard
firm portion of oils and fats, by containing two atoms of hydrogen less in the molecule.
Theoretically it should be a simple matter to introduce two atoms of hydrogen into oleic
acid or olein, and by this mere addition convert liquid oleic acid and olein into solid
stearic acid and stearine.
For years this was attempted and all attempts to apply the well known methods of
reduction (addition of hydrogen) in organic chemistry, such as treatment with tin and
acid, sodium amalgam, etc., were unsuccessful. In recent years, however, it has been
discovered that in the presence of a catalyzer, nickel in finely divided form or the oxides [Pg 20]
of nickel are usually employed, the process of hydrogenating an oil is readily attained
upon a practical basis.
The introduction of hardened oils has opened a new source of raw material for the soap
manufacturer in that it is now possible to use oils in soap making which were formerly
discarded because of their undesirable odors. Thus fish or train oils which had up to the
time of oil hydrogenating resisted all attempts of being permanently deodorized, can now
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be employed very satisfactorily for soap manufacture. A Japanese chemist, Tsujimoto[3]

has shown that fish oils contain an unsaturated acid of the composition C18H28O2, for
which he proposed the name clupanodonic acid. By the catalytic hardening of train oils
this acid passes to stearic acid and the problem of deodorizing these oils is solved.[4]
At first the introduction of hardened oils for soap manufacture met with numerous
objections, due to the continual failures of obtaining a satisfactory product by the use of
same. Various attempts have now shown that these oils, particularly hardened train oils,
produce extraordinarily useful materials for soap making. These replace expensive tallow
and other high melting oils. It is of course impossible to employ hardened oils alone, as a
soap so hard would thus be obtained that it would be difficultly soluble in water and
possess very little lathering quality. By the addition of 20-25% of tallow oil or some other
oil forming a soft soap a very suitable soap for household use may be obtained. Ribot[5]
discusses this matter fully. Hardened oils readily saponify, may be perfumed without any [Pg 21]
objections and do not impart any fishy odor to an article washed with same.
Meyerheim[6] states that through the use of hydrogenated oils the hardness of soap is
extraordinarily raised, so that soap made from hardened cottonseed oil is twelve times as
hard as the soap made from ordinary cottonseed oil. This soap is also said to no longer
spot yellow upon aging, and as a consequence of its hardness, is able to contain a
considerably higher content of rosin through which lathering power and odor may be
improved. Hardened oils can easily be used for toilet soap bases, provided they are not
added in too great a percentage.
The use of hardened oils is not yet general, but there is little doubt that the introduction of
this process goes a long way toward solving the problem of cheaper soap material for the
soap making industry.

GREASE.

Grease varies so greatly in composition and consistency that it can hardly be classed as a
distinctive oil or fat. It is obtained from refuse, bones, hides, etc., and while it contains
the same constituents as tallow, the olein content is considerably greater, which causes it
to be more liquid in composition. Grease differs in color from an off-white to a dark
brown. The better qualities are employed in the manufacture of laundry and chip soap,
while the poorer qualities are only fit for the cheapest of soaps used in scrubbing floors
and such purposes. There is usually found in grease a considerable amount of gluey
matter, lime and water. The percentage of free fatty acid is generally high.
The darker grades of grease are bleached before being used. This is done by adding a
small quantity of sodium nitrate to the melted grease and agitating, then removing the [Pg 22]
excess saltpeter by decomposing with sulphuric acid. A better method of refining,
however, is by distillation. The chrome bleach is also applicable.

ROSIN (COLOPHONY, YELLOW ROSIN, RESINA).

Rosin is the residue which remains after the distillation of turpentine from the various
species of pines. The chief source of supply is in the States of Georgia North and South
Carolina. It is a transparent, amber colored hard pulverizable resin. The better grades are
light in color and known as water white (w. w.) and window glass (w. g.). These are
obtained from a tree which has been tapped for the first year. As the same trees are tapped
from year to year, the product becomes deeper and darker in color until it becomes almost
black.
The constituents of rosin are chiefly (80-90%) abietic acid or its anhydride together with
pinic and sylvic acids. Its specific gravity is 1.07-1.08, melting point about 152.5 C., and
it is soluble in alcohol, ether, benzine, carbon disulfide, oils, alkalis and acetic acid. The
main use of rosin, outside of the production of varnishes, is in the production of laundry

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soaps, although a slight percentage acts as a binder and fixative for perfumes in toilet
soaps and adds to their detergent properties. Since it is mainly composed of acids, it
readily unites with alkaline carbonates, though the saponification is not quite complete
and the last portion must be completed through the use of caustic hydrates, unless an
excess of 10% carbonate over the theoretical amount is used. A lye of 20° B. is best
adapted to the saponification of rosin when caustic hydrates are employed for this
purpose, since weak lyes cause frothing. While it is sometimes considered that rosin is an
adulterant for soap, this is hardly justifiable, as it adds to the cleansing properties of soap.
Soaps containing rosin are of the well known yellowish color common to ordinary [Pg 23]
laundry soaps. The price of rosin has so risen in the last few years that it presents a
problem of cost to the soap manufacturer considering the price at which laundry soaps
are sold.

ROSIN SAPONIFICATION.
As has been stated, rosin may be saponified by the use of alkaline carbonates. On account
of the possibility of the soap frothing over, the kettle in which the operation takes place
should be set flush with the floor, which ought to be constructed of cement. The kettle
itself is an open one with round bottom, equipped with an open steam coil and skimmer
pipe, and the open portion is protected by a semi-circular rail. A powerful grid, having a
3-inch mesh, covers one-half of the kettle, the sharp edges protruding upwards.
The staves from the rosin casks are removed at the edge of the kettle, the rosin placed on
the grid and beaten through with a hammer to break it up into small pieces.
To saponify a ton of rosin there are required 200 lbs. soda ash, 1,600 lbs. water and 100
lbs. salt. Half the water is run into the kettle, boiled, and then the soda ash and half the
salt added. The rosin is now added through the grid and the mixture thoroughly boiled.
As carbon dioxide is evolved by the reaction the boiling is continued for one hour to
remove any excess of this gas. A portion of the salt is gradually added to grain the soap
well and to keep the mass in such condition as to favor the evolution of gas. The
remainder of the water is added to close the soap and boiling continued for one or two
hours longer. At this point the kettle must be carefully watched or it will boil over
through the further escape of carbon dioxide being hindered. The mass, being in a frothy [Pg 24]
condition, will rapidly settle by controlling the flow of steam. The remaining salt is then
scattered in and the soap allowed to settle for two hours or longer. The lyes are then
drained off the top. If the rosin soap is required for toilet soaps, it is grained a second
time. The soap is now boiled with the water caused by the condensation of the steam,
which changes it to a half grained soap suitable for pumping. A soap thus made contains
free soda ash 0.15% or less, free rosin about 15%. The mass is then pumped to the kettle
containing the soap to which it is to be added at the proper stage. The time consumed in
thus saponifying rosin is about five hours.

NAPHTHENIC ACIDS.

The naphtha or crude petroleum of the various provinces in Europe, as Russia, Galacia,
Alsace and Roumania yield a series of bodies of acid character upon refining which are
designated under the general name of naphthenic acids. These acids are retained in
solution in the alkaline lyes during the distillation of the naphtha in the form of alkaline
naphthenates. Upon adding dilute sulphuric acid to these lyes the naphthenates are
decomposed and the naphthenic acids float to the surface in an oily layer of characteristic
disagreeable odor and varying from yellow to brown in color[7]. In Russia particularly
large quantities of these acids are employed in the manufacture of soap.

The soaps formed from naphthenic acids have recently been investigated[8] and found to
resemble the soaps made from cocoanut oil and palm kernel oil, in that they are difficult [Pg 25]
to salt out and dissociate very slightly with water. The latter property makes them
valuable in textile industries when a mild soap is required as a detergent, e. g., in the silk
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industry. These soaps also possess a high solvent power for mineral oils and emulsify
very readily. The mean molecular weight of naphthenic acids themselves is very near that
of the fatty acids contained in cocoanut oil, and like those of cocoanut oil a portion of the
separated acids are volatile with steam. The iodine number indicates a small content of
unsaturated acids.
That naphthenic acids are a valuable soap material is now recognized, but except in
Russia the soap is not manufactured to any extent at the present time.

ALKALIS.
The common alkali metals which enter into the formation of soap are sodium and
potassium. The hydroxides of these metals are usually used, except in the so called
carbonate saponification of free fatty acids in which case sodium and potassium
carbonate are used. A water solution of the caustic alkalis is known as lye, and it is as
lyes of various strengths that they are added to oils and fats to form soap. The density or
weight of a lye is considerably greater than that of water, depending upon the amount of
alkali dissolved, and its weight is usually determined by a hydrometer. This instrument is
graduated by a standardized scale, and while all hydrometers should read alike in a liquid
of known specific gravity, this is generally not the case, so that it is advisable to check a
new hydrometer for accurate work against one of known accuracy. In this country the
Baumé scale has been adopted, while in England a different graduation known as the
Twaddle scale is used. The strength of a lye or any solution is determined by the distance
the instrument sinks into the solution, and we speak of the strength of a solution as so [Pg 26]
many degrees Baumé or Twaddle which are read to the point where the meniscus of the
lye comes on the graduated scale. Hydrometers are graduated differently for liquids of
different weights. In the testing of lyes one which is graduated from 0° to 50° B. is
usually employed.
Caustic soda is received by the consumer in iron drums weighing approximately 700 lbs.
each. The various grades are designated as 60, 70, 74, 76 and 77%. These percentages
refer to the percentage of sodium oxide (Na2O) in 100 parts of pure caustic soda formed
by the combination of 77-1/2 parts of sodium oxide and 22-1/2 parts of water, 77-1/2%
being chemically pure caustic soda. There are generally impurities present in commercial
caustic soda. These consist of sodium carbonate, sodium chloride or common salt and
sometimes lime. It is manufactured by treating sodium carbonate in an iron vessel with
calcium hydroxide or slaked lime, or by electrolysis of common salt. The latter process
has yet been unable to compete with the former in price. Formerly all the caustic soda
used in soap making was imported, and it was only through the American manufacturer
using a similar container to that used by foreign manufacturers that they were able to
introduce their product. This prejudice has now been entirely overcome and most of the
caustic soda used in this country is manufactured here.

CAUSTIC POTASH.

The output of the salts containing potassium is controlled almost entirely by Germany.
Formerly the chief source of supply of potassium compounds was from the burned ashes
of plants, but about fifty years ago the inexhaustible salt mines of Stassfurt, Germany,
were discovered. The salt there mined contains, besides the chlorides and sulphates of [Pg 27]
sodium, magnesium, calcium and other salts, considerable quantities of potassium
chloride, and the Stassfurt mines at present are practically the entire source of all
potassium compounds, in spite of the fact that other localities have been sought to
produce these compounds on a commercial basis, especially by the United States
government.
After separating the potassium chloride from the magnesium chloride and other
substances found in Stassfurt salts the methods of manufacture of caustic potash are
identical to those of caustic soda. In this case, however, domestic electrolytic caustic
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potash may be purchased cheaper than the imported product and it gives results equal to
those obtained by the use of the imported article, opinions to the contrary among soap
makers being many. Most of the caustic potash in the United States is manufactured at
Niagara Falls by the Niagara Alkali Co., and the Hooker Electrochemical Co., chlorine
being obtained as a by-product. The latter concern employs the Townsend Cell, for the
manufacture of electrolytic potash, and are said to have a capacity for making 64 tons of
alkali daily.
Since the molecular weight of caustic potash (56) is greater than that of caustic soda (40)
more potash is required to saponify a pound of fat. The resulting potash soap is
correspondingly heavier than a soda soap. When salt is added to a potassium soap double
decomposition occurs, the potassium soap being transformed to a sodium soap and the
potassium uniting with the chlorine to form potassium chloride. This was one of the
earliest methods of making a hard soap, especially in Germany, where potash was derived
from leeching ashes of burned wood and plants. [Pg 28]

SODIUM CARBONATE (SODA ASH).

While carbonate of soda is widely distributed in nature the source of supply is entirely
dependent upon the manufactured product. Its uses are many, but it is especially
important to the soap industry in the so called carbonate saponification of free fatty acids,
as a constituent of soap powders, in the neutralization of glycerine lyes and as a filler for
laundry soaps.
The old French Le Blanc soda process, which consists in treating common salt with
sulphuric acid and reducing the sodium sulphate (salt cake) thus formed with carbon in
the form of charcoal or coke to sodium sulphide, which when treated with calcium
carbonate yields a mixture of calcium sulphide and sodium carbonate (black ash) from
which the carbonate is dissolved by water, has been replaced by the more recent Solvay
ammonia soda process. Even though there is a considerable loss of salt and the by-
product calcium chloride produced by this process is only partially used up as a drying
agent, and for refrigerating purposes, the Le Blanc process cannot compete with the
Solvay process, so that the time is not far distant when the former will be considered a
chemical curiosity. In the Solvay method of manufacture sodium chloride (common salt)
and ammonium bicarbonate are mixed in solution. Double decomposition occurs with the
formation of ammonium chloride and sodium bicarbonate. The latter salt is
comparatively difficultly soluble in water and crystallizes out, the ammonium chloride
remaining in solution. When the sodium bicarbonate is heated it yields sodium carbonate,
carbon dioxide and water; the carbon dioxide is passed into ammonia which is set free
from the ammonium chloride obtained as above by treatment with lime (calcium oxide)
calcium chloride being the by-product. [Pg 29]

Sal soda or washing soda is obtained by recrystallizing a solution of soda ash in water.
Large crystals of sal soda containing but 37% sodium carbonate are formed.

POTASSIUM CARBONATE.

Potassium carbonate is not extensively used in the manufacture of soap. It may be used in
the forming of soft soaps by uniting it with free fatty acids. The methods of manufacture
are the same as for sodium carbonate, although a much larger quantity of potassium
carbonate than carbonate of soda is obtained from burned plant ashes. Purified potassium
carbonate is known as pearl ash.

ADDITIONAL MATERIAL USED IN SOAP MAKING.

Water is indispensable to the soap manufacturer. In the soap factory hard water is often
the cause of much trouble. Water, which is the best solvent known, in passing through the
crevices of rocks dissolves some of the constituents of these, and the water is known as
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hard. This hardness is of two kinds, temporary and permanent. Temporarily hard water is
formed by water, which contains carbonic acid, dissolving a portion of calcium carbonate
or carbonate of lime. Upon boiling, the carbonic acid is driven from the water and the
carbonate, being insoluble in carbon dioxide free water, is deposited. This is the cause of
boiler scale, and to check this a small amount of sal ammoniac may be added to the
water, which converts the carbonate into soluble calcium chloride and volatile
ammonium carbonate. Permanent hardness is caused by calcium sulphate which is
soluble in 400 parts of water and cannot be removed by boiling.
The presence of these salts in water form insoluble lime soaps which act as inert bodies
as far as their value for the common use of soap is concerned. Where the percentage of
lime in water is large this should be removed. A method generally used is to add about [Pg 30]
5% of 20° B. sodium silicate to the hard water. This precipitates the lime and the water is
then sufficiently pure to use.
Salt, known as sodium chloride, is used to a large extent in soap making for "salting out"
the soap during saponification, as well as graining soaps. Soap ordinarily soluble in water
is insoluble in a salt solution, use of which is made by adding salt to the soap which goes
into solution and throws any soap dissolved in the lyes out of solution. Salt may contain
magnesium and calcium chlorides, which of course are undesirable in large amounts. The
products on the market, however, are satisfactory, thus no detail is necessary.
Filling materials used are sodium silicate, or water glass, talc, silex, pumice, starch,
borax, tripoli, etc.
Besides these other materials are used in the refining of the oils and fats, and glycerine
recovery, such as Fuller's earth, bichromates of soda or potash, sulphate of alumina,
sulphuric and hydrochloric acids and alcohol.
A lengthy description of these substances is not given, as their modes of use are detailed
elsewhere.

FOOTNOTES:
[1] Seifensieder Zeit, 1913, 40, p. 687, 724, 740.
[2] Official Methods, see Bull. 107, A. O. A. C., U. S. Dept. Agricult.
[3] Journ. Coll. of Engin. Tokyo Imper. Univ. (1906), p. 1. Abs. Chem. Revue f. d.
Fett-u. Harz, Ind. 16, p. 84; 20, p. 8.
[4] Meyerheim—Fort. der Chem., Physik. und Physik. Chem. (1913), 8. 6, p. 293-
307.
[5] Seifs. Ztg. (1913), 40, p. 142.
[6] Loc. cit.
[7] Les Matieres Graisses (1914), 7, 69, p. 3367.
[8] Zeit. f. Angew. Chem. (1914), 27, 1, p. 2-4.

CHAPTER II [Pg 31]

Construction and Equipment of a Soap Plant.

No fixed plan for the construction and equipment of a soap plant can be given. The
specifications for a soap factory to be erected or remodeled must suit the particular cases.
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Very often a building which was constructed for a purpose other than soap manufacture
must be adapted for the production of soap. In either case it is a question of engineering
and architecture, together with the knowledge obtained in practice and the final decision
as to the arrangement is best solved by a conference with those skilled in each of these
branches.
An ideal soap plant is one in which the process of soap making, from the melting out of
the stock to the packing and shipping of the finished product, moves downward from
floor to floor, since by this method it is possible to utilize gravitation rather than pumping
liquid fats and fluid soaps. Convenience and economy are obtained by such an
arrangement.
The various machinery and other equipment for soap manufacture are well known to
those connected with this industry. It varies, of course, depending upon the kind of soap
to be manufactured, and full descriptions of the necessary machinery are best given in the
catalogs issued by the manufacturers of such equipment, who in this country are most
reliable.
To know just what equipment is necessary can very easily be described by a brief outline
of the process various soaps undergo to produce the finished article. After the
saponification has taken place in the soap kettle the molten soap is run directly into the
soap frames, which consist of an oblong compartment, holding anywhere from 400 to [Pg 32]
1,200 pounds, with removable steel sides and mounted upon trucks, in which it solidifies.
In most cases it is advisable to first run the soap into a crutcher or mixer which produces
a more homogeneous mass than if this operation is omitted. Color and perfume may also
be added at this point, although when a better grade of perfume is added it must be
remembered that there is considerable loss due to volatilization of same. When a drying
machine is employed the molten soap is run directly upon the rollers of this machine,
later adding about 1.0% zinc oxide to the soap from which it passes continuously through
the drying chamber and is emitted in chip form ready for milling. After the soap has been
framed, it is allowed to cool and solidify, which takes several days, and then the sides of
the frame are stripped off. The large solid cake is cut with wires by hand or by a slabber
into slabs of any desired size. These slabs are further divided into smaller divisions by the
cutting table. In non-milled soaps (laundry soaps, floating soaps, etc.), these are pressed
at this stage, usually by automatic presses, after a thin hard film has been formed over the
cake by allowing it to dry slightly. In making these soaps they are not touched by hand at
any time during the operation, the pressing, wrapping and packing all being done by
machinery. For a milled soap the large slabs are cut into narrow oblong shapes by means
of the cutting table to readily pass into the feeder of the chipper, the chips being spread
upon trays and dried in a dry house until the moisture content is approximately 15%.
The process of milling is accomplished by passing the dried soap chips through a soap
mill, which is a machine consisting of usually three or four contiguous, smooth, granite [Pg 33]
rollers operated by a system of gears and set far enough apart to allow the soap to pass
from a hopper to the first roller, from which it is constantly conveyed to each succeeding
roller as a thin film, and finally scraped from the last roller to fall into the milling box in
thin ribbon form. These mills are often operated in tandem, which necessitates less
handling of soap by the operator. The object of milling is to give the soap a glossy,
smooth finish and to blend it into a homogeneous mass. The perfume, color, medication
or any other material desired are added to the dried soap chips prior to milling. Some
manufacturers use an amalgamator to distribute these uniformly through the soap, which
eliminates at least one milling. When a white soap is being put through the mill, it is
advisable to add from 0.5% to 1% of a good, fine quality of zinc oxide to the soap, if this
substance has not been previously added. This serves to remove the yellowish cast and
any translucency occasioned by plodding. Too great a quantity of this compound added,
later exhibits itself by imparting to the soap a dead white appearance. Inasmuch as the
milling process is one upon which the appearance of a finished cake of toilet soap largely
depends, it should be carefully done. The number of times a soap should be milled
depends upon the character of a soap being worked. It should of course be the object to
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mill with as high a percentage of moisture as possible. Should the soap become too dry it
is advisable to add water directly, rather than wet soap, since water can more easily be
distributed through the mass. As a general statement it may be said it is better policy to
overmill a soap, rather than not mill it often enough.
After the soap has been thoroughly milled it is ready for plodding. A plodder is so
constructed as to take the soap ribbons fed into the hopper by means of a worm screw [Pg 34]
and continuously force it under great pressure through a jacketed cylinder through which
cold water circulates in the rear to compensate the heat produced by friction and hot
water at the front, to soften and polish the soap which passes out in solid form in bars of
any shape and size depending upon the form of the shaping plate through which it is
emitted. The bars run upon a roller board, are cut into the required length by a special
cake cutting table, allowed to dry slightly and pressed either automatically or by a foot
power press in any suitable soap die. The finished cake is then ready for wrapping and
after due time in stock reaches the consumer.
Besides the various apparatus mentioned above there are many other parts for the full
equipment of a modern soap plant, such as remelters, pumps, mixers, special tanks,
power equipment, etc. As has been stated, however, practical experience will aid in
judging the practicability as to installation of these. The various methods of powdering
soap are, however, not generally known. Where a coarse powder is to be produced, such
as is used for common washing powders, no great difficulty is experienced with the well
known Blanchard mill. In grinding soap to an impalpable powder the difficulties
increase. The methods adapted in pulverizing soaps are by means of disintegrators,
pebble mills and chaser mills. The disintegrator grinds by the principle of attrition, that is,
the material is reduced by the particles being caused to beat against each other at great
velocity; a pebble mill crushes the substance by rubbing it between hard pebbles in a
slowly revolving cylinder; the chaser mill first grinds the material and then floats it as a
very fine powder above a curb of fixed height. The last method is particularly adapted for
the finest of powder (140 mesh and over).

CHAPTER III [Pg 35]

Classification of Soap-Making Methods.

In the saponification of fats and oils to form soap through the agency of caustic alkalis, as
has been stated, the sodium or potassium salts of the mixed fatty acids are formed.
Sodium soaps are usually termed hard soaps, and potassium soaps soft. There are,
however, a great many varieties of soaps the appearance and properties of which depend
upon their method of manufacture and the oils or fats used therein.
The various methods adopted in soap making may be thus classified:
1. Boiling the fats and oils in open kettles by open steam with indefinite quantities of
caustic alkali solutions until the finished soap is obtained; ordinarily named full boiled
soaps. These may be sub-divided into (a) hard soaps with sodium hydrate as a base, in
which the glycerine is recovered from the spent lyes; (b) hard soaps with soda as a base,
in which the glycerine remains in the soap, e. g., marine cocoanut oil soaps; (c) soft
potash soaps, in which the glycerine is retained by the soap.
2. Combining the required amount of lye for complete saponification of a fat therewith,
heating slightly with dry heat and then allowing the saponification to complete itself.
This is known as the cold process.
3. Utilizing the fatty acid, instead of the neutral fat, and combining it directly with caustic
alkali or carbonate, which is incorrectly termed carbonate saponification, since it is
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merely neutralizing the free fatty acid and thus is not a saponification in the true sense of
the word. No glycerine is directly obtained by this method, as it is usually previously [Pg 36]
removed in the clearage of the fat by either the Twitchell or autoclave saponification
method.
In the methods thus outlined the one most generally employed is the full boiled process
to form a sodium soap. This method of making soap requires close attention and a
knowledge which can only be obtained by constant practice. The stock, strength of lyes,
heat, amount of salt or brine added, time of settling, etc., are all influencing factors.
The principles involved in this process are briefly these:
The fat is partly saponified with weak lyes (usually those obtained from a previous
boiling in the strengthening change are used), and salt is added to grain the soap. The
mass is then allowed to settle into two layers. The upper layer is partly saponified fat; the
lower layer, or spent lye, is a solution of salt, glycerine, and contains any albuminous
matter or any other impurity contained in the fat. This is known as the killing or glycerine
change. Strong lyes are now added and the fat entirely saponified, which is termed the
strengthening change. The mass is then allowed to settle and the fluid soap run off above
the "nigre." This operation is called the finish or finishing change.
The method may be more fully illustrated by a concrete example of the method of
manufacture of a tallow base:

Charge—
Tallow 88 per cent.
Cocoanut oil 10 per cent.
Rosin w. w. 2 per cent.
Amount charge 10 tons

About five tons of tallow and one ton of cocoanut oil are pumped or run into the soap
kettle and brought to a boil with wet steam until it briskly comes through the hot fat. The
caustic soda (strengthening lyes from former boilings may be used here) is gradually [Pg 37]
added by the distributing pipe, any tendency to thicken being checked by the introduction
of small quantities of brine ("salt pickle"). If the lye is added too rapidly the soap
assumes a granular appearance, indicating that the addition of same must be
discontinued. Water should then be added and the mass boiled through until it again
closes. When the addition of the proper amount of caustic soda is nearing its completion
the soap gradually thins. The steam is now cut down to about one turn of the valve, and
brine is rapidly added or salt shoveled in. In ten to fifteen minutes the steam again breaks
through and, from the appearance of the soap, it can be seen whether sufficient brine has
been added. A sample taken out by means of a long wooden paddle should show the soap
in fine grains with the lyes running from it clear. The steam is then shut off and the soap
allowed to settle from one and one-half to two hours. In all settlings the longer time this
operation is permitted to continue, the better will the subsequent operations proceed.
The mixture now consists of a partly saponified layer of fat above the spent lyes. The lyes
are drawn off until soap makes its appearance at the exit pipe. The valve is then closed
and the soap blown back into the kettle by steam. The lyes thus obtained are known as
spent lyes, from which the glycerine is recovered. They should show an alkalinity of
approximately 0.5 per cent. if the operation is carefully carried out.
The remaining tallow is now added and the above operations repeated.
After the spent lyes have been drawn off, the soap is closed with water and the proper
percentage of rosin soap previously formed, or rosin itself is added to the mass in the
kettle. More lye is then allowed to flow in until the mixture is up to "strength." This is [Pg 38]
usually tested by the "bite" on the tongue of a small cooled sample. After boiling until the
steam comes through, the mass is grained with salt as before and allowed to settle one
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and one-half to three hours. These lyes, known as strengthening lyes are run to storage to
be used subsequently with fresh fat to take up the caustic soda contained therein.
The soap is now ready for finishing and is first boiled through and tried for strength. A
drop of phenolphthalein (1 per cent. phenolphthalein in 98 per cent. alcohol) is allowed to
drop on the molten soap taken up on a trowel. The red color should be instantly produced
and develop to a full deep crimson in a few seconds, or more lye must be added until this
condition is realized. Should it flash a deep crimson immediately it is on the strong side.
This cannot be conveniently remedied; it can only serve as a guide for the next boil, but
in any case it is not of any serious consequence, unless it is too strong.
With the steam on, the soap is now examined with a trowel which must be thoroughly
heated by working it about under the surface of the hot soap. The appearance of the soap
as it runs from the face of the trowel indicates its condition. It is not possible to
absolutely describe the effect, which can only be properly judged by practice, yet the
following points may serve as a guide. The indications to be noticed are the shape and
size of the flakes of soap as the sample on the trowel breaks up and runs from the hot iron
surface, when the latter is turned in a vertical position, as well as the condition of the iron
surface from which the soap flakes have fallen. A closed soap will run slowly into a
homogeneous sheet, leaving the trowel's surface covered with a thin layer of transparent
soap; a grained mass will run rapidly down in tiny grains, about one-half an inch in
diameter or less, leaving the hot trowel absolutely dry. The object of the finish is to [Pg 39]
separate the soaps of the lower fatty acids from those of the higher, and both from excess
of liquid. A point midway between "open" and "closed" is required to arrive at this point.
Having arrived at the above condition, the soap is allowed to settle anywhere from one to
three days and then run off through the skimmer pipes to the nigre and framed or pumped
to the tank feeding the drying machine.
The stock thus obtained should be fairly white, depending upon the grade of tallow used
and slightly alkaline to an alcoholic phenolphthalein solution. If removed at exactly the
neutral point or with a content of free fat the soap will sooner or later develop rancidity.
The soap thus obtained is an ordinary tallow base, and the one by far greatest used in the
manufacture of toilet soaps. The percentage of cocoanut oil indicated is not fixed and
may readily be varied, while in fine toilet soap the rosin is usually eliminated.
In the manufacture of full boiled soda soaps in which no glycerine is obtained as a by-
product, it being retained in the soap itself, the soap formed is known as a "run" soap.
The process is used most extensively in the manufacture of marine soaps by which the
method may be best illustrated. This soap is known as marine soap because of its
property of readily forming a lather with salt water and is mostly consumed aboard
vessels.
Marine soaps are manufactured by first placing in the kettle a calculated amount of lye of
25 deg. to 35 deg. B., depending upon the amount of moisture desired in the finished
soaps, plus a slight excess required to saponify a known weight of cocoanut oil. With
open steam on, the cocoanut oil is then gradually added, care being taken that the soap
does not froth over. Saponification takes place readily and when the oil is entirely
saponified the finished soap is put through the process known as running. This consists in [Pg 40]
constantly pumping the mass from the skimmer pipe back into the top of the kettle, the
object being to prevent any settling of the nigre or lye from the soap, as well as producing
a homogeneous mass. It is customary to begin the saponification in the morning, which
should be completed by noon. The soap is then run for about three hours and framed the
next morning. After having remained in the frame the time required to solidify and cool,
the soap is slabbed and cut into cakes. This process is difficult to carry out properly, and
one not greatly employed, although large quantities of marine soap are purchased by the
government for use in the navy and must fulfill certain specifications required by the
purchasing department.

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In making potash soaps it is practically impossible to obtain any glycerine directly

because of the pasty consistency of the soap, and no graining is possible because the
addition of salt to a soft soap, as already explained, would form a soda soap. Large
quantities of soft soaps are required for the textile industries who desire mostly a strong
potash soap, and the large number of automobiles in use at the present time has opened a
field for the use of a soft soap for washing these. A soap for this purpose must be neutral
so as not to affect the varnish or paint of automobiles.
A suitable soap for textile purposes may be made as follows:

Red oil 80 parts

House grease 20 parts
Caustic soda lye, 36 degs. B. 3 parts
Carbonate of potash 5-1/2 parts
Caustic potash 23-1/4 parts

Olive oil, corn oil, soya bean oil, olive oil foots or cottonseed oil may replace any of the [Pg 41]
above oils. A large quantity of cottonseed oil will cause the soap to fig.
To carry out the process, the caustic potash and carbonate of potash are dissolved and
placed in the kettle together with the soda lye, and the oils added. This is most
satisfactorily accomplished by being finished the day before the boiling is begun. The
next day the boiling is begun and water added to bring the soap up to the desired
percentage of fatty acid, due allowance being made for the water formed by the
condensation of the open steam in boiling. Care must be taken that the soap in the kettle
does not swell and run over during the saponification. A good procedure is to use open
steam for a period of about two hours, then close the valve and allow the saponification
to continue without boiling, and repeat this until it is entirely saponified. After the
saponification has been completed the soap is briskly boiled all day and the proper
corrections made; that is, if too alkaline, more oil is added, and if free fat is present, more
potash. About 2 per cent. carbonate of potash is the proper amount for a soap containing
50 per cent. fatty acid. The soap is sampled by allowing it to drop on a clean, cold glass
surface. In so doing, the soap should not slide or slip over the glass surface when pressed
thereon, but should adhere to the glass, or it is too alkaline. A sample worked between the
fingers showing too much stringiness should have more strong potash and oil added. A
sample taken out in a pail and allowed to cool over night will serve as a guide as to the
body of the soap in the kettle. When the soap has thus been properly finished it is run into
barrels.
For an automobile soap the following is a good working formula:

Corn oil 1,000 parts

Potash lye, 31-1/2 degs. B. 697 parts

Proceed as in the directions just given for textile soap in placing charge in the kettle. [Pg 42]
When the kettle is boiling up well, shut off the steam and the saponification will
complete itself. The soap may be run into the barrels the next day.
A heavy soap with a smaller percentage of fat may be made as follows:

Corn oil 1,000 parts

Potash lye, 24-1/2 degs. B. 900 parts

Boil until the soap bunches, and shovel the finished soap into barrels. Upon standing it
will clear up. By the addition of more water the yield of soap per pound of oil may be run
up to 300 per cent.

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After soft soaps have been allowed to stand for some time the phenomenon known as
"figging" often occurs. This term is applied to a crystalline-like formation, causing spots
of a star-like shape throughout the soap. This is undoubtedly due to the stearine content
of the soap crystallizing out as it cools, and forming these peculiarly-shaped spots. It
more generally occurs in the winter and may be produced artificially by adding a small
quantity of soda to the potash lye before saponification.
The oils usually employed in the manufacture of potash soaps are cottonseed oil, corn oil,
soya bean oil, olive oil foots, red oil, cocoanut oil, grease and the various train oils. The
usual percentage yield is from 225 per cent. to 300 per cent., based upon the weight of oil
used. In calculating the weight of a soft soap it is to be remembered that since potassium
has a higher molecular weight (56) than sodium (40), the corresponding soap formed is
that much greater in weight when compared with a sodium soap. Rosin may be added to
soft soaps as a cheapening agent. [Pg 43]

COLD PROCESS.
The cold process for manufacturing soap is the simplest method of soap making, and the
equipment required is small when compared to the other methods. All the more expensive
equipment that is necessary is a crutcher, a tank to hold the lye, frames, a slabber or
cutting table, and a press. Yet, in spite of the simplicity of thus making soap, the
disadvantages are numerous for the production of a good piece of soap. The greatest
difficulty is to obtain a thorough combination of oil or fat and lye so that there will not be
an excess of one or the other in the finished soap. At its best there is either a considerable
excess of free fat which later exhibits itself in producing rancidity or uncombined caustic,
which produces an unpleasant effect on the skin when the soap is consumed for washing.
The latter objection, of course, can only be applied to toilet soaps.
Cocoanut oil is used very largely in the manufacture of cold-made soaps as it is well
adapted for this purpose, although it is by no means true that other oils may not be
employed. Since by this process of manufacture no impurity contained in the fat or oil is
removed in the making of the soap, it is necessary that in order to obtain a fine finished
product, any impurity contained in these may be removed if present, or that the fats be as
pure as can be obtained. If inedible tallow is used for cold-made soap, it is advisable to
bleach it by the Fuller's Earth Process.
The carrying out of this method is best illustrated by an example of a cold-made cocoanut
oil soap.

Charge:
Cochin cocoanut oil 846 parts
Lye (soda), 35 degs. B. 470 parts
Water 24 parts

The oil is run into the crutcher and the temperature of the oil raised to 100 degs. F. by dry [Pg 44]
steam. The lye and water are at room temperature. After all the oil is in the crutcher, the
lye and water are slowly added to prevent any graining of the soap. Toward the end the
lye may be added more rapidly. When all the lye is in, the mass is crutched for about
three hours, or until upon stopping the crutcher a finger drawn over the surface of the
soap leaves an impression. If this condition is not realized, the soap must be mixed until
such is the case. Having arrived at this point, the mixture is dropped into a frame which
should remain uncovered. The heat produced by the further spontaneous saponification
will cause the soap to rise in the middle of the frame. After having set for some days it is
ready to be slabbed and cut into cakes.
A potash soap may be made by the cold process just as readily as a soda soap. Soaps of
this type may be made by either of these formulae in a crutcher:

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Olive oil foots 600

Potash lye, 18 degs. B. hot, 20 degs. B. cold 660

or

Corn oil 800

Rosin 200
Potash lye, 27 degs. B. 790
Water 340

Heat the oils to 190 degs. F., add the lye and crutch until the soap begins to bunch, when
it is ready to be run into barrels where the saponification will be completed.
Semi-boiled soaps differ from those made by the cold process in temperature. In making
semi-boiled soaps the fats are usually heated to 140° F. The addition of the lye raises the [Pg 45]
temperature to 180°—200° F. when saponification takes place.

CARBONATE SAPONIFICATION.
The method of the formation of soap by the utilization of the fatty acid directly, from
which the glycerine has already been removed by some method of saponification other
than with caustic soda, and neutralizing this with alkali, is becoming increasingly
popular. The glycerine is more easily recovered from a previous cleavage of the fats or
oils, but a soap made from the mixed fatty acids thus obtained is seldom white in color
and retains an unpleasant odor. Since soda ash or sodium carbonate is cheaper than
caustic soda and readily unites with a fatty acid, it is used as the alkali in the carbonate
saponification. The process is similar to that already given under Rosin Saponification.
About 19 per cent. by weight of the fatty acids employed of 58 per cent. soda ash is
dissolved in water until it has a density of 30 degs. B., and the solution is run into the
kettle, which is usually equipped with a removable agitator. The fatty acids, previously
melted, are then slowly added while the mixture is boiled with open steam and agitated
with the stirring device. The fatty acids instantly unite with the carbonate and rise in the
kettle, due to the generation of carbon dioxide, and care must be exercised to prevent
boiling over. After all the fatty acid has been added, and the mass is boiled through the
saponification must be completed with caustic soda, as there is as yet no practical method
known which will split a fat entirely into fatty acid and glycerine. Thus about 10 per cent.
of the fatty acids are true neutral fats and require caustic soda for their saponification.
This is then added and the soap completed, as in full-boiled soaps.
In carrying out this method upon a large scale, large [Pg 46]
sue\Neanderthal\doroteer\Neanderthal\Josephine\ quantities of carbon dioxide are formed
during the boiling of the soap, which replaces a quantity of the air contained therein. The
kettle room should therefore be well ventilated, allowing for a large inflow of fresh air
from out of doors.

CHAPTER IV [Pg 47]

Classification of Soaps.

In considering the many different varieties of soaps, their classification is purely an

arbitrary one. No definite plan can be outlined for any particular brand to be
manufactured nor can any very sharp distinction be drawn between the many soaps of
different properties which are designated by various names. It is really a question to what
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use a soap is to be put, and at what price it may be sold. There is, of course, a difference
in the appearance, form and color, and then there are soaps of special kinds, such as
floating soaps, transparent soaps, liquid soaps, etc., yet in the ultimate sense they are
closely allied, because they are all the same chemical compound, varying only in their
being a potash or soda soap, and in the fatty acids which enter into combination with
these alkalis. Thus we can take a combination of tallow and cocoanut oil and make a
great many presumably different soaps by combining these substances with caustic soda,
by different methods of manufacture and by incorporating various other ingredients, as
air, to form a floating soap, alcohol to make a transparent soap, dyestuffs to give a
different color, etc., but essentially it is the same definite compound.
The manufacturer can best judge the brand of soaps he desires to manufacture, and much
of his success depends upon the name, package, shape, color or perfume of a cake of
soap. It is the consumer whom he must please and many of the large selling brands upon
the market today owe their success to the above mentioned details. The great majority of
consumers of soap know very little concerning soap, except the fact that it washes or has [Pg 48]
a pleasant odor or looks pretty, and the manufacturer of soap must study these phases of
the subject even more carefully than the making of the soap itself.
For a matter of convenience we will classify soap under three general divisions:
I. Laundry soaps, including chip soaps, soap powders and scouring soaps.
II. Toilet soaps, including floating soap, castile soap, liquid soap, shaving soap, etc.
III. Textile soaps.

LAUNDRY SOAP.
The most popular household soap is laundry soap. A tremendous amount of this soap is
consumed each day in this country, and it is by far manufactured in larger quantities than
any other soap. It is also a soap which must be sold cheaper than any other soap that
enters the home.
The consumers of laundry soap have been educated to use a full boiled settled rosin soap
and to make a good article at a price this method should be carried out, as it is the one
most advisable to use. The composition of the fats entering into the soap depends upon
the market price of these, and it is not advisable to keep to one formula in the
manufacture of laundry soap, but rather to adjust the various fatty ingredients to obtain
the desired results with the cheapest material that can be purchased. It is impossible to
use a good grade of fats and make a profit upon laundry soap at the price at which it must
be retailed. The manufacturer of this grade of soap must look to the by-product,
glycerine, for his profit and he is fortunate indeed if he realizes the entire benefit of this
and still produces a superior piece of laundry soap. [Pg 49]

SEMI-BOILED LAUNDRY SOAPS.

It is advantageous at times to make a laundry soap by a method other than the full boiled
settled soap procedure as previously outlined. This is especially the condition in making a
naphtha soap, in which is incorporated naphtha, which is very volatile and some of the
well known manufacturers of this class of soap have adopted this process entirely. A
laundry soap containing rosin cannot be advantageously made by the cold process, as the
soap thus made grains during saponification and drops a portion of the lye and filling
materials. By making a semi-boiled soap this objection is overcome. The half boiled
process differs from the cold process by uniting the fats and alkalis at a higher
temperature.
To carry out this process the following formulae have been found by experience to give
satisfactory results.

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I. lbs.
Tallow 100
Rosin 60
Soda Lye, 36° B. 80
II.
Tallow 100
Rosin 60
Silicate of Soda 25
Soda Lye, 36° B. 85
III.
Tallow 100
Rosin 100
Lye, 36° B. 105
Silicate of Soda 25
Sal Soda Solution 20

In any of these formulas the sodium silicate (40° B.) may be increased to the same [Pg 50]
proportion as the fats used. By so doing, however, twenty pounds of 36° B. lye must be
added for every hundred pounds of silicate additional to that indicated or in other words,
for every pound of silicate added 20 per cent. by weight of 36° B. lye must be put into the
mixture. The rosin may also be replaced by a previously made rosin soap.
To make a semi-boiled soap, using any of the above formulae, first melt the rosin with all
or part of the fat, as rosin when melted alone readily decomposes. When the mixture is at
150° F. run it into the crutcher and add the lye. Turn on sufficient dry steam to keep the
temperature of the soap at about 150° F. in the winter or 130° F. in summer. After the
mass has been mixed for half an hour, by continuously crutching the soap it will at first
thicken, then grain and it may again become thick before it becomes smooth. When the
mass is perfectly smooth and homogeneous drop into a frame and crutch in the frame by
hand to prevent streaking. After standing the required length of time the soap is finished
into cakes as usual.

SETTLED ROSIN SOAP.

Settled rosin soaps are made from tallow, grease, cottonseed oil, bleached palm oils of the
lower grades, corn oil, soya bean oil, arachis oil, distilled garbage grease, cottonseed
foots or fatty acids together with an addition of rosin, varying from 24 per cent. to 60 per
cent. of the fatty acids which should titer from 28 to 35. A titer lower than 28 will prevent
the finished kettle of soap from being capable of later taking up the filling materials. As
has already been stated under hardened oils, these being very much higher in titer allow a
greater percentage of rosin to be added. Thus hardened fish oils and cottonseed oil are [Pg 51]
gradually being more extensively employed in soaps of this character.
The procedure of handling the kettle is similar to that given under full boiled soap. The
stock is steamed out into a settling tank and allowed to settle over night, after which it is
pumped into the soap kettle. Having stocked the kettle, open steam is turned on and
10°-12° B. lye is run in, while using a steam pressure of ninety to one hundred pounds in
order to prevent too great a quantity of condensation of the steam, the water thus being
formed weakening the lye. If a steam pressure of fifty to sixty pounds is available, a
stronger lye (20° B.) should be added. Care must be taken not to allow the lye to flow in
too rapidly or the soap will not grain. The saponification is only attained by prolonged
boiling with sufficient lye of proper strength. When saponification has taken place, the
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mass begins to clear and a sample taken out with a paddle and cooled should show a
slight pink with a 1 per cent. alcoholic phenolphthalein solution.
It may be stated here that in using this indicator or any other to test the alkalinity of soap,
the soap should always be cooled and firm, as whenever water is present, the dissociation
of the soap thereby will always react alkaline. When this state is reached the mass is
ready for graining, which is accomplished by distributing salt brine or pickle or spreading
dry salt over the surface of the soap. The kettle is then thoroughly boiled until the mass
shows a soft curd and the lye drops clearly from a sample taken out with a trowel or
paddle. The steam is then shut off and the soap allowed to settle over night. The lyes are
then run off to the spent lye tank for glycerine recovery. In saponifying a freshly stocked
kettle it is apt to bunch. To prevent this salt is added at various times to approximately
one per cent. of the fat used. [Pg 52]

If, by any possibility the soap has bunched, this condition may be remedied by the
addition of more strong lye and boiling until it is taken up. To work a kettle to its full
capacity it is advisable to make two "killing" changes. First add about 75 per cent. of the
fat and grain as directed. Run off the spent lyes and then add the remainder of the stock
and repeat the process. When the spent lye has been run to storage, the open steam is
again turned on and 18° B. lye gradually allowed to run in. The rosin is now broken up
and put into the kettle, or a previously made rosin soap is pumped in.
Lye is then added until the soap has a sharp taste after about three hours of continuous
boiling, or when the soap is in the closed state. More lye should then be run into the
kettle to grain the soap well, the grain not being too small. Then allow the soap to settle
over night and draw off the strengthening lye. The next day again boil up the kettle and
add water until the soap thins out and rises or swells high in the kettle. A sample taken
out at this stage upon a hot trowel should run off in large flakes. The surface of the soap
should be bright and shiny.
If the sample clings to the trowel, a slight addition of lye will remedy this defect. The
kettle is then allowed to rest, to drop the nigre and to cool for some time, depending upon
the size of the kettle. The proper temperature is such that after having been pumped to the
crutcher and the filling materials having been added, a thermometer placed into the mass
should indicate 128°-135° F. after the crutcher has run from ten to fifteen minutes. The
filling material may consist of from 7-9 per cent. of sal soda solution, 36°-37° B. warm or
just enough to close up the soap and make it rise high in the center of a screw crutcher
and make it cling close to a warm trowel. Other fillers such as outlined below are added
at this point. [Pg 53]

An addition of from 2-3 per cent. of a special mineral oil for this purpose will impart a
finish to the soap and 3-5 per cent. starch added prevents the soap from cracking in the
frames. Other filling material as silicate of soda, borax, talc or silex are used. After the
filling material has been thoroughly crutched through the soap it is framed, and, after
being several days in the frame to solidify and cool the soap is ready for slabbing,
pressing and wrapping.
In order to more definitely illustrate the composition of the mixture of fats and oils
entering into the formation of a laundry soap a typical formula may be given for such a
soap containing 40 per cent. rosin added to the amount of fats used:

lbs.
Grease 7,000
Tallow 4,000
Corn Oil 7,000
Cottonseed Oil 3,000
Rosin 8,400

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The following have been found to be satisfactory filling materials and are calculated
upon the basis of a 1,400-pound frame of soap.

I. lbs.
Sodium Silicate, 38°-40° B. 100
Mineral Oil 25
Sal Soda Solution, 36° B. 80
Borax 1
II.
Sal Soda Solution, 36° B. 80
Mineral Oil 25
Sodium Silicate 60
[Pg 54]
III.
Soda Ash 10
Sal Soda 55
Sodium Silicate 115
Mineral Oil 40
Brine (Saturated Solution) 10
Sodium Silicate, 38°-40° B. 100
IV.
Sodium Silicate 100
Silex or Talc 200
Soda Ash 50
V.
Sal Soda Solution, 36° B. 90
Sodium Silicate 50-60
Mineral Oil 25
Borax Solution, 25° B. (hot) 15

CHIP SOAP.
Chip soap is used extensively in laundries but is also used largely in other branches. It
may be made either as a settled soap or by the cold made process.
To make a full boiled settled chip soap, proceed as directed under settled laundry soap.
The kettle is stocked with light grease or a mixture of grease with corn oil or other cheap
oils. For this kind of soap the rosin is eliminated.
Chip soap may be filled as well as laundry soap. This is done in the crutcher and the
following adulterations are suitable.

lbs.
Settled Soap 700
Soda Ash 35
Sodium Silicate 215

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or
Settled Soap 700
[Pg 55]
Silicate of Soda 560
Soda Ash 18
Carbonate of Potash, 26° B. 50

The cheapest method of drying is by running this soap through a drying machine and this
is the procedure usually carried out for making dried chip soap.

COLD MADE CHIP SOAPS.

To make chip soaps by the cold process a sweet tallow of low percentage of free fatty
acid should be employed. The tallow is heated to 120° to 135° F. and the lye run in
slowly at first and then the silicate of soda is added. The mass is then mixed until a finger
drawn through the soap leaves a slight impression, then dropped into frames or barrels.
Soaps containing a small percentage of fat should be well covered in the frame for
twenty-four hours to retain their heat and insure proper saponification. The following
formulae are suitable:

I. lbs.
Tallow 1,200
Soda Lye, 35° B. 850
Sodium Silicate 750
II.
Tallow 475
Ceylon Cocoanut Oil 100
Soda Lye, 37° B. 325
Potash Lye, 37° B. 56
III.
Tallow 500
Soda Lye, 37-1/2° B. 297
Sodium Silicate 416
Potash Lye, 37-1/2° B. 37-1/2
[Pg 56]
IV.
Tallow 450
Soda Lye, 37-1/2° B. 255
Sodium Silicate 450
Potash Lye, 37-1/2° B. 50
V.
Tallow 450
Soda Lye, 35° B. 470
Sodium Silicate 650
VI.
Tallow 420
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Sodium Silicate 600

Soda Lye, 37-12° B. 270

UNFILLED CHIP SOAP.

A very good grade of chip soap is made by employing no filling material whatsoever, but
unfortunately the price of this soap has been cut to such an extent that these can not
compete with a filled chip. A number of the best soaps of this kind are made from a
settled soap using a light grease with corn oil. A soap of this nature is made as follows.

lbs.
Settled Soap 800
Sal Soda Solution, 36°-37° B. 252
Soda Ash 182

If this soap is run into frames it may be stripped and chipped in two days.

SOAP POWDERS.

Soap powders have become so great a convenience as a general cleansing agent that to
eliminate them from the household necessities would mean much unnecessary energy and [Pg 57]
work to the great number of consumers of this product. They may be manufactured so
cheaply and still be efficient, that their use has almost become universal for cleansing and
scouring purposes. The uses to which soap and scouring powders are adapted are too well
known to enter into a description of their employment. Since they offer a greater profit to
the manufacturer than ordinary household soap, many brands are extensively advertised.
Numerous combinations for soap powders might be cited and it is a simple matter to vary
the ingredients as to fat content and manufacture a powder of this sort as low as a cent a
pound. Many substances are incorporated with soap, such as salt, soda ash, tripoli,
crushed volcanic deposits, ground feldspar, infusorial earth of various kinds, silex, etc. In
addition to these various fillers, compounds with true cleansing and bleaching properties,
in addition to soap, are added, such as the salts of ammonium (sal ammoniac, carbonate
of ammonia), sodium perborate and the peroxides of various metals. The public,
however, have been accustomed to receive a large package of soap or scouring powder
for a small amount of money and it is a difficult matter for the manufacturer to add more
expensive substances of this nature to his product, to increase its efficiency, without
raising the price or decreasing the size of the package.
In manufacturing soap powders, the dried soap chips might be mixed with the filler and
alkali and then pulverized. This method is not extensively employed nevertheless. The
process which is the most economical is one whereby the ingredients are mixed in a
specially adapted mixer for heavy material until dry and then run directly to the crusher
and pulverizer, after which it is automatically packed, sealed and boxed. Another method [Pg 58]
of procedure is to run out the mixture from the crutcher to the frames, which are stripped
before the soap cools, and is cut up at once, for if it hardens it could not be cut with
wires. It is better, however, to run the mixture into sheets upon a specially constructed
floor and break up the mass when cool.
Formulae for soap powders which have been found to be suitable for running dry in the
mixer follow:

I
Soda ash, 58 per cent. 42 lbs.
Silica 220 "

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Settled soap (usually cottonseed). 25 "

Salt 10 "
II
Soap (settled cottonseed) 40 lbs.
Soda ash, 58 per cent. 60 "
III
Settled soap 100 lbs.
Soda ash, 58 per cent. 400 "

Fillers in varying proportions may replace the soda ash in the above formulae. It is of
course understood that the soap has been previously made and run as molten soap into
the crutcher.
The following soap powders will not dry up in the crutcher upon running, but are of the
class which may be framed or run on the floor to solidify:

I
Soap 850 lbs.
Filler 400 "
Sal soda solution, 20 degs. B 170 "
[Pg 59]
II
Soap 650 lbs.
Filler 550 "
Sal soda solution, 20 degs. B. 340 "
III
Soap 80 lbs.
Filler 550 "
Sal soda solution 170 "
IV
Soap (settled tallow) 800 lbs.
Filler 400 "
Sal soda solution 170 "
Water 100 "

V
First saponify 100 parts house grease and 100 parts ordinary grease and make a run soap.
Then use in crutcher either:

Soap 400 lbs.

Filler 575 "
Hot water 60 "
or
Soap 200 lbs.
Hot water 200 "

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Filler 625 "

It would be a simple matter to write numerous additional formulae, but the above are
typical. The manufacturer must judge for himself just what filling material to use. The
filler indicated in the above formulae is therefore left open. A few formulae for more
expensive powders than those given recently appeared among others in the "Seifensieder
Zeitung"[9]: [Pg 60]

I
Powdered soap 90 lbs.
Sodium perborate 10 "

The perborate should be added when the powder is perfectly dry or it loses its bleaching
properties.

II
Soap powder, 20 per cent. fat.
Cocoanut oil fatty acids 25 lbs.
Olein 25 "
Bone fat 70 "
Soda lye, 30 degs. B. 90 "
Water 150 "
Ammonium carbonate 125 "
III
Soap powder, 10 per cent. fat.
Cocoanut oil fatty acids 20 lbs.
Olein 10 "
Bone fat 20 "
Soda lye, 30 degs. B. 30 "
Water 175 "
Ammonium carbonate 175 "

LIGHT OR FLUFFY POWDERS.

Light or fluffy powders containing 35-45% moisture can be made in two ways. The first
method requiring a minimum equipment is to mix the powder and sal soda in a mixer,
allow it to stand in frames for a week to crystallize or spread it on the floor for a few
hours to dry and then grinding it.
The continuous method finishes the powder in a few minutes and with a minimum
amount of labor. By this process the various ingredients, soap, soda ash solution, etc., are
measured, run by gravity into the mixer, mixed and the molten mass run over the
crystallizer or chilling rolls thru which either cold water or brine is pumped. From the roll [Pg 61]
the powder is scraped off clean by a knife, passes to a screen which sends the tailings to a
grinder, falls into a storage bin from whence it is weighed and packed by an automatic
weighing machine into cartons made up in most cases by another machine. Due to the
large percentage of moisture contained in these soap powders the carton is generally
wrapped in wax paper to aid in the prevention of the escape of moisture.

Scouring Powders.
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Scouring powders are very similar to soap powders and differ only in the filler used. We
have already considered these fillers under scouring soap, from which they do not differ
materially. They are usually insoluble in water to aid in scouring. The mixer used for
substances of this kind in incorporating the soap and alkali must be of strong
construction.

SCOURING SOAP.
Scouring soaps resemble soap powders very closely in their composition, in that they are
a combination of soap and filling material. Since more lather is required from a scouring
soap than in soap powders, a cocoanut oil soap is generally used. The usual filling
material used is silex. The greatest difficulty in the manufacture of scouring soap is the
cracking of the finished cake. This is usually due to the incorporation of too great an
amount of filler, or too high a percentage of moisture.
In manufacturing these soaps the cocoanut oil is saponified in the crutcher with 38 degs.
B. lye, or previously saponified as a run soap, as already described under "Marine
Soaps." To twenty-five parts of soap are added a percentage of 38 degs. B. sal soda or [Pg 62]
soda ash solution, together with a small quantity of salt brine. To this mixture in the
crutcher seventy-five parts of silex are then added, and a sufficient amount of hot water
to make the mass flow readily. Care must be exercised to not add too great a quantity of
water or the mass will crack when it cools. The mass is then framed and cut before it sets,
or poured into molds and allowed to set. While silex is the most extensively used filler
for scouring soaps, it is feasible to incorporate other substances of like character,
although it is to be remembered that the consumer is accustomed to a white cake, such as
silex produces. Any other material used to replace silex should also be as fine as this
product.

FLOATING SOAP.

Floating soap occupies a position midway between laundry and toilet soap. Since it is not
highly perfumed and a large piece of soap may be purchased for small cost, as is the case
with laundry soap, it is readily adaptable to general household use. Floating soap differs
from ordinary soap in having air crutched into it which causes the soap to float in water.
This is often advantageous, especially as a bath soap, and undoubtedly the largest selling
brand of soap on the American market today is a floating soap.
In the manufacture of floating soap a high proportion of cocoanut oil is necessary. A most
suitable composition is one part cocoanut oil to one part of tallow. This is an expensive
stock for the highest grade of soap and is usually cheapened by the use of cottonseed or
various other liquid oils. Thus it is possible to obtain a floating soap from a kettle stocked
with 30 per cent. cocoanut oil, 15 per cent. cottonseed oil and 55 per cent. tallow. With
this quality of soap, however, there is a possibility of sweating and rancidity, and of the [Pg 63]
soap being too soft and being poor in color.
The process of manufacture is to boil the soap in an ordinary soap kettle, after which air
is worked into the hot soap by a specially constructed crutcher, after which the soap is
framed, slabbed, cut into cakes and pressed.
Concerning the boiling of the soap, the saponification must be carefully carried out, as
the high proportion of cocoanut oil may cause a violent reaction in the kettle causing it to
boil over.
The method of procedure is the same as for a settled soap up to the finishing. When the
mass is finally settled after the finish, the soap should be more on the "open" side, and the
object should be to get as long a piece of goods as possible.
Due to its high melting point, a much harder crust forms on the surface of a floating soap
and in a greater proportion than on a settled soap during the settling. In a large kettle, in
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fact, it has been found impossible to break through this crust by the ordinary procedure to
admit the skimmer pipe. Much of the success of the subsequent operations depends upon
the completeness of the settling, and in order to overcome the difficulties occasioned by
the formation of the crust everything possible should be done in the way of covering the
kettle completely to enable this period of settling to continue as long as possible.
When the soap is finished it is run into a specially constructed U-shape crutcher, a Strunz
crutcher is best adapted to this purpose, although a rapidly revolving upright screw
crutcher has been found to give satisfaction upon a smaller scale, and a sufficient quantity
of air beaten into the soap to make it light enough to float. Care must be taken not to run
the crutcher too rapidly or the soap will be entirely too fobby. During this operation the
mass of soap increases in bulk, and after it has been established how much air must be [Pg 64]
put into the soap to satisfy the requirements, this increase in bulk is a criterion to estimate
when this process is completed.
It is of course understood that the longer the crutching continues the greater quantity of
air is incorporated and the increase of volume must be established for a particular
composition by sampling, cooling the sample rapidly and seeing if it floats in water. If
the beating is continued too long an interval of time, the finished soap is too spongy and
useless.
The temperature of the mass during crutching is most important. This must never exceed
158 degrees F. At 159 degrees F. the operation is not very successful, yet the thermometer
may indicate 140 degrees F. without interfering with this operation. If, however, the
temperature drops too low, trouble is liable to be met with, by the soap solidifying too
quickly in the frames.
When the crutching is completed, the soap is allowed to drop into frames through the
valve at the bottom of the crutcher and rapidly crutched by the hand in the frames to
prevent large air spaces and then allowed to cool. It is an improvement to jolt the frames
as they are drawn away as this tends to make the larger air bubbles float to the surface
and thus reduce the quantity of waste. When the soap has cooled, the frame is stripped
and the soap slabbed as usual. At this point a layer of considerable depth of spongy soap
will be found to have formed. This of course must be cut away and returned to the kettle.
The last few slabs are also often rejected, inasmuch as the weight of the soap above them
has forced out so much of the air that the soap no longer floats. As a fair average it may
be estimated that not more than 50 to 60 per cent. of the soap in the kettle will come out
as finished cakes. the remaining 40 to 50 per cent. being constituted by the heavy crust in [Pg 65]
the kettle, the spongy tops, the bottom slabs and scrapings. This soap is of course
reboiled and consequently not lost, but the actual cakes obtained are produced at a cost of
practically double labor.
It is advisable to add a small quantity of soap blue color to the mass while crutching to
neutralize the yellowish tint a floating soap is liable to have.
Some manufacturers add a percentage of carbonate of soda, about 3 per cent., to prevent
the soap from shrinking. Floating soap may also be loaded with sodium silicate to the
extent of about 5 per cent.

TOILET SOAP.
It is not a simple matter to differentiate between toilet soaps and various other soaps,
because numerous soaps are adaptable to toilet purposes. While some soaps of this
variety are manufactured by the cold made or semi-boiled process, and not milled, the
consumer has become accustomed to a milled soap for general toilet use.
The toilet base most extensively employed is a tallow and cocoanut base made as a full
boiled settled soap. The manufacture of this base has already been outlined and really
needs no further comment except that it is to be remembered that a suitable toilet soap
should contain no great excess of free alkali which is injurious to the skin. Cochin
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cocoanut oil is preferable to the Ceylon cocoanut oil or palm kernel oil, to use in
conjunction with the tallow, which should be a good grade and color if a white piece of
goods is desired. The percentage of cocoanut oil may be anywhere from 10 to 25 per
cent., depending upon the kind of lather required, it being remembered that cocoanut oil
increases the lathering power of the soap.
In addition to a tallow base, numerous other oils are used in the manufacture of toilet [Pg 66]
soaps, especially palm oil, palm kernel oil, olive oil and olive oil foots, and to a much
less extent arachis or peanut oil, sesame oil and poppy seed oil, oils of the class of
cottonseed, corn and soya bean oils are not adapted to manufacturing a milled soap, as
they form yellow spots in a finished cake of soap which has been kept a short time.
Palm oil, especially the Lagos oil, is much used in making a palm base. As has already
been stated, the oil is bleached before saponification. A palm base has a yellowish color, a
sweetish odor, and a small quantity added to a tallow base naturally aids the perfume. It is
especially good for a violet soap. The peculiarity of a palm oil base is that this oil makes
a short soap. By the addition of some tallow or twenty to twenty-five per cent. of
cocoanut oil, or both, this objection is overcome. It is a good plan in using a straight palm
base to add a proportion of yellow color to hold the yellowish tint of this soap, as a soap
made from this oil continues bleaching upon exposure to air and light.
Olive oil and olive oil foots are used most extensively in the manufacture of castile soaps.
The peculiarity of an olive oil soap is that it makes a very slimy lather, and like palm oil
gives the soap a characteristic odor. An olive oil soap is usually considered to be a very
neutral soap and may readily be superfatted. Much olive oil soap is used in bars or slabs
as an unmilled soap and it is often made by the cold process. Peanut oil or sesame and
poppy seed oil often replaces olive oil, as they form a similar soap to olive oil.
In the manufacture of a toilet soap it is hardly practical to lay down a definite plan for the
various bases to be made. From the combination of tallow, palm oil, cocoanut oil, palm
kernel oil, olive oil and olive oil foots, a great many bases of different proportions might [Pg 67]
be given. The simplest method is to make a tallow base, a palm base and an olive oil
base. Then from these it is an easy matter to weigh out any proportion of these soap bases
and obtain the proper mixture in the mill. If, however, as is often the case, a large
quantity of soap base of certain proportions of these, four or even more of these fats and
oils is required, it is not only more economical to stock the kettle with the correct
proportion of these oils, but a more thorough mixture is thus obtained by saponifying
these in the kettle. In view of the fact that it is really a question for the manufacturer to
decide for himself what combination of oils he desires for a particular soap we will
simply outline a few typical toilet soap bases in their simplest combination. It is
understood that these soaps are suitable for milled soaps and are to be made as fully
boiled settled soaps. Palm kernel oil may be substituted for cocoanut oil in all cases.

TALLOW BASE.

Tallow 75-90 parts

Cocoanut oil 25-10 parts

PALM BASE.

Bleached Lagos palm oil 75-80 parts

Cocoanut oil 25-20 parts

or

Tallow 30 parts

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Palm oil 60 parts

Cocoanut oil 10 parts

OLIVE OIL BASE (WHITE).

Olive oil 75-90 parts

Cocoanut oil 25-10 parts

or [Pg 68]

Olive oil 40 parts

Tallow 40 parts
Cocoanut 20 parts

Where a green olive oil base is desired, olive oil foots are substituted for the olive oil.
Peanut oil may replace the olive oil or part of it, the same being true of sesame oil and
poppy seed oil.

PALM AND OLIVE BASE.

Palm oil 50 parts

Olive oil 30 parts
Cocoanut oil 20 parts

or

Palm oil 20 parts

Olive oil 10 parts
Tallow 50 parts
Cocoanut oil 20 parts

CHEAPER TOILET SOAPS.

It is often necessary to manufacture a cheaper grade of soap for toilet purposes to meet
the demand of a certain class of trade as well as for export. To accomplish this it is of
course necessary to produce a very inferior product and run down the percentage of fatty
acids contained in the soaps by the addition of fillers or to use cheaper oils in
manufacturing. The most simple method of filling a soap is to load it at the mill with
some substance much less expensive than the soap itself. Many of the cheaper toilet
soaps, however, are not milled and it is, therefore, necessary to follow out some other
procedure.
Milled soaps, as has just been stated, are loaded at the mill. The consumers of cheaper
toilet soaps in this country are accustomed to a milled soap and this grade of soap for
home consumption is very often filled with numerous substances, but most generally by [Pg 69]
adding starch and talc. The addition of such materials of course later exhibit themselves
by imparting to the cake of soap a dead appearance. Talc is more readily detected in the
soap than starch by washing with it, as talc is insoluble and imparts a roughness to the
soap, like sand or pumice, as the soap wears down. It may readily be added to 20 per
cent. by weight. Starch is to be preferred to talc, in loading a soap, as it is not so readily
noticeable in washing. It leaves the cake itself absolutely smooth although the lather
formed is more shiny. This substance may be employed to as high a percentage as one-

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third the weight of the soap. It is, of course, possible to cheapen the best soap base by this
method and the price may be further lowered by using the less expensive oils and fats to
make the soap base.

RUN AND GLUED UP SOAPS.

A very cheap grade of soap may be made by making a run soap and adding the filler e. g.
sodium silicate in the kettle during saponification. The percentage of fatty acids may be
brought down to 10 per cent., although of course a soap of this type shrinks a whole lot
upon exposure.
In making a "glued up" soap the procedure is the same for making the soap itself as with
a settled soap, except that the soap is finished "curd" and later filled in the crutcher. The
percentage of fatty acids in a soap of this type is seldom below 50 per cent.
The method of "gluing up" a soap is best illustrated by a typical soap of this character in
which the kettle is charged with the following stock.

Bleached palm oil 5 parts

Distilled grease 2 "
Cotton oil foots stock, 63% fatty acid 1 "
Rosin 4 "

The palm oil is first run into the kettle, saponified and washed to extract any glycerine, [Pg 70]
then the rest of the fats and finally the rosin. The soap is then finished and settled as with
a boiled settled soap. To assure success it is absolutely necessary that the soap settle as
long a period as possible, or until the temperature is about 150 degs. F. The ideal
temperature for carrying out the "gluing up" process is 140 degs. F., as at a lower
temperature than this the soap is liable to cool too quickly and not be thoroughly glued
up. A higher temperature than 150 degs. F. causes delay in that the soap does not properly
take the filler at a higher temperature and the soap must be kept in the crutcher until the
temperature drops to the right point.
The soap is run into the crutcher and the percentage of fatty acids run down to 50-55 per
cent. with one of the following mixtures:

Sodium silicate, 59-1/2° B. 1 part

Potassium carbonate, 51° B. 1 "

or

Sodium silicate, 59-1/2° B. 1 part

Potassium carbonate, 51° B. 1 "
Sodium sulfate, 28° B. 1 "

From 230 to 300 pounds of either of these mixtures are required for a crutcher holding
2,600 pounds of soap.
The crutching is continued until the mass is well "spiked," that is to say, a freshly broken
surface of the soap, as the crutcher blade is jerked away, stands up like shattered sheets in
triangular form (Δ Δ Δ), which retain their shape perfectly. When this condition is realized
the soap is run into frames which are carefully crutched by hand to remove any air
spaces. The surface of the soap is then smoothed down and heaped up in the center. After
standing a day to contract, the surface is again leveled and a snugly-fitting board placed [Pg 71]
on the top of the soap upon which a weight is placed or upon which the workman treads
and stamps until the surface is flat, thus assuring the further removal of air spaces. The

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soap remains in the frame from six to eight days and is then slabbed, barred and pressed
by the usual method employed for soaps thus handled without milling.
In a soap of this nature no hard and fast rule can be laid down as to the quantity of
solution to be used for "gluing up" or the strength of the solution. In a soap of the type
described the most satisfactory appearing cake will be obtained from a soap containing
58 per cent. fatty acids. That is to say, about 8 per cent. to 10 per cent. filling solution is
added per hundred pounds of soap. The filling solutions given are very satisfactory.
Carbonate of soda should be avoided in connection with sodium silicate as the property
of efflorescing on the surface of the finished cake after a short time will prove
detrimental. To assure successful gluing up it is advisable to experiment upon a small
scale to determine the exact extent to which the filling solution should be diluted. Various
proportions of water are added to a certain quantity of the filled soap. After the soap has
been filled in a small receptacle a sample is taken and rubbed between the fingers. If the
freshly exposed surface is smooth and glossy, the filling solution is weak enough, if
rough it is too strong. It is of course understood that the temperature must be correct, 140
degs. to 150 degs. F., or the soap will be rough. By this means the operator can readily
judge the correct strength of his filling solution. When properly carried out a perfectly
satisfactory soap is obtained.

CURD SOAP.
The object of a soap which is finished "curd" or grained, is to obtain a harder piece of
goods from low titer fat or to increase the percentage of fatty acids in the finished soap. [Pg 72]
This is still another method of producing a cheap grade of soap as by its adoption the
cheaper oils and fats may be used to obtain a firm piece of soap.
A typical charge for curd soap is:

Red oil 63 parts

Tallow 10 "
Rosin 27 "

Cotton seed foots may be employed in place of red oil and a tallow of too high titer is not
suitable for this kind of soap.
The red oil and tallow are first saponified with 15 degs. B. lye, boiler pressure 80-90
pounds, 18 degs. B. lye for lower steam pressure, and two washings given to extract the
glycerine. The rosin is added at the strengthening change and at the finish the soap is
"pitched," that is to say, the soap is settled over night only. The next day the lyes are
drawn off and a portion of the nigre pumped to another kettle which prevents later
streaking of the soap. The soap is then boiled with 18 degs. B. lye as with another
strengthening change under closed steam. Salt brine or "pickle," 15 degs. B. is then added
and the mass boiled with closed steam until the brine reaches a density of 18 degs. B. and
the kettle pumped the next day. A soap of this type requires either hand or power
crutching to assure homogeneity and prevention of streaks. To obviate any air spaces it is
advisable to place over the top of the frame a tightly-fitted board which is heavily
weighted down. This soap is also pressed without any milling.

COLD MADE TOILET SOAPS.

Comparatively little toilet soap is made by the cold or semi-boiled processes. While these
are the simplest methods of manufacturing soaps the drawbacks of using them are [Pg 73]
numerous and only in a few cases are they very extensively employed. To make a toilet
soap by the cold process a combination of good grade tallow and cocoanut oil is required.
It requires 50 per cent. by weight of 36 degs. B. lye to saponify a given weight of tallow
and 50 per cent. of 38 degs. B. lye for cocoanut oil. The lyes are used full strength or may

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be reduced slightly with water and the method of procedure is the same as already given
in the general directions for cold made soaps.
Cold made soaps are readily filled with sodium silicate which is added at the same time
the stock is put into the crutcher. In adding the silicate it is necessary to add additional lye
to that required for saponifying the fats, about 20 per cent. of 36 degs. B. lye is the proper
amount. There is of course a certain amount of shrinking due to the addition of this filler
and the finished cake is exceedingly hard, yet the author has seen a good looking cake of
cheap soap made from as high a proportion as 420 parts of tallow to 600 parts of silicate.
Cold made soaps are usually pressed without milling, although it is readily feasible to
mill a cold made soap provided it is not a filled soap such as has just been described.

PERFUMING AND COLORING TOILET SOAPS.

Equally important as the soap itself or even to a greater extent is the perfume of a toilet
soap. A prominent manufacturer recently made the statement, which is often the truth,
that it makes no difference to the public what kind of soap you give them, as long as you
put plenty of odor into it. The perfuming of soaps is an art in itself and a subject to be
treated by one versed in this particular branch. We can only take into account the
importance of the perfume as related to toilet soap not only, but the necessity of adding a [Pg 74]
certain proportion of the cheaper products of odoriferous nature to laundry soap to cover
and disguise the odor of even this type of soap.
The price of a cake of toilet soap to a great extent depends upon the perfume, and the
manufacturer should aim to give the best possible perfume for a certain price. He should
not allow his personal likes or dislikes to enter into the judgment of whether an odor is
good or not, but submit it to a number of persons to obtain the concensus of opinion. In
giving or selling a piece of soap to the consumer, it is second nature for him to smell it,
and in the great majority of cases his opinion is formed not from any quality the soap
itself may have during use, but from the odor. This only emphasizes the fact that the
perfume must be pleasing, not to one person, but to the majority, and many brands owe
their popularity to nothing more than the enticing perfume.
Perfuming of soap is closely allied to the soap making industry, but as stated a branch in
itself. It is, therefore, not our purpose to give numerous formulae of how to perfume a
soap, but rather to advise to go for information to some one who thoroughly understands
the characteristics of the numerous essential oils and synthetics and give positive
information for the particular odor desired. Under no circumstances is it advisable to
purchase a perfume already compounded, but since all perfumes are a blend of several or
many essential oils and synthetics, it is a more positive assurance of obtaining what is
desired, by purchasing the straight oils and blending or mixing them as one desires.
The perfume is added to a milled soap just before the milling process in the proper
proportion per hundred pounds of soap. In cold made or unmilled soaps it is added in the [Pg 75]
crutcher while the soap is still hot. By this method, of course, a proportion of the perfume
is lost due to its being more or less volatile.

COLORING SOAP.

While much toilet soap is white or natural in color, many soaps are also artificially
colored. The soap colors used for this purpose are mostly aniline dyestuffs. The price of
these dyestuffs is no criterion as to their quality, as the price is usually regulated by the
addition of some inert, water soluble substance like common salt or sugar.
The main properties that a dyestuff suitable for producing a colored soap should have are
fastness to light and to alkali. They should further be of such a type that the color does
not come off and stain a wash cloth or the hands when the soap is used and should be
soluble in water. Under no circumstances is it advisable to add these in such a quantity
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that the lather produced in the soap is colored. It is customary to first dissolve the dye in
hot water as a standardized solution. This can then be measured out in a graduate and
added to the soap the same time as the perfume is put in. About one part of color to fifty
parts of water is the proper proportion to obtain a perfect solution, though this is by no
means fixed. In making up a solution thus it is an improvement to add to the same about
one-half of one per cent. of an alkali either as the hydroxide or carbonate. Then, if there
is any possibility of change of color due to alkalinity of the soap, it will exhibit itself
before the color is added.
A particularly difficult shade to obtain is a purple, as there is up to the present time no
purplish aniline color known which is fast to light. Very good results in soap may be
obtained by mixing a fast blue, as ultramarine or cobalt blue, with a red as rhodamine or
eosine. [Pg 76]

Inasmuch as the colors for soap have been carefully tested by most of the dyestuff
manufacturers, and their information, usually reliable, is open to any one desiring to
know about a color for soap, it is better to depend upon their experience with colors after
having satisfied one's self that a color is what it is represented for a particular shade, than
to experiment with the numerous colors one's self.

MEDICINAL SOAPS.
Soap is often used for the conveyance of various medicants, antiseptics or other material
presumably beneficial for treatment of skin diseases. While soap is an ideal medium for
the carrying of such materials, it is an unfortunate condition that when incorporated with
the soap, all but a very few of the numerous substances thus employed lose their
medicinal properties and effectiveness for curing skin disorders, as well as any antiseptic
value the substance may have. Soap is of such a nature chemically that many of the
substances used for skin troubles are either entirely decomposed or altered to such an
extent so as to impair their therapeutic value. Thus many of the claims made for various
medicated soaps fall flat, and really have no more antiseptic or therapeutic merit than
ordinary soap which in itself has certain germicidal and cleaning value.
In medicating a soap the material used for this purpose is usually added at the mill. A
tallow and cocoanut oil base is best adapted for a soap of this type. The public have been
educated more or less to the use of colored soap to accentuate its medicinal value, and
green is undoubtedly the most popular shade. This inference, however, is by no means
true for all soaps of this character. Possibly the best method of arranging these soaps is [Pg 77]
briefly to outline some medicinal soaps.

SULPHUR SOAPS.

The best known sulphur soaps contain anywhere from one to 20 per cent. of flowers of
sulphur. Other soaps contain either organic or inorganic sulphur compounds.

TAR SOAP.
The tar used in the manufacturing of tar soap is obtained by the destructive distillation of
wood, the pine tar being the most extensively employed. While the different wood tars
contain numerous aromatic compounds, such as phenols, phenyl oxides, terpenes and
organic acids, these are present in such a slight proportion so as to render their
effectiveness practically useless. It has, therefore, been tried to use these various
compounds contained in the tar themselves to make tar soap really effective, yet tar is so
cheap a substance that it is usually the substance used for medicating a tar soap. About 10
per cent. of tar is usually added to the soap with 2 ounces of lamp black per hundred
pounds of soap.

SOAPS CONTAINING PHENOLS.

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Phenol (Carbolic Acid) is most extensively used in soaps of this kind, which are called
carbolic soaps. Carbolic soaps are generally colored green and contain from 1 to 5 per
cent. phenol crystals.
The cresols are also extensively used for making soaps named carbolic. These substances
impart more odor to the soap and really have more disinfecting powers than phenol when
incorporated with soap.
Other soaps, containing the phenol group, which are well known are resorcinol soap,
salol soap, thymol soap, naphthol soap, etc. From one to five per cent of the compound [Pg 78]
after which the soap is named is usually incorporated with the soap.

PEROXIDE SOAP.
Hydrogen peroxide in itself is an excellent disinfectant. It loses all its medicinal value,
however, when added to the soap. To overcome this objection various metallic peroxides
are added to the soap, as sodium peroxide, zinc peroxide and barium peroxide. These
generate hydrogen peroxide by the addition of water. Sodium perborate is also used in
peroxide soaps, as this substance is decomposed by water into hydrogen peroxide and
sodium metaborate.

MERCURY SOAPS.

Mercuric chloride (corrosive sublimate) is most extensively used for the production of
mercury soaps. Because of its extremely poisonous properties care should be taken in
using it. Since it really eventually loses any antiseptic value in the soap through forming
an insoluble mercury soap it might better be omitted entirely.

LESS IMPORTANT MEDICINAL SOAPS.

While the above mentioned soaps are probably the best known medicated soaps, there are
numerous other soaps which may be classed under these kinds of soaps. Thus we have
cold cream soap, which can be made by adding Russian Mineral Oil, 1 to 5 per cent., to
the soap; witch hazel soap, made by the addition of extract of witch hazel; iodine soap,
made by adding iodine or iodoform; formaldehyde soap, made by adding formaldehyde;
tannin soaps, made by adding tannin. In fact, there have been incorporated in soap so
great a number of substances that the list might be greatly enlarged. [Pg 79]

Medicated soaps are not only used in solid form, but in powder, paste and liquid soap as
well. The only difference in a soap like those just referred to is that the medicant is
incorporated with these forms of soaps as convenience directs.

CASTILE SOAP.

A pure castile soap should be made from olive oil. This, however, is not always the case,
as a number of oils as well as tallow are used to adulterate this oil to cheapen it, and there
are even some soaps called castile which contain no olive oil at all. Most of the pure
castile soap used in this country is imported, as it is a difficult matter for the American
manufacturer to compete with the pure imported castile soap, since both labor and oil
itself are so much cheaper in the vicinities of Europe where this oil is produced, that this
advantage is more than compensated by the carrying and custom charges by importing
the castile soap.
Castile soap may be made either by the full boiled or cold process. There are numerous
grades of olive oil, and those used for soap making are denatured to lower the duty
charges. Olive oil makes a hard white soap, usually sold in bars, and olive oil foots a
green soap, due to the coloring matter contained in this oil.

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To make a boiled castile soap, a composition of 10 per cent. Cochin cocoanut oil and 90
per cent. olive oil may be used. To cheapen this, peanut oil (Arachis oil) may entirely
replace the olive oil, or about 20 per cent. of corn or soya bean oil may be added. The oils
are saponified as usual in making a settled soap and to prevent rancidity the soap is
boiled near the finish for some time in the closed state with sufficient excess of alkali to [Pg 80]
give it a sharp taste, then grained with lye, the lye drawn off, closed with water and then
grained with salt. This process is repeated until the desired strength is reached. The last
graining should not be too great, and on the last change the soap should not be thinned
out, as it will contain too great a quantity of water when slabbed.
In making a cold castile soap the usual method is pursued as already directed under cold
made soap. When the soap is taken from the crutcher it is advisable, however, to keep the
soap in the frame well covered to assure complete saponification. Some manufacturers
use very small frames which are placed into compartments, well insulated to retain heat.
Several formulae for cold made castile soaps, follow. It may be noted that some of these
contain practically no olive oil.

I
Olive oil 2030
Palm kernel 674
Soda lye, 35 per cent. B. 1506
II
Olive oil 2030
Cochin cocoanut oil 674
Soda lye, 36 per cent. B. 1523
Sodium Silicate 82
III
Palm kernel oil 1578
Tallow 940
Olive oil 7
Sodium silicate, 20 per cent. 190
Soda lye, 36 per cent. B. 1507
[Pg 81]
IV
Olive oil (yellow) 1000
Soda lye, 37 per cent. B. 500
V
Olive oil 90
or
Palm kernel } 10
Cochin or cocoanut oil } 10
Lye, 37 per cent. B. 51

If any of the soaps containing a high proportion of cocoanut oil are boiled the soap will
float. It is therefore necessary to keep the temperature as low as possible.

ESCHWEGER SOAP (BLUE MOTTLED).

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Eschweger soap is a colored mottled or marbled soap made to a very slight extent in this
country. Inasmuch as it has been introduced to the export trade, it is made for this
purpose by some manufacturers. A high percentage of cocoanut oil is usually used
together with tallow and grease. About one-third of each is a typical formula. In a soap of
this character the fact that cocoanut oil soap takes up a large quantity of water and salts of
various kinds and is difficult to salt out is made use of. The tallow and grease are first
saponified as usual, then the cocoanut oil is pumped and saponified. When the
saponification is nearly completed either silicate or carbonate of soda or common salt are
added to make the soap "short" so as to form the mottle. The finishing of a soap of this
type can only be gained by practice and it is rather difficult to explain the exact
appearance of the kettle at this stage. The surface of the soap should be bright and
lustrous with the steam escaping in numerous places in rose-like formation. A sample on [Pg 82]
the trowel should have a slight sharpness to the tongue and be plastic. When the soap
slides from the trowel it should break short. When the soap has reached this stage the
desired coloring matter, usually ultramarine, is added to the soap either in the kettle or
crutcher and the soap framed. The yield is 200-215 pounds per hundred pounds of stock.
Several modifications of this general method for Eschweger soap are used by adopting
the half boiled or cold process.

Transparent Soap.

Transparent soap is really not a most desirable soap for toilet purposes, as it contains an
excess of free alkali. It has, nevertheless, met with public approval because of the fact it
is novel in being transparent. Except for this fact very little merit can be claimed for a
soap of this kind.
The transparency of soap is generally due to the presence of alcohol, sugar or glycerine in
the soap when it is made. It is very essential in a soap of this character, where lightness
and clearness of color are desired, that the material for making the soap be carefully
selected as to color and purity. The perfumes also play an important part in the color of
the soap and many of the tinctures, balsams and infusions used in perfuming soap may
eventually cause trouble by spotting. If the soap is artificially colored, which is almost
always the case, the dyestuffs used for this purpose should have careful attention and
only those should be used which are known to resist the action of alkalis. Where rosin is
used this product must be of the better grade. Distilled water is always preferable for use
in transparent soap. The government permits the use of a specially denatured alcohol.
This alcohol is not taxed and consists of grain (ethyl) alcohol denatured with 5 per cent.
wood (methyl) alcohol. Some soapmakers prefer to use a more expensive refined methyl [Pg 83]
alcohol, but outside of adding to the cost of the soap, there is no particular advantage.
The glycerine should be chemically pure. As to the oils and fats these should be low in
acid and of good color. Under no circumstances should the crutcher or kettle in which the
soap is made be rusty or unclean in any way. For a light soap enameled utensils are to be
preferred.
To obtain transparency in soap the following general methods may be given.
1. Where the transparency is due to sugar.
2. Where alcohol and glycerine produce transparency.
3. Where (1) or (2) is supplemented by the use of castor oil.
4. Where transparency depends upon the percentage of fatty acid in a soap and the
number of times the soap is milled.
Under the first method at least 25 per cent. of the charge should be cocoanut oil, the other
constituent being tallow or any fat or oil capable of giving a sufficiently hard soap. The
soap is boiled and finished as usual, then run to the crutcher to be mixed with a strong
cane sugar solution, containing 10-20 per cent. sugar of the weight of the soap. The sugar
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is dissolved in its own weight of water and the solution heated to 175 degs. F. before
being very slowly added to the soap. As the water evaporates, soaps of this type show
spots due to the sugar thus being thrown out of solution.
Transparent soap made under the second method may be saponified as usual and consist
of any good toilet base. The soap is run to the crutcher and mixed with 95 per cent.
alcohol in the proportion of one part alcohol to two parts of fatty acid contained in the
soap together with glycerine in the same proportion. [Pg 84]

By the third method castor oil alone may be used to make the soap or added to any of the
above bases up to 33-1/3 per cent. of the charge. If castor oil only is used, but 2 per cent.
or 3 per cent. of sugar is required.
In the last method a combination of 80 per cent. tallow, very low in free acid, 20 per cent.
cocoanut oil and 5 per cent. W. W. rosin is a suitable charge. The saponification and
finishing is carried out as with a full boiled soap. The soap is then placed into a jacketed
vessel, provided with dry-steam coils, by which the excess water is evaporated from the
soap until it contains 73 per cent. fatty acids. When the thick mass reaches this stage it is
framed and when cool is suitable for obtaining a semi transparency which now depends
upon the number of times the soap is milled, it being, of course, inferred that no solid
matter of any sort be added to the soap.

Cold Made Transparent Soap.

While transparent soaps may be made by the above general methods they are usually
made by the semi-boiled or cold process. By this process a more satisfactory soap is
obtained and it is more simple to carry out. A detailed description of this method is best
and most easily given by using a typical formula.

Charge:
Tallow 193-1/2 lbs.
Cochin Cocoanut Oil 169-1/2 "
Castor Oil 89-1/2 "
Soda Ash 7-3/4 "
Soda Lye, 36 degs. B. 256 "
Sugar (Cane) 198 "
Alcohol 126 "
Water (Distilled) 80 "

To proceed, first place into a crutcher or jacketed kettle the oils and fat and heat to 140 [Pg 85]
degs. F. Then add the soda ash dissolved in about 30 pounds of the water, after which the
lye is added and the mass stirred until a finger or stick run over the surface leaves an
imprint. Where the soap has reached this stage, it is well covered and allowed to stand
about two hours or until it bulges in the center, after which the rest of the water which
should contain no lime or other mineral substance and which is preferably distilled water,
is added. The sugar is then slowly shoveled in while the mass is stirring and finally the
alcohol is poured in. The heat is then increased to 160 degs. F. by dry steam and the soap
crutched until dissolved. Under no circumstances should any soap be allowed to remain
above the surface of the mass on the sides of the mixer. This crutching operation
consumes about one hour, and when finished the soap should stand in the vessel about
half an hour when a small sample is taken out to cool. This sample should be clear and
show an excess of alkali. If it is not clear more alcohol is added, if not of sufficient
strength more lye put in until the desired condition is reached. The perfume and color are
now added.

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The soap is then framed and allowed to set after which it is cut, allowed to dry slightly
and then pressed. To obtain a polished cake transparent soaps are often planed before
pressing and after pressing polished with a soft cloth, dampened with alcohol. Instead of
framing this soap, it is sometimes "tubed," that is to say, the soap from the crutcher is run
into specially constructed tubes of a shape near that of the desired cake and allowed to
cool, after which it is cut and pressed. All scraps are returned to the crutcher, but in so
doing the soap is slightly darkened in color. It is advisable to expose a finished cake of
transparent soap to the air for some time as by so doing it becomes clearer. [Pg 86]

Other formulae for cold made transparent soaps made as just outlined follow:

I.
Bleached Tallow 134 lbs.
Cochin Cocoanut Oil 88 "
Castor Oil 20 "
W. W. Rosin 7 "
Cane Sugar 64 "
Water 32 "
Glycerine 34 "
Soda Lye, 38 degs. B. 135 "
Alcohol 16 gal.
II.
Tallow 211 lbs.
Cochin Cocoanut Oil 185 "
Castor Oil 97-1/2 "
Soda Ash 8-1/2 "
Water 106 "
Soda Lye, 38 degs. B. 279 "
Sugar 216 "
Alcohol 137 "
III.
Castor Oil 60 lbs.
Cochin Cocoanut Oil 195 "
Tallow 120 "
Alcohol 115 "
Sugar 90 "
Water 53 "
Glycerine 53 "
Soda Lye, 38 degs. B. 205-1/2 "
[Pg 87]
IV.
Tallow 100 lbs.
Cochin Cocoanut Oil 100 "
Castor Oil 60 "

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Glycerine 20 "
Rosin, W. W. 20 "
Sugar 40 "
Water 50 "
Soda Lye, 36 degs. B. 164 "
Alcohol 8 gal.
V.
Tallow 174 lbs.
Cocoanut Oil 114 "
Soda Lye, 38 degs. B. 170 "
Sugar 80 "
Water 72 "
Alcohol 16 gal.

Rosin may be added in this formula up to 20 per cent. of fats used and the tallow cut
down correspondingly.

SHAVING SOAPS.
The requirements of a shaving soap are somewhat different than those of other soaps. To
be a good shaving soap the lather produced therefrom must be heavy, creamy, but not
gummy, and remain moist when formed on the face. The soap itself should be of a soft
consistency so as to readily adhere to the face when used in stick form. It should
furthermore be neutral or nearly so to prevent the alkali from smarting during shaving.
Shaving soap is made in the form of a stick, and a tablet for use in the shaving mug.
Some shavers prefer to have the soap as a powder or cream, which are claimed to be
more convenient methods of shaving. While a liquid shaving soap is not as well known
because it has not yet become popular, some soap for shaving is made in this form. [Pg 88]

Formerly shaving soap was extensively made from a charge of about 80 parts tallow and
20 parts cocoanut oil as a boiled settled soap, but either making the strengthening change
with potash lye or using potash lye in saponifying the stock and graining with salt. Soaps
for shaving made in this manner are very unsatisfactory, as they do not produce a
sufficiently thick or lasting lather and discolor very materially upon ageing. Potassium
stearate forms an ideal lather for shaving, but readily hardens and hence needs some of
the softer oils, or glycerine incorporated with it to form a satisfactory soap for shaving.
The selection of materials for making a shaving soap is important. The tallow used
should be white and of high titer. Cochin cocoanut oil is to be preferred to the other
kinds, and the alkalis should be the best for technical use that can be purchased—76 per
cent. caustic soda and 88-92 per cent. caustic potash are suitable. By the use of stearic
acid it is a simple matter to reach the neutral point which can be carefully approximated.
The following are shaving soap formulae which have been found to give good
satisfaction:

I. lbs.
Tallow 360
Stearic acid 40
Soda lye, 41° B. 147

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Potash lye, 34° B. 87

Water 32
Gum tragacanth 1
II. lbs.
Tallow 282
Cocoanut oil 60
[Pg 89]
Stearic acid 50
Bayberry wax 18
Soda lye, 41° B. 147
Potash lye, 34° B. 90
Water 32
III. lbs.
Tallow 400
Cocoanut oil 176
Stearic acid 415
Caustic soda, 40° B. 182
Caustic potash, 38° B. 108

To proceed, first run into the crutcher the tallow, cocoanut oil and bayberry wax when
used, and bring the temperature of the mass up to 140°-160° F. by dry steam. Then add
the caustic soda lye and keep on heat with occasional mixing until it is all taken up.
When this stage is reached gradually add all but about 5 per cent. of the potash lye, and
complete the saponification. This point having been reached, the heat is turned off; the
crutcher is run and the stearic acid, previously melted by dry steam in a lead-lined or
enameled vessel, is run in in a continuous stream and the crutching continued for fifteen
minutes to half an hour. Samples are taken at this time, cooled and tested by alcoholic
phenolphthalein solution. If too alkaline more stearic acid is added, if too acid more
potash lye from that previously reserved. After each addition of lye or stearic acid the
mass is crutched from 10 to 15 minutes longer, another sample is taken, cooled and again
tested. When the phenolphthalein shows a very light pink after several minutes, the soap
is practically neutral, although at this point one can better judge by dissolving a sample in
hot neutralized alcohol made by putting into the alcohol a few drops of phenolphthalein,
and then adding weak alkali drop by drop from a burette until a slight pink, not yellow, [Pg 90]
tint is obtained, and noting the color of the solution. The solution should show a very
light pink when the soap is properly neutralized. When this stage is arrived at the gum
tragacanth, previously softened in water, is crutched in if it is to be added. The soap is
then framed, stripped in three or four days, dried and milled.
The formulae as given are for shaving sticks, and do not readily press unless thoroughly
dried. A more satisfactory result is obtained by adding at the mill 25 per cent. of white
tallow base to obtain a satisfactory mug soap.

SHAVING POWDER.
Shaving powder differs from the soaps just described in being pulverized, usually adding
up to 5 per cent. starch to prevent caking. Any of the above soaps, dried bone dry, with or
without the addition of tallow base make a satisfactory powder for shaving.

SHAVING CREAM.

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Shaving cream is now a very popular shaving medium due to the rapidity and
convenience with which one can shave by the use of this product. Formerly shaving
cream was made from the liquid oils like olive oil and a soft fat like lard, together with
cocoanut oil. Now, however, most of the popular shaving creams are made from stearic
acid and cocoanut oil, as a far superior product is obtained by the use of these substances.
By using these a more satisfactory cream is obtained, and it is far more convenient to
make. The lather also produced therefrom is more suitable for shaving, being thick,
creamy and remaining moist.
A few typical formulae for shaving creams of this type are as follows: [Pg 91]

I. lbs.
Cochin cocoanut oil 26
Stearic acid 165
Caustic potash lye, 50° B. 69
Glycerine C. P. 76
Water 38
II. lbs.
Cochin cocoanut oil 18
Stearic acid 73
Caustic potash lye, 39° B. 54
Glycerine 33
Water 27
III. lbs.
Cochin cocoanut oil 18
Stearic acid 73
Caustic potash lye, 39° B. 54
Glycerine 20
Water 40
and lbs.
Stearic acid 60
Glycerine C. P. 85
Water 165
Sodium carbonate 50
Borax 1

To make a shaving cream by Formula I or II, the cocoanut oil and glycerine are first put
into a suitable mixing apparatus or crutcher, and heated to 120° F. A part or all the potash
lye is then added and the cocoanut oil saponified. The rest of the potash lye and the water [Pg 92]
are then added, and with the mixer running the stearic acid, previously melted in a lead-
lined or enameled vessel, is then poured in in a stream and the mass stirred until smooth,
care being exercised not to aerate it too much. The cream is then tested for alkalinity, the
best method being by that described under shaving soap, in which the sample is dissolved
in alcohol. Because of the large quantity of water present, phenolphthalein is
unsatisfactory, as dissociation of the soap may show a pink indication in spite of the fact
the mass is on the acid side. For a quick method of testing the bite on the tongue is a
satisfactory criterion. If a cooled sample bites the tongue more stearic acid is added until
there is a 3% excess of this. When the proper neutralization has taken place the cream is
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perfumed and framed in a special frame, or it may be allowed to cool in the mixer and
perfumed the next day. When cool the cream is strained, or put through an ointment mill,
after which it is ready to fill into tubes.
The procedure for the first part of Formula III is the same as that just given. The second
part of the formula is made the same as a vanishing cream for toilet purposes. To make
this, first melt the stearic acid as already directed. Dissolve the sodium carbonate and
borax in water and when dissolved add the glycerine and stir. Then heat this solution to
about 100°-120° F. and while stirring in a suitable mixing machine into which this
solution has been poured after being heated, or better still in which it has been heated by
dry steam, add the stearic acid. Continue mixing until smooth and then allow to cool, or
run into frames to cool.
When the shaving cream and vanishing cream are both cool, they are mixed in the
proportion of one of the former to two of the latter. It is claimed that in thus making a [Pg 93]
shaving cream a smoother product is obtained, although it may be said that the vanishing
cream is merely a soft soap and the ultimate result is the same as though the various
ingredients were added in one operation, rather than making two separate products and
then mixing them, thereby considerably increasing the cost of manufacture.

PUMICE OR SAND SOAPS.

Pumice and sand are at times added to soap to aid in the removal of dirt in cleansing the
hands. In some cases these soaps are made in the form of a cake, in others they are sold
in cans in the form of a paste.
A hand paste is usually made by merely dissolving ordinary tallow base in two or three
times its weight of hot water and mixing in the desired quantity of pumice or sand and in
some instances adding a little glycerine to keep it soft or a solvent of some kind for
grease. It may also be made by directly incorporating any of these in a potash soap.
A cold made or semi-boiled cocoanut or palm kernel oil soap is the base used to add the
pumice or sand to in making a cake soap of this sort. The following formulae serve as a
guide for these soaps.

I.
Palm Kernel or Ceylon Cocoanut Oil 705 lbs.
Pumice (Powdered) 281 "
Soda Lye, 38° B. 378 "
II.
Cocoanut Oil 100 "
Soda Lye, 38° B. 55 "
Water 6 "
Silver Sand (fine) 60 "

To proceed place the oil in a crutcher and heat to 140° F. Sift in the pumice and mix [Pg 94]
thoroughly. The lye is then added which causes a curdling of the grain. The stirring is
continued until the grain closes and the soap is smooth, after which the desired perfume
is added and the soap dropped into a frame and crutched by hand. When the soap is set, it
is slabbed, cut into cakes, dried slightly and pressed.

LIQUID SOAPS.

Liquid soaps are merely solutions of a potash soap, usually cocoanut oil soap, although
corn oil is used to make a cheap soap. One of the difficulties encountered in liquid soap is
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to keep it clear. At a low temperature a sediment is often formed, but this can be
overcome by the use of sugar and filtering the soap through a filter press at a low
temperature. In order to prevent the soap from freezing, it is necessary to lower the
freezing point by the addition of glycerine or alcohol.
To make liquid soap by any of the formulae given below, the oil is first run into a
jacketed kettle with a stirring device, and heated to about 120° F. The potash lye is then
added and the oil saponified. When the saponification takes place, especially when
cocoanut oil is used, the mass swells rapidly and may foam over the sides of the kettle
unless water is used to check this, or a kettle of about four to five times the capacity of
the total charge of soap is used. When the saponification has occurred, the sugar, borax
and glycerine are added, the water run in and the mixture stirred until the soap is
thoroughly dissolved. Heat aids materially in dissolving the soap. The soap is then
allowed to cool and if color or perfume is to be added this is stirred in, after which the
soap is cooled and filtered or else run directly into barrels. [Pg 95]

Tallow is not suitable for making a clear liquid soap since it is too high in stearine which
when formed into the stearate makes an opaque solution. The formulae herewith given
have been found to give good practical results.

I. lbs.
Cocoanut oil 130
Caustic potash lye, 28° B. 135
Sugar 72
Borax 2
Water 267
II. lbs.
Corn oil 130
Caustic potash lye, 26° B. 135
Sugar 72
Borax 2
Water 267
III. lbs.
Cocoanut oil 100
Caustic potash lye, 28° B. 102
Glycerine 100
Sugar 70
Water 833

Formulae I and II contain about 20 per cent. fatty acids. It is possible, of course, to either
increase or decrease the percentage of fatty acid by varying the amount of water. The
water used in making liquid soaps, of course, should be soft, for hard water forms
insoluble soaps which precipitate and cause a sediment. [Pg 96]

USE OF HARDENED OILS IN TOILET SOAPS.

While the introduction of the hydrogenation of oils is a decided advance in the
production of suitable cheaper oils for soap making, comparatively little hardened oil is
employed for soap making in America up to the present time. In Europe, however,
considerable advance has been made by the use of such oils for manufacturing soap
therefrom and a number of plants turn out large quantities of hydrogenated oils for soap
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making as well as for edible purposes. Recently a company has been formed in this
country for hardening oils and it is very probable that the future will see this material
extensively used in our own country, as these appear to be the one present hope of the
soap manufacturer as a check on the ever increasing cost of fats and oils now used in
making soap.
It is an unfortunate condition that hydrogenated oils produced abroad are sold under
names which give absolutely no indication as to the oil which has been hardened. The
softer and cheaper oils like fish oil, linseed oil, cottonseed oil, etc., are generally
hardened for soap manufacture to different degrees of hardness. While it is impossible to
definitely state just what products as Candelite, Talgol, Krutolin or several other coined
names of hardened oils are, various investigators have experimented with them as to their
adaptability for producing toilet soaps and found that suitable toilet soaps may be made
from them. While many objections were at first met with concerning soaps made from
these products, as to their unsatisfactory saponification, the poor lathering quality of the
soaps and their odor and consequent difficulty in perfuming, the results of most
investigators along these lines indicate that these in many cases were due to prejudice
against or unfamiliarity with handling oils of this type for soap making.
In manufacturing soap from hardened oils it is usually necessary to incorporate with the [Pg 97]
charge lard, tallow, tallow oil or some other soft oil of this nature. Satisfactory bases for
toilet soaps, made as boiled settled soap by the use of Talgol (undoubtedly hardened fish
oil), are said to be made by the formulae[10] below.

I.
Tallow 45 parts
Talgol 40 "
Cocoanut Oil 15 "
II.
Cocoanut Oil (Ceylon) 6 "
Tallow 12 "
Talgol, Extra 12 "

The method of boiling a soap of this type does not differ materially from that of making
settled tallow soap base. The soap itself has a different odor than a straight tallow base,
but is said to make a very satisfactory soap for milling and to be of good appearance.
Satisfactory transparent soaps are made from the hardened oil Candelite, which replaces
the tallow in transparent soap formulae such as have already been given in the section
under "Transparent Soaps." The method of manufacturing a soap by the use of this
product varies in no way from the usual method employed for making these soaps.
Since hydrogenated oils are high in stearine, their use in shaving soaps is a decided
advantage. It has previously been pointed out that potassium stearate forms an ideal
lather for shaving, and in the hydrogenating process the olein is converted to stearine.
Thus a hardened oil is advantageous in a shaving soap. As an example of a cold made [Pg 98]
soap for shaving the following may be taken.[11]

Talgol Extra 50 lbs.

Cocoanut Oil 10 "
Lard 10 "
Soda Lye, 38° B. 20 "
Potash Lye, 37° B. 21 "

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This soap may be made in a crutcher by the method generally used in making soap by the
cold process.

TEXTILE SOAPS.
Soap is a very important product to every branch of the textile industry. For woolen
fabrics it is used for scouring, fulling and throwing the wool; in the silk industry it is
necessary for degumming the raw silk, as well as for dyeing; in the cotton mills it is used
to finish cotton cloth and to some extent in bleaching; it is, furthermore, employed in a
number of ways in the manufacture of linen. Large quantities of soap are thus consumed
in an industry of so great an extent and the requirements necessitate different soaps for
the different operations. We will, therefore, consider these in detail.

SCOURING AND FULLING SOAPS FOR WOOL.

The soaps used to scour wool and for fulling the woven cloth are usually made as cheaply
as possible. They are, however, generally pure soaps, as filling material such as sodium
silicate does not readily rinse out of the wool and if used at all must be added very
sparingly. Both cold made and boiled settled soaps are made for this purpose. The soap is
generally sold in barrels, hence is run directly to these from the crutcher or soap kettle.
As cold made soaps the following serve for wool scouring or fulling. [Pg 99]

I.
Palm Oil 200 lbs.
Bone Grease 460 "
Soda Lye, 36° B. 357 "
Water 113 "
Soda Ash 50 "
Citronella 2"
II.
Palm Oil (Calabar, unbleached) 155 "
House Grease 360 "
Soda Lye, 36° B. 324 "
Water 268 "
Sodium Silicate 83 "
III.
House Grease 185 "
Palm Oil (unbleached) 309 "
Soda Lye, 36° B. 309 "
Water 391 "
Soda Ash 70 "
Sodium Silicate 60 "
Corn Starch 10 "

These soaps are made in a crutcher by the usual process for cold-made soaps, crutched
until smooth, dropped into a barrel and crutched by hand the next day or just before
cooling.
As a settled soap for these operations the following charge is typical:
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Palm Oil 34 parts

Cottonseed foots or its equivalent in fatty acids 33 "
Rosin 10 "
House Grease 23 "

The method of boiling such a soap is the same as for any settled soap up to the [Pg 100]
strengthening change. When this stage is reached, sufficient lye is added to strengthen the
kettle strongly. It is then boiled down with closed steam on salt brine or "pickle" until a
sample of the lye taken from the bottom stands at 16°-22° B. The soap is then run into
barrels and after standing therein for a day is hand crutched until cool to prevent
streaking of the soap.
Besides a soap of this type a settled tallow chip soap is used.

WOOL THROWER'S SOAP.

Soaps for wool throwing are sometimes made from olive oil foots but these are often
objected to because of the sulphur-like odor conveyed to the cloth due to the method by
which this oil is extracted with carbon disulphide. A potash soap hardened somewhat
with soda is also used. As a formula for a suitable soap of this type this may be given.

Olive Oil Foots 12 parts

Corn Oil 46 "
House Grease 20 "
Soda Lye, 36° B. 3"
Potassium Carbonate (dry) 5-3/4 "
Potassium Hydrate (solid) 23 "

This soap is made as a "run" soap by the general directions already given for a soap thus
made. The kettle is boiled with open and closed steam, adding water very slowly and
aiming to obtain a 220-225 per cent. yield or fatty acid content of the finished soap of 46
per cent. When the soap is finished a sample cooled on a plate of glass should be neither
slippery or short, but should string slightly. The finished soap is run directly into barrels. [Pg 101]
A soap for wool throwing by the semi-boiled process may be made from olive oil foots in
a crutcher thus:

Olive Oil Foots 600 lbs.

Potash Lye, 20° B. 660 "

The oil is heated to 180° F., the lye added and the mass stirred until it bunches, when it is
dropped into barrels.

WORSTED FINISHING SOAPS.

For the finishing of worsted cloth soaps high in cocoanut oil or palm kernel oil are
preferred. These soaps are finished very neutral, being made as settled soaps, but given
an extra wash change after strengthening strongly. They are then finished as usual and
run into barrels. If framed too hot, the high percentage of cocoanut oil causes mottling,
which is prevented by crutching by hand until the temperature of the soap is 140°-145° F.
Some typical charges, all of which are saponified with soda lye, follow:

I.
Palm Kernel Oil 60 parts
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Corn Oil 40 "

II.
Palm Kernel Oil 30 "
Red Oil (single pressed) 70 "
III.
Red Oil 33-1/3 "
Corn Oil 33-1/3 "
Cocoanut Oil or Palm Kernel Oil 33-1/3 "

SOAPS USED IN THE SILK INDUSTRY.

Soap is used to a very large extent in silk mills, both for degumming the raw silk and in [Pg 102]
silk dyeing. Raw silk consists of the true silk fibre known as fibroin and a gummy
coating, sericin, which dulls the lustre of the silk unless removed. For this purpose a
slightly alkaline olive oil foots soap is best adapted, although palm oil and peanut oil
soaps are sometimes used, as well as soaps made from a combination of house grease to
the extent of 30 per cent., together with red oil or straight olein soaps, both of which are
artificially colored green. In using house grease, if 30 per cent. is exceeded in
combination with red oil, the titer is raised to such an extent that the soap does not readily
rinse from the silk nor dissolve readily. They are also not advisable because they impart a
disagreeable odor to the silk.
To make a soap for this purpose from olive oil foots it is made as a settled soap, care
being taken to thoroughly boil the mass on the saponification change in the closed state
to assure proper saponification. The kettle is usually grained with lye and given a good
wash change to remove the excess strength. The change previous to the finish should not
be too heavy or too large a nigre results. The lighter the grain is, the better the finished
kettle is. A yield of 150 per cent. is usually obtained. This soap is generally run to a
frame, slabbed upon cooling and packed directly into wooden cases.
For silk dyeing the above soap is suitable, although any well-made soap of good odor and
not rancid is useable. While soap alone is often used in the bath for silk dyeing, certain
dyestuffs require the addition of acetic or sulphuric acid, which sets free the fatty acids. If
these be of bad odor it is taken up by the silk and is difficult to remove. The most
generally used soaps are the just mentioned olive foots soap or a soap made from a good
grade red oil.
Both kinds are extensively used. [Pg 103]

SOAPS USED FOR COTTON GOODS.

In the manufacture of cotton goods, as compared to the wool and silk industries, very
much less soap is used and it is only applied to the finished fabric either to clean the cloth
preparatory to dyeing or to aid in dyeing with certain colors. It is also used in calico
printing. For cleansing the cloth ordinary chip soap is suitable although a more alkaline
soap finished as a curd soap is an advantage in that the free alkali contained therein aids
in removing the dirt and has no harmful effect on the cotton. For dyeing cotton goods or
to brighten certain colors after dyeing an olive oil foots soap is most generally employed.
In calico printing soap is used to wash and clear the cloth after printing. A soap for this
purpose should be easily soluble in water and contain no free alkali, rosin or filler. The
best soaps for use in calico printing are either an olive oil foots soap or an olein soap.

SULPHONATED OILS.

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While sulphonated oils are not used to any great extent in the manufacture of soap, they
are used very largely in the dyeing and printing of turkey and alizarine reds on cotton as
well as other colors. Just what action these oils have is not known. Turkey red oil or
sulphonated castor oil is the best known sulphonated oil.
The process of making these oils is simple. The equipment necessary is a wooden tank or
barrel of suitable capacity, approximately two and a half times the amount of oil to be
treated. There are furthermore required other tanks or vessels to hold the solutions used
such as caustic soda, ammonia and acid. The tank to be used for the preparation of
sulphonated oil should be provided with a valve at the bottom of the tank and a gauge to
measure the quantity of liquid therein. [Pg 104]

The process is carried out as follows:

Three hundred pounds of castor oil are placed in the tank and 80 pounds at 66 deg. B.
sulphuric acid are weighed out in another vessel. The acid is run into the tank containing
the oil in a very thin stream while the oil is well stirred. At no time should the
temperature exceed 40 deg. C. This operation should consume at least an hour and
stirring should be continued half an hour longer to insure the thorough mixing of the oil
with the acid. The mass is then allowed to settle for 24 hours, after which 40 gallons of
water are added and the mixture stirred until it has a uniform creamy color indicating no
dark streaks. This mixing process should be carefully carried out and when completed
allowed to settle 36 hours. At this point the mass will have separated into two layers, the
lower layer consisting of a water solution of acid and the upper layer of oil. The former is
run out through the valve located at the bottom of the tank. Another wash may now be
given or dispensed with as desired. In this wash the addition of salt or sodium sulphate at
the rate of 1-1/2 pounds per gallon of water is advisable. A 24 deg. B. caustic soda
solution is prepared and added slowly to the acidified oil with constant stirring. The mass
first turns creamy, then becomes streaked, increasing in streaks as the caustic solution is
poured in, and finally becomes clear and transparent. Water is now added to bring the
volume to 75 gallons. The oil is now milky in appearance, but the addition of a little more
soda solution restores the transparency.
In some cases ammonia is used in addition to caustic soda in neutralizing the oil. Three-
fourths of the amount of caustic soda required to complete the neutralization is first
added and then the neutralization is completed with a one to one liquid ammonia and
water solution.

FOOTNOTES:
[9] Seifensieder Ztg., 40, 47, 1266 (1913).
[10] Seifensieder Ztg. (1913), p. 334 and 338.
" " (1912), p. 1229 and 1257.
[11] Seifensieder Ztg. (1912), p. 954.

CHAPTER V [Pg 105]

Glycerine Recovery.
The recovery of glycerine is very closely allied with the soap-making industry, because
glycerine is the very valuable by-product obtained in the saponification of oils and fats.
No soap plant is, therefore, fully equipped unless it has some method whereby the

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glycerine is recovered and the importance of recovering this product cannot be too
strongly emphasized.
It has already been pointed out that neutral fats or the glycerides are a combination of
fatty acid with glycerine. These are split apart in the process of saponification. While by
the term saponification as used in soap making it is inferred that this is the combination
of caustic alkalis with the fatty acids to form soap, this term is by no means limited to
this method of saponification, as there are various other methods of saponifying a fat.
The chemical definition of saponification is the conversion of an ester, of which
glycerides are merely a certain type, into an alcohol and an acid or a salt of this acid.
Thus, if we use caustic alkali as our saponifying agent for a fat or oil, we obtain the
sodium or potassium salt of the higher fatty acids or soap and the alcohol, glycerine. On
the other hand, if we use a mineral acid as the saponifying agent, we obtain the fatty
acids themselves in addition to glycerine. While the former is by far the most generally
employed for making soap, other processes consist in saponifying the fats by some
method other than caustic alkalis and then converting the fatty acids into soap by either
neutralizing them with sodium or potassium carbonate or hydrate.
It is important to again point out here that fats and oils develop free fatty acid of [Pg 106]
themselves and that the development of this acid represents a loss in glycerine. The
selection of an oil or fat for soap making should therefore to a large extent be judged as
to its adaptability by the free fatty acid content, as the higher this content is, the greater is
the loss in the glycerine eventually obtained. Glycerine often represents the only profit to
a soap manufacturer. It is indeed necessary to determine the percentage of free fatty acid
before purchasing a lot of stock to be made into soap.
In taking up the question of glycerine recovery we will consider the various methods
thus:
1. Where the glycerine is obtained from spent lye by saponifying the fats or oils with
caustic alkali.
2. Where the glycerine is obtained by saponifying the fats or oils by some other method
than the above, of which there are the following:
(a) Twitchell process.
(b) Saponification by lime in autoclave.
(c) Saponification by acid.
(d) Saponification by water in autoclave.
(e) Fermentative (Enzymes).
(f) Krebitz process.

RECOVERY OF GLYCERINE FROM SPENT LYE.

The spent lye obtained from the glycerine changes in making soap varies greatly, the
quality depending upon the stock saponified and the soap maker's care in handling the
operation. No two lyes run exactly alike as to proportion of the various ingredients,
although they are all similar in containing the same substances either in solution or
suspension. Spent lye is a water solution of mainly glycerine, free alkali either as caustic
alkali or carbonate and salt, including sodium sulfate, but furthermore contains some
soap and albuminous matter either in solution or suspension. Upon standing in the [Pg 107]
storage tank the greater part of the soap usually separates when the lye cools. In order to
assure the greatest economical yield of glycerine by saponifying a fat with caustic soda it
is necessary to obtain a proportion of three parts of water to every part of fat made into
soap. Test runs have shown that this is the proper proportion and that it is not economical
to greatly exceed this amount, and if a much less proportion is used the full yield of
glycerine is not obtained.
The spent lyes contain varying amounts of glycerine, the first change being richest in
glycerine content, and this being reduced in the subsequent changes. If the lyes always
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run high in glycerine it is an indication that it is not all being obtained. The usual
percentage is from 0.5% to 5% or even more, although the average is somewhere around
2% to 3%. The lye as it comes from the kettle should not contain any more than 0.5% to
0.6% of free alkali calculated as sodium carbonate, Na2CO3. If the proportion is higher
than this, it shows that the saponification has been conducted with too high a proportion
of alkali, a condition which should be corrected in the kettle room. An excess of free
alkali does not interfere to any great extent with the successful recovery of the glycerine,
but is a waste of both alkali and the acid used in neutralizing this. It is, therefore, more
economical to run a strong lye over fresh stock and neutralize the alkali thus, rather than
treating the lye for glycerine recovery.
Before the spent lye can be run into the evaporator it is necessary to remove the
albuminous impurities and soap and to neutralize the excess alkali to between exactly
neutral and 0.02% alkalinity. The lye should never be fed into the evaporator in the acid
condition.
In order to treat the spent lyes for evaporation, they are first allowed to cool in the storage
tank, after which any soap which may have separated is skimmed off and returned to the [Pg 108]
soap kettle. This lye is then pumped to the treatment tank, an ordinary tank equipped with
some method of agitating the liquor, either by a mechanical stirrer, steam blower or
compressed air, until it is about two feet from the top.
After the lye has been skimmed off it is thoroughly agitated and a sample taken. The
amount of lye in the tank is then calculated. Spent lye is about 1.09 times heavier than
water, or weighs about 9 pounds to the gallon. While the sample is being tested for
alkalinity it is advisable to add sulfate of alumina, which may be dissolving while the
sample is being titrated. This substance should be added in the proportion of anywhere
from 6 to 14 pounds per thousand pounds of lye, depending upon the amount of
impurities contained therein. For a clean lye six pounds per thousand is sufficient, but for
an impure lye a greater quantity is necessary. The sulfate of alumina used should be free
from arsenic and sulfides and should contain a minimum amount of grit (silica), as grit
reduces the life of the pump valves. This may be estimated with sufficient accuracy by
rubbing the filtered-off portions, insoluble in water between the fingers and a plate of
glass. The object of adding the sulfate of alumina is to transform the soap contained in
the lye into the insoluble aluminum soaps, and at the same time to coagulate the
albuminous impurities. It must be remembered that the sulfate of alumina is added only
for the fresh lye put into the tank. Thus if there were 10,000 pounds of lye in the treating
tank when the fresh lye was run in, and 50,000 pounds when the tank is filled, adding
nine pounds of sulfate of alumina per thousand of lye, only 360 pounds would be added
or enough for 40,000 pounds. Sulfate of alumina neutralizes one-third of its weight of
caustic. [Pg 109]

To determine the alkali in the sample, 10 cubic centimeters are pipetted into a beaker, a
little distilled water added, then 3 or 4 drops of phenolphthalein indicator. From a burette,
quarter normal (N/4) sulfuric acid is added until the pink color is just discharged. When
this point is reached 4 to 5 c. c. more of acid are added and the solution is boiled to expel
the carbon dioxide. Should the solution turn pink, it is necessary to add more acid. After
having boiled for 3 to 4 minutes, N/4 caustic soda is added until the pink color just
returns and the amount of caustic soda used is read on the burette. The difference
between the number of cubic centimeters of N/4 sulfuric acid and N/4 caustic soda gives
the amount of alkali in the sample. By using a 10 c. c. sample and N/4 sulfuric acid and
N/4 caustic soda each c. c. obtained by the difference of these two solutions is equal to
one-tenth of one per cent. (0.1%) of the total alkali in the lye. As an example, say we first
used 7.7 c. c. of N/4 sulfuric acid to just discharge the pink, then added 4 c. c. more, or
11.7 c. c. in total. After boiling it required 5.3 c. c. to bring back a slight pink, the total
alkalinity would be 11.7 c. c. - 5.3 c. c. = 6.4 c. c., or 0.64% total alkali in the lye in terms
of caustic soda. If there were 40,000 pounds of lye to be treated then we should have to
neutralize:

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40,000 × .0064 = 256 lbs. alkali. Since sulfate of alumina neutralizes one-third of its
weight in caustic, and there are say 9 lbs. of this added per thousand pounds of lye we
would add
40,000 × 9 = 360 lbs. of sulfate of alumina. This would neutralize 360 × 1/3 = 120 lbs of
alkali. There are then 256 - 120 = 136 lbs. of alkali still to be neutralized. If 60° B.
sulfuric acid is used it requires about 1.54 lbs. of acid to one pound of caustic. Therefore
to neutralize the caustic soda remaining it requires: [Pg 110]

136 × 1.54 = 209.44 lbs. 60° B. sulfuric acid to neutralize the total alkali in the 40,000
pounds of spent lye.
The acid is added and the lye well stirred, after which another sample is taken and again
titrated as before. From this titration the amount of acid to be added is again calculated
and more acid is added if necessary. Should too much acid have been added, caustic soda
solution is added until the lye is between exactly neutral and 0.02% alkaline. The filtered
lyes at this stage have a slight yellowish cast.
To be sure that the lyes are treated correctly the precipitation test is advisable. To carry
this out filter about 50 c. c. of the treated lye and divide into two portions in a test tube.
To one portion add ammonia drop by drop. If a cloudiness develops upon shaking, more
alkali is added to the lye in the tank. To the other portion add a few drops of 1 to 5
sulfuric acid and shake the test tube. If a precipitate develops or the solution clouds, more
acid is needed. When the lyes are treated right no cloudiness should develop either upon
adding ammonia or the dilute acid.
The properly treated lye is then run through the filter press while slightly warm and the
filtered lye is fed to the evaporator from the filtered lye tank. The lye coming from the
filter press should be clear and have a slight yellowish cast. As the pressure increases it is
necessary to clean the press or some of the press cake will pass through the cloths. Where
sodium silicate is used as a filler, the silicate scrap should never be returned to the soap
kettle until the glycerine lyes have been withdrawn. This practice of some soapmakers is
to be strongly censured, as it causes decided difficulty in filtering the lye, since during the
treatment of the lye, free silicic acid in colloidal form is produced by the decomposition
of the sodium silicate by acid. This often prevents filtering the treated lye even at excess [Pg 111]
pressure and at its best retards the filtering.
As to the filter press cake, this may be best thrown away in a small factory. Where,
however, the output of glycerine is very large it pays to recover both the fatty acids and
alumina in the press cakes.
In some cases, especially when the lyes are very dirty and the total residue in the crude
glycerine runs high, for which there is a penalty usually attached, a double filtration of
the lye is advisable. This is carried out by first making the lye slightly acid in reaction by
the addition of alum and acid, then filtering. This filtered lye is then neutralized to the
proper point with caustic, as already described, and passed through the filter press again.
While in the method of treating the lyes as given sulfuric acid is used for neutralizing,
some operators prefer to use hydrochloric acid, as this forms sodium chloride or common
salt, whereas sulfuric acid forms sodium sulfate, having 3/5 the graining power of salt,
which eventually renders the salt useless for graining the soap, as the percentage of
sodium sulfate increases in the salt. When the salt contains 25 per cent. sodium sulfate it
is advisable to throw it away. Sulfuric acid, however, is considerably cheaper than
hydrochloric and this more than compensates the necessity of having to eventually reject
the recovered salt. It may here also be mentioned that recovered salt contains 5-7 per
cent. glycerine which should be washed out in the evaporator before it is thrown away.
The following tables give the approximate theoretical amounts of acids of various
strengths required to neutralize one pound of caustic soda:
For 1 pound of caustic soda—

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3.25 lbs. 18° B. hydrochloric (muriatic) acid are required.

2.92 " 20° B. " " " " "
2.58 " 22° B. " " " " "

For 1 pound of caustic soda— [Pg 112]

1.93 lbs. 50° B. sulphuric acid are required.

1.54 " 60° B. " " " "
1.28 " 66° B. " " " "

It is, of course, feasible to neutralize the spent lye without first determining the causticity
by titrating a sample and this is often the case. The operator under such conditions first
adds the sulfate of alumina, then the acid, using litmus paper as his indicator.
Comparatively, this method of treatment is much slower and not as positive, as the
amount of acid or alkali to be added is at all times uncertain, for in the foaming of the
lyes their action on litmus is misleading.
After the lye has been filtered to the filtered lye tank it is fed to the evaporator, the
method of operation of which varies somewhat with different styles or makes. When it
first enters the evaporator the lye is about 11°-12° B. After boiling the density will
gradually rise to 27° B. and remain at this gravity for some time and during which time
most of the salt is dropped out in the salt filter. As the lye concentrates the gravity
gradually rises to 28°-30° B., which is half crude glycerine and contains about 60 per
cent. glycerine. Some operators carry the evaporation to this point and accumulate a
quantity of half crude before going on to crude. After half crude is obtained the
temperature on the evaporator increases, the vacuum increases and the pressure on the
condensation drain goes up (using the same amount of live steam). As the liquor grows
heavier the amount of evaporation is less, and less steam is required necessitating the
regulation of the steam pressure on the drum. When a temperature of 210° F. on the
evaporator, with 26 or more inches vacuum on the pump is arrived at, the crude stage has
been reached and the liquor now contains about 80 per cent. glycerine in which shape it
is usually sold by soap manufacturers. A greater concentration requires more intricate [Pg 113]
apparatus. After settling a day in the crude tank it is drummed.
Crude glycerine (about 80 per cent. glycerol) free from salt is 33° B., or has a specific
gravity of 1.3. A sample boiled in an open dish boils at a temperature of 155° C. or over.

TWITCHELL PROCESS.
The Twitchell process of saponification consists of causing an almost complete cleavage
of fats and oils by the use of the Twitchell reagent or saponifier, a sulfo-aromatic
compound. This is made by the action of concentrated sulfuric acid upon a solution of
oleic acid or stearic acid in an aromatic hydrocarbon. From 0.5 per cent. to 3 per cent. of
the reagent is added and saponification takes place from 12-48 hours by heating in a
current of live steam. The reaction is usually accelerated by the presence of a few per
cent. of free fatty acids as a starter. Recently the Twitchell double reagent has been
introduced through which it is claimed that better colored fatty acids are obtained and the
glycerine is free from ash.

The advantages claimed for the Twitchell process as outlined by Joslin[12] are as follows:
1. All the glycerine is separated from the stock before entering the kettle, preventing loss
of glycerine in the soap and removing glycerine from spent lye.
2. The liquors contain 15-20 per cent. glycerine whereas spent lyes contain but 3-5 per
cent. necessitating less evaporation and consequently being more economical in steam,
labor and time.
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3. No salt is obtained in the liquors which makes the evaporation cheaper and removes
the cause of corrosion of the evaporator; also saves the glycerine retained by the salt. [Pg 114]

4. The glycerine liquors are purer and thus the treatment of the lyes is cheaper and
simpler and the evaporation less difficult.
5. The glycerine can readily be evaporated to 90 per cent. crude rather than 80 per cent.
crude, thus saving drums, labor in handling and freight. The glycerine furthermore
receives a higher rating and price, being known as saponification crude which develops
no glycols in refining it.
6. The fatty acids obtained by the Twitchell saponifier may be converted into soap by
carbonates, thus saving cost in alkali.
7. There is a decrease in the odor of many strong smelling stocks.
8. The glycerine may be obtained from half boiled and cold made soaps as well as soft
(potash) soaps.
While the advantages thus outlined are of decided value in the employment of the
Twitchell process, the one great disadvantage is that the fatty acids obtained are rather
dark in color and are not satisfactorily employed for the making of a soap where
whiteness of color is desired.
To carry out the process the previously heated oil or fat to be saponified is run into a lead
lined tank. As greases and tallow often contain impurities a preliminary treatment with
sulfuric acid is necessary. For a grease 1.25 per cent. of half water and half 66° B.
sulfuric acid is the approximate amount. The undiluted 66° B. acid should never be added
directly, as the grease would be charred by this. The grease should be agitated by steam
after the required percentage of acid, calculated on the weight of the grease, has been
added. The wash lye coming off should be 7°-10° B. on a good clean grease or 15°-22°
B. on cotton oil or a poor grease. As has been stated the grease is heated before the acid is [Pg 115]
added or the condensation of the steam necessitates the addition of more acid. After
having boiled for 1-2 hours the grease is allowed to settle for 12 hours and run off
through a swivel pipe.
After the grease has been washed, as just explained, and settled, it is pumped into a
covered wooden tank containing an open brass coil. Some of the second lye from a
previous run is usually left in this tank and the grease pumped into this. The amount of
this lye should be about one-third to one-half the weight of the grease so that there is
about 60 per cent. by weight of grease in the tank after 24 hours boiling. Where occasions
arise when there is no second lye about 50 per cent. by weight of distilled water to the
amount of grease is run into the tank to replace the lye. The saponifier is then added
through a glass or granite ware funnel after the contents of the tank have been brought to
a boil. If the boiling is to be continued 48 hours, 1 per cent. of saponifier is added. For 24
hours boiling add 1.5 per cent. The boiling is continued for 24-48 hours allowing 18
inches for boiling room or the grease will boil over.
After boiling has continued the required length of time the mass is settled and the
glycerine water is drawn off to the treatment tank. Should a permanent emulsion have
formed, due to adding too great an amount of saponifier, a little sulfuric acid (0.1 per
cent.-0.3 per cent.) will readily break this. During the time this is being done the space
between the grease and the cover on the tank is kept filled with steam as contact with the
air darkens the fatty acids.
To the grease remaining in the tank distilled water (condensed water from steam coils) to
one-half its volume is added and the boiling continued 12-24 hours. The grease is then [Pg 116]
settled and the clear grease run off through a swivel pipe. A layer of emulsion usually
forms between the clear grease and lye so that it may easily be determined when the
grease has all been run off. To prevent discoloration of the fatty acids it is necessary to
neutralize the lye with barium carbonate. The amount of this to be added depends upon
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the percentage of saponifier used. About 1/10 the weight of saponifier is the right
amount. The barium carbonate is added through the funnel at the top of the tank mixed
with a little water and the lye tested until it is neutral to methyl orange indicator. When
the fatty acids are thus treated they will not darken upon exposure to the air when run off.
Fresh grease is now pumped into the lye or water remaining in the tank and the process
repeated.
The glycerine water or first lye is run to the treatment tank, the fat skimmed off and
neutralized with lime until it shows pink with phenolphthalein, after having been
thoroughly boiled with steam. About 0.25 per cent. lime is the proper amount to add. The
mixture is then allowed to settle and the supernatant mixture drawn off and run to the
glycerine evaporator feed tank. The lime which holds considerable glycerine is filtered
and the liquor added to the other. The evaporation is carried out in two stages. The
glycerine water is first evaporated to about 60 per cent. glycerol, then dropped into a
settling tank to settle out the calcium sulfate. The clear liquor is then evaporated to crude
(about 90 per cent. glycerine) and the sediment filtered and also evaporated to crude.
As to the amount of saponifier to use on various stocks, this is best determined by
experiment as to how high a percentage gives dark colored fatty acids. For good stock
such as clean tallow, prime cottonseed oil, corn oil, cocoanut oil and stock of this kind
0.75 per cent. saponifier is sufficient. For poorer grades of tallow, house grease, poor [Pg 117]
cottonseed oil, etc., 1 per cent. saponifier is required and for poorer grade greases higher
percentages. The percentage of fatty acids developed varies in various stocks, and also
varies with the care that the operation is carried out, but is usually between 85 per
cent.-95 per cent. Due to the water taken up in the saponification process there is a yield
of about 103 pounds of fatty acids and glycerine for 100 pounds of fat.
The Twitchell reagent has undoubtedly caused a decided advance in the saponification of
fats and oils and has been of great value to the soap manufacturer, because with a small
expenditure it is possible to compete with the much more expensive equipment necessary
for autoclave saponification. The drawback, however, has been that the reagent imparted
a dark color to the fatty acids obtained, due to decomposition products forming when the
reagent is made, and hence is not suitable for use in soaps where whiteness of color is
desired.
There have recently been two new reagents introduced which act as catalyzers in splitting
fats, just as the Twitchell reagent acts, but the fatty acids produced by the cleavage are of
good color. The saponification, furthermore, takes place more rapidly. These are the
Pfeilring reagent and Kontact reagent.
The Pfeilring reagent is very similar to the Twitchell reagent, being made from
hydrogenated castor oil and naphthalene by sulfonation with concentrated sulfuric acid. It
is manufactured in Germany and is being extensively used in that country with good
success.
The Kontact or Petroff reagent, discovered by Petroff in Russia, is made from sulfonated
mineral oils. Until very recently it has only been manufactured in Europe, but now that it
has been found possible to obtain the proper mineral constituent from American [Pg 118]
petroleum, it is being manufactured in this country, and it is very probable that it will
replace the Twitchell reagent because of the advantages derived by using it, as compared
to the old Twitchell reagent.
The method and equipment necessary for employing either the Pfeilring or Kontact
reagents is exactly the same as in using the Twitchell process.

AUTOCLAVE SAPONIFICATION.
While the introduction of the Twitchell process to a great extent replaced the autoclave
method of saponification for obtaining fatty acids for soap making, the autoclave method
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is also used. This process consists in heating the previously purified fat or oil in the
presence of lime and water, or water only, for several hours, which causes a splitting of
the glycerides into fatty acids and glycerine. The advantage of autoclave saponification
over the Twitchell process is that a greater cleavage of the fats and oils results in less time
and at a slightly less expense. The glycerine thus obtained is also purer and of better color
than that obtained by Twitchelling the fats.
An autoclave or digestor consists of a strongly constructed, closed cylindrical tank,
usually made of copper, and is so built as to resist internal pressure. The digestor is
usually 3 to 5 feet in diameter and from 18 to 25 feet high. It may be set up horizontally
or vertically and is covered with an asbestos jacket to retain the heat. Various inlets and
outlets for the fats, steam, etc., as well as a pressure gauge and safety valve are also a
necessary part of the equipment.

LIME SAPONIFICATION.
The saponification in an autoclave is usually carried out by introducing the fats into the
autoclave with a percentage of lime, magnesia or zinc oxide, together with water. If the [Pg 119]
fats contain any great amount of impurities, it is first necessary to purify them either by a
treatment with weak sulfuric acid, as described under the Twitchell process, or by boiling
them up with brine and settling out the impurities from the hot fat.
To charge the autoclave a partial vacuum is created therein by condensation of steam just
before running the purified oil in from an elevated tank. The required quantity of
unslaked lime, 2 to 4 per cent. of the weight of the fat, is run in with the molten fat,
together with 30 per cent. to 50 per cent. of water. While 8.7 per cent. lime is
theoretically required, practice has shown that 2 per cent. to 4 per cent. is sufficient. The
digestor, having been charged and adjusted, steam is turned on and a pressure of 8 to 10
atmospheres maintained thereon for a period of six to ten hours. Samples of the fat are
taken at various intervals and the percentage of free fatty acids determined. When the
saponification is completed the contents of the autoclave are removed, usually by
blowing out the digestor into a wooden settling tank, or by first running off the glycerine
water and then blowing out the lime, soap and fatty acids. The mass discharged from the
digestor separates into two layers, the upper consisting of a mixture of lime soap or
"rock" and fatty acids, and the lower layer contains the glycerine or "sweet" water. The
glycerine water is first run off through a clearing tank or oil separator, if this has not been
done directly from the autoclave, and the mass remaining washed once or twice more
with water to remove any glycerine still retained by the lime soap. The calculated amount
of sulfuric acid to decompose the lime "rock" is then added, and the mass agitated until
the fatty acids contained therein are entirely set free. Another small wash is then given
and the wash water added to the glycerine water already run off. The glycerine water is [Pg 120]
neutralized with lime, filtered and concentrated as in the Twitchell process.
Due to the difficulties of working the autoclave saponification with lime, decomposing
the large amount of lime soap obtained and dealing with much gypsum formed thereby
which collects as a sediment and necessitates cleaning the tanks, other substances are
used to replace lime. Magnesia, about 2 per cent. of the weight of the fat, is used and
gives better results than lime. One-half to 1 per cent. of zinc oxide of the weight of the fat
is even better adapted and is now being extensively employed for this purpose. In using
zinc oxide it is possible to recover the zinc salts and use them over again in the digestor,
which makes the process as cheap to work as with lime, with far more satisfactory
results.

ACID SAPONIFICATION.

While it is possible to saponify fats and oils in an autoclave with the addition of acid to
the fat, unless a specially-constructed digestor is built, the action of the acid on the metal

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from which the autoclave is constructed prohibits its use. The acid saponification is
therefore carried out by another method.
The method of procedure for acid saponification, therefore, is to first purify the fats with
dilute acid as already described. The purified, hot or warm, dry fat is then run to a
specially-built acidifier or a lead-lined tank and from 4 per cent. to 6 per cent. of
concentrated sulfuric acid added to the fat, depending upon its character, the degree of
saponification required, temperature and time of saponification. A temperature of 110
degrees C. is maintained and the mass mixed from four to six hours. The tank is then
allowed to settle out the tar formed during the saponification, and the fatty acids run off [Pg 121]
to another tank and boiled up about three times with one-third the amount of water. The
water thus obtained contains the glycerine, and after neutralization is concentrated.

AQUEOUS SAPONIFICATION.
While lime or a similar substance is ordinarily used to aid in splitting fats in an autoclave,
the old water process is still used. This is a convenient, though slower and more
dangerous method, of producing the hydrolysis of the glyceride, as well as the simplest in
that fatty acids and glycerine in a water solution are obtained. The method consists in
merely charging the autoclave with fats and adding about 30 per cent. to 40 per cent. of
their weight of water, depending on the amount of free fatty acid and subjecting the
charge to a pressure of 150 to 300 pounds, until the splitting has taken place. This is a
much higher pressure than when lime is used and therefore a very strong autoclave is
required. Since fatty acids and pure glycerine water are obtained no subsequent treatment
of the finished charge is necessary except separating the glycerine water and giving the
fatty acids a wash with water to remove all the glycerine from them.

SPLITTING FATS WITH FERMENTS.

In discussing the causes of rancidity of oils and fats it was pointed out that the initial
splitting of these is due to enzymes, organized ferments. In the seeds of the castor oil
plant, especially in the protoplasm of the seed, the enzyme which has the property of
causing hydrolysis of the glycerides is found. The ferment from the seeds of the castor oil
plant is now extracted and used upon a commercial basis for splitting fats.
The equipment necessary to carry out this method of saponification is a round, iron, lead- [Pg 122]
lined tank with a conical bottom, preferably about twice as long as it is wide. Open and
closed steam coils are also necessary in the tank.
The oils are first heated and run into this tank. The right temperature to heat these to is
about 1 degree to 2 degrees above their solidification point. For liquid oils 23 degrees C.
is the proper heat as under 20 degrees C. the cleavage takes place slowly. Fats titering 44
degrees C. or above must be brought down in titer by mixing with them oils of a lower
titer as the ferment or enzyme is killed at about 45 degrees C. and thus loses its power of
splitting. It is also necessary to have the fat in the liquid state or the ferment does not act.
The proper temperature must be maintained with dry steam.
It is, of course, necessary to add water, which may be any kind desired, condensed, water
from steam coils, well, city, etc. From 30 per cent. to 40 per cent., on the average 35 per
cent. of water is added, as the amount necessary is regulated so as to not dilute the
glycerine water unnecessarily. To increase the hydrolysis a catalyzer, some neutral salt,
usually manganese sulfate is added in the proportion of 0.15 per cent. appears to vary
directly as the saponification number of the fat or oil. The approximate percentages of
fermentive substance to be added to various oils and fats follow:

Cocoanut oil 8%
Palm Kernel oil 8%

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Cottonseed oil 6-7%

Linseed oil 4-5%
Tallow oil 8-10%

The oil, water, manganese sulfate and ferment having been placed in the tank in the order
named, the mixture is agitated with air for about a quarter of an hour to form an even [Pg 123]
emulsion, in which state the mass is kept by stirring occasionally with air while the
saponification is taking place. A temperature is maintained a degree or two above the titer
point of the fat with closed steam which may be aided by covering the tank for a period
of 24 to 48 hours. The splitting takes place rapidly at first, then proceeds more slowly. In
24 hours 80 per cent. of the fats are split and in 48 hours 85 per cent. to 90 per cent.
When the cleavage has reached the desired point the mass is heated to 80 degrees-85
degrees C. with live or indirect steam while stirring with air. Then 0.1 per cent.-0.15 per
cent of concentrated sulfuric acid diluted with water is added to break the emulsion.
When the emulsion is broken the glycerine water is allowed to settle out and drawn off.
The glycerine water contains 12 per cent. to 25 per cent. glycerine and contains
manganese sulfate, sulfuric acid and albuminous matter. Through neutralization with lime
at boiling temperature and filtration the impurities can almost all be removed after which
the glycerine water may be fed to the evaporator. Should it be desired to overcome the
trouble due to the gypsum formed in the glycerine, the lime treatment may be combined
with a previous treatment of the glycerine water with barium hydrate to remove the
sulfuric acid, then later oxalic acid to precipitate the lime.
The fatty acids obtained by splitting with ferments are of very good color and adaptable
for soap making.

KREBITZ PROCESS.
The Krebitz process which has been used to some extent in Europe is based upon the
conversion of the fat or oil into lime soap which is transformed into the soda soap by the
addition of sodium carbonate. To carry out the process a convenient batch of, say, 10,000
pounds of fat or oil, is run into a shallow kettle containing 1,200 to 1,400 pounds of lime [Pg 124]
previously slaked with 3,700 to 4,500 pounds of water. The mass is slowly heated with
live steam to almost boiling until an emulsion is obtained. The tank is then covered and
allowed to stand about 12 hours. The lime soap thus formed is dropped from the tank into
the hopper of a mill, finely ground and conveyed to a leeching tank. The glycerine is
washed out and the glycerine water run to a tank for evaporation. The soap is then further
washed and these washings are run to other tanks to be used over again to wash a fresh
batch of soap. About 150,000 pounds of water will wash the soap made from 10,000
pounds of fat which makes between 15,000 and 16,000 pounds of soap. The first wash
contains approximately 10 per cent. glycerine and under ordinary circumstances this only
need be evaporated for glycerine recovery.
After extracting the glycerine the soap is slowly introduced into a boiling solution of
sodium carbonate or soda ash and boiled until the soda has replaced the lime. This is
indicated by the disappearance of the small lumps of lime soap. Caustic soda is then
added to saponify the fat not converted by the lime saponification. The soap is then salted
out and allowed to settle out the calcium carbonate. This drops to the bottom of the kettle
as a heavy sludge entangling about 10 per cent. of the soap. A portion of this soap may be
recovered by agitating the sludge with heat and water, pumping the soap off the top and
filtering the remaining sludge.
While the soap thus obtained is very good, the percentage of glycerine recovered is
greatly increased and the cost of alkali as carbonate is less. The disadvantages are many.
Large quantities of lime are required; it is difficult to recover the soap from the lime
sludge; the operations are numerous prior to the soap making proper and rather
complicated apparatus is required. [Pg 125]
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DISTILLATION OF FATTY ACIDS.

The fatty acids obtained by various methods of saponification may be further improved
by distillation.
In order to carry out this distillation, two methods may be pursued, first, the continuous
method, whereby the fatty acids are continually distilled for five to six days, and, second,
the two phase method, whereby the distillation continues for 16 to 20 hours, after which
the residue is drawn off, treated with acid, and its distillate added to a fresh charge of
fatty acids. The latter method is by far the best, since the advantages derived by thus
proceeding more than compensate the necessity of cleaning the still. Better colored fatty
acids are obtained; less unsaponifiable matter is contained therein; there is no
accumulation of impurities; the amount of neutral fat is lessened because the treatment of
the tar with acid causes a cleavage of the neutral fat and the candle tar or pitch obtained is
harder and better and thus more valuable.
The stills are usually built of copper, which are heated by both direct fire and superheated
steam. Distillation under vacuum is advisable. To begin the distilling operation, the still is
first filled with dry hot fatty acids to the proper level. Superheated steam is then admitted
and the condenser is first heated to prevent the freezing of the fatty acids, passing over
into same. When the temperature reaches 230 deg. C. the distillation begins. At the
beginning, the fatty acids flow from the condenser, an intense green color, due to the
formation of copper soaps produced by the action of the fatty acids on the copper still.
This color may easily be removed by treating with dilute acid to decompose the copper
soaps.
In vacuum distillation, the operation is begun without the use of vacuum. Vacuum is [Pg 126]
introduced only when the distillation has proceeded for a time and the introduction of this
must be carefully regulated, else the rapid influence of vacuum will cause the contents of
the still to overflow. When distillation has begun a constant level of fatty acids is retained
therein by opening the feeding valve to same, and the heat is so regulated as to produce
the desired rate of distillation. As soon as the distillate flows darker and slower, the
feeding valve to the still is shut off and the distillation continued until most of the
contents of the still are distilled off, which is indicated by a rise in the temperature.
Distillation is then discontinued, the still shut down, and in about an hour the contents are
sufficiently cool to be emptied. The residue is run off into a proper receiving vessel,
treated with dilute acid and used in the distillation of tar.
In the distillation of tar the same method as the above is followed, only distillation
proceeds at a higher temperature. The first portion and last portion of the distillate from
tar are so dark that it is necessary to add them to a fresh charge of fatty acids. By a well
conducted distillation of tar about 50 per cent. of the fatty acids from the tar can be used
to mix with the distilled fatty acids. The residue of this operation called stearine pitch or
candle tar consists of a hard, brittle, dark substance. Elastic pitch only results where
distillation has been kept constant for several days without interrupting the process, and
re-distilling the tar. In a good distillation the distillation loss is 0.5 to 1.5% and loss in
pitch 1.5%. Fatty acids which are not acidified deliver about 3% of pitch. Very impure
fats yield even a higher percentage in spite of acidifying. For a long time it was found
impossible to find any use for stearine pitch, but in recent years a use has been found for
same in the electrical installation of cables.

FOOTNOTES:
[12] Journ. Ind. Eng. Chem. (1909), I, p. 654.

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CHAPTER VI [Pg 127]

Analytical Methods.

While it is possible to attain a certain amount of efficiency in determining the worth of

the raw material entering into the manufacture of soap through organoleptic methods,
these are by no means accurate. It is, therefore, necessary to revert to chemical methods
to correctly determine the selection of fats, oil or other substances used in soap making,
as well as standardizing a particular soap manufactured and to properly regulate the
glycerine recovered.
It is not our purpose to cover in detail the numerous analytical processes which may be
employed in the examination of fats and oils, alkalis, soap and glycerine, as these are
fully and accurately covered in various texts, but rather to give briefly the necessary tests
which ought to be carried out in factories where large amounts of soap are made.
Occasion often arises where it is impossible to employ a chemist, yet it is possible to
have this work done by a competent person or to have someone instruct himself as just
how to carry out the more simple analyses, which is not a very difficult matter. The
various standard solutions necessary to carrying out the simpler titrations can readily be
purchased from dealers in chemical apparatus and it does not take extraordinary
intelligence for anyone to operate a burette, yet in many soap plants in this country
absolutely no attention is paid to the examining of raw material, though many thousand
pounds are handled annually, which, if they were more carefully examined would result
in the saving of much more money than it costs to examine them or have them at least [Pg 128]
occasionally analyzed.

ANALYSIS OF FATS AND OILS.

In order to arrive at proper results in the analysis of a fat or oil, it is necessary to have a
proper sample. To obtain this a sample of several of the packages of oil or fat is taken and
these mixed or molten together into a composite sample which is used in making the
tests. If the oil or fat is solid, a tester is used in taking the sample from the package and if
they are liquid, it is a simple matter to draw off a uniform sample from each package and
from these to form a composite sample.
In purchasing an oil or fat for soap making, the manufacturer is usually interested in the
amount of free fatty acid contained therein, of moisture, the titer, the percentage of
unsaponifiable matter and to previously determine the color of soap which will be
obtained where color is an object.

DETERMINATION OF FREE FATTY ACIDS.

Since the free fatty acid content of a fat or oil represents a loss of glycerine, the greater
the percentage of free fatty acid, the less glycerine is contained in the fat or oil, it is
advisable to purchase a fat or oil with the lower free acid, other properties and the price
being the same.
While the mean molecular weight of the mixed free fatty acids varies with the same and
different oils or fats and should be determined for any particular analysis for accuracy,
the free fatty acid is usually expressed as oleic acid, which has a molecular weight of
282.
To carry out the analysis 5 to 20 grams of the fat are weighed out into an Erlenmeyer [Pg 129]
flask and 50 cubic centimeters of carefully neutralized alcohol are added. In order to
neutralize the alcohol add a few drops of phenolphthalein solution to same and add a
weak caustic soda solution drop by drop until a very faint pink color is obtained upon
shaking or stirring the alcohol thoroughly. The mixture of fat and neutralized alcohol is
then heated to boiling and titrated with tenth normal alkali solution, using
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phenolphthalein as an indicator. As only the free fatty acids are readily soluble in the
alcohol and the fat itself only slightly mixes with it, the flask should be well agitated
toward the end of the titration. When a faint pink color remains after thoroughly agitating
the flask the end point is reached. In order to calculate the percentage of free fatty acid as
oleic acid, multiply the number of cubic centimeters of tenth normal alkali used as read
on the burette by 0.0282 and divide by the number of grams of fat taken for the
determination and multiply by 100.
When dark colored oils or fats are being titrated it is often difficult to obtain a good end
point with phenolphthalein. In such cases about 2 cubic centimeters of a 2 per cent.
alcoholic solution of Alkali Blue 6 B is recommended.
Another method of directly determining the free fatty acid content of tallow or grease
upon which this determination is most often made is to weigh out into an Erlenmeyer
flask exactly 5.645 grams of a sample of tallow or grease. Add about 75 cubic
centimeters of neutralized alcohol. Heat until it boils, then titrate with tenth normal alkali
and divide the reading by 2, which gives the percentage of free fatty acid as oleic. If a
fifth normal caustic solution is used, the reading on the burette gives the percentage of
free fatty acid directly. This method, while it eliminates the necessity of calculation, is [Pg 130]
troublesome in that it is difficult to obtain the exact weight of fat.

MOISTURE.
To calculate the amount of moisture contained in a fat or oil 5 to 10 grams are weighed
into a flat bottom dish, together with a known amount of clean, dry sand, if it is so
desired. The dish is then heated over a water bath, or at a temperature of 100-110 degs.
C., until it no longer loses weight upon drying and reweighing the dish. One hour should
elapse between the time the dish is put on the water bath and the time it is taken off to
reweigh. The difference between the weight of the dish is put on the water bath and the
time it is taken off when it reaches a constant weight is moisture. This difference divided
by the original weight of the fat or oil × 100 gives the percentage of moisture.
When highly unsaturated fats or oils are being analyzed for moisture, an error may be
introduced either by the absorption of oxygen, which is accelerated at higher temperature,
or by the formation of volatile fatty acids. The former causes an increase in weight, the
latter causes a decrease. To obviate this, the above operation of drying should be carried
out in the presence of some inert gas like hydrogen, carbon dioxide, or nitrogen.

TITER.

The titer of a fat or oil is really an indication of the amount of stearic acid contained
therein. The titer, expressed in degrees Centigrade, is the solidification point of the fatty
acids of an oil or fat. In order to carry out the operation a Centigrade thermometer
graduated in one or two-tenths of a degree is necessary. A thermometer graduated [Pg 131]
between 10 degs. centigrade to 60 degs. centigrade is best adapted and the graduations
should be clear cut and distinct.
To make the determination about 30 grams of fat are roughly weighed in a metal dish and
30-40 cubic centimeters of a 30 per cent. (36 degs. Baumé) solution of sodium
hydroxide, together with 30-40 cubic centimeters of alcohol, denatured alcohol will do,
are added and the mass heated until saponified. Heat over a low flame or over an asbestos
plate until the soap thus formed is dry, constantly stirring the contents of the dish to
prevent burning. The dried soap is then dissolved in about 1000 cubic centimeters of
water, being certain that all the alcohol has been expelled by boiling the soap solution for
about half an hour. When the soap is in solution add sufficient sulphuric acid to
decompose the soap, approximately 100 cubic centimeters of 25 degs. Baumé sulphuric
acid, and boil until the fatty acids form a clear layer on top of the liquid. A few pieces of
pumice stone put into the mixture will prevent the bumping caused by boiling. Siphon off

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the water from the bottom of the dish and wash the fatty acids with boiling water until
free from sulphuric acid. Collect the fatty acids in a small casserole or beaker and dry
them over a steam bath or drying oven at 110 degs. Centigrade. When the fatty acids are
dry, cool them to about 10 degs. above the titer expected and transfer them to a titer tube
or short test tube which is firmly supported by a cork in the opening of a salt mouth
bottle. Hang the thermometer by a cord from above the supported tube so it reaches close
to the bottom when in the titer tube containing the fatty acids and so that it may be used
as a stirrer. Stir the mass rather slowly, closely noting the temperature. The temperature
will gradually fall during the stirring operation and finally remain stationary for half a [Pg 132]
minute or so then rise from 0.1 to 0.5 degs. The highest point to which the mercury rises
after having been stationary is taken as the reading of the titer.

DETERMINATION OF UNSAPONIFIABLE MATTER.

In order to determine the unsaponifiable matter in fats and oils they are first saponified,
then the unsaponifiable, which consists mainly of hydrocarbons and the higher alcohols
cholesterol or phytosterol, is extracted with ether or petroleum ether, the ether evaporated
and the residue weighed as unsaponifiable.
To carry out the process first saponify about 5 grams of fat or oil with an excess of
alcoholic potassium hydrate, 20-30 cubic centimeters of a 1 to 10 solution of potassium
hydroxide in alcohol until the alcohol is evaporated over a steam bath. Wash the soap
thus formed into a separatory funnel of 200 cubic centimeters capacity with 80-100 cubic
centimeters water. Then add about 60 cubic centimeters of ether, petroleum ether or 86
degs. gasoline and thoroughly shake the funnel to extract the unsaponifiable. Should the
two layers not separate readily, add a few cubic centimeters of alcohol, which will readily
cause them to separate. Draw off the watery solution from beneath and wash the ether
with water containing a few drops of sodium hydrate and run to another dish. Pour the
watery solution into the funnel again and repeat the extraction once or twice more or until
the ether shows no discoloration. Combine the ether extractions into the funnel and wash
with water until no alkaline reaction is obtained from the wash water. Run the ether
extract to a weighed dish, evaporate and dry rapidly in a drying oven. As some of the [Pg 133]
hydrocarbons are readily volatile at 100 degs. Centigrade, the drying should not be
carried on any longer than necessary. The residue is then weighed and the original weight
of fat taken divided into the weight of the residue × 100 gives the percentage
unsaponifiable.

TEST FOR COLOR OF SOAP.

It is often desirable to determine the color of the finished soap by a rapid determination
before it is made into soap. It often happens, especially with the tallows, that a dark
colored sample produces a light colored soap, whereas a bleached light colored tallow
produces a soap off shade.
To rapidly determine whether the color easily washes out of the tallow with lye, 100
cubic centimeters of tallow are saponified in an enameled or iron dish with 100 cubic
centimeters of 21 degs. Baumé soda lye and 100 cubic centimeters of denatured alcohol.
Continue heating over a wire gauze until all the alcohol is expelled and then add 50 cubic
centimeters of the 21 degs. Baumé lye to grain the soap. Allow the lyes to settle and with
an inverted pipette draw off the lyes into a test tube or bottle. Close the soap with 100
cubic centimeters of hot water and when closed again grain with 50 cubic centimeters of
the lye by just bringing to a boil over an open flame. Again allow the lyes to settle and
put aside a sample of the lye for comparison. Repeat the process of closing, graining and
settling and take a sample of lye. If the lye is still discolored repeat the above operations
again or until the lye is colorless. Ordinarily all the color will come out with the third lye.
The soap thus obtained contains considerable water which makes it appear white. The
soap is, therefore, dried to about 15 per cent. moisture and examined for color. The color [Pg 134]
thus obtained is a very good criterion as to what may be expected in the soap kettle.
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By making the above analyses of fats or oils the main properties as to their adaptability
for being made into soap are determined. In some cases, especially where adulteration or
mixtures of oils are suspected, it is necessary to further analyze same. The methods of
carrying out these analyses are fully covered by various texts on fats and oils and we will
not go into details regarding the method of procedure in carrying these out.

TESTING OF ALKALIS USED IN SOAP MAKING.

The alkalis entering into the manufacture of soap such as caustic soda or sodium
hydroxide, caustic potash or potassium hydrate, carbonate of soda or sodium carbonate,
carbonate of potash or potassium carbonate usually contain impurities which do not enter
into combination with the fats or fatty acids to form soap. It is out of the question to use
chemically pure alkalis in soap making, hence it is often necessary to determine the
alkalinity of an alkali. It may again be pointed out that in saponifying a neutral fat or oil
only caustic soda or potash are efficient and the carbonate contained in these only
combines to a more or less extent with any free fatty acids contained in the oils or fats.
Caustic soda or potash or lyes made from these alkalis upon exposure to the air are
gradually converted into sodium or potassium carbonate by the action of the carbon
dioxide contained in the air. While the amount of carbonate thus formed is not very great
and is greatest upon the surface, all lyes as well as caustic alkalis contain some carbonate.
This carbonate introduces an error in the analysis of caustic alkalis when accuracy is
required and thus in the analysis of caustic soda or potash it is necessary to remove the
carbonate when the true alkalinity as sodium hydroxide or potassium hydroxide is [Pg 135]
desired. This may be done by titration in alcohol which has been neutralized.
In order to determine the alkalinity of any of the above mentioned alkalis, it is first
necessary to obtain a representative sample of the substance to be analyzed. To do this
take small samples from various portions of the package and combine them into a
composite sample. Caustic potash and soda are hygroscopic and samples should be
weighed at once or kept in a well stoppered bottle. Sodium or potassium carbonate can be
weighed more easily as they do not rapidly absorb moisture from the air.
To weigh the caustic soda or potash place about five grams on a watch glass on a balance
and weigh as rapidly as possible. Wash into a 500 cubic centimeter volumetric flask and
bring to the mark with distilled water. Pipette off 50 cubic centimeters into a 200 cubic
centimeter beaker, dilute slightly with distilled water, add a few drops of methyl orange
indicator and titrate with normal acid. For the carbonates about 1 gram may be weighed,
washed into a 400 cubic centimeter beaker, diluted with distilled water, methyl orange
indicator added and titrated with normal acid. It is advisable to use methyl orange
indicator in these titrations as phenolphthalein is affected by the carbon dioxide generated
when an acid reacts with a carbonate and does not give the proper end point, unless the
solution is boiled to expel the carbon dioxide. Litmus may also be used as the indicator,
but here again it is necessary to boil as carbon dioxide also affects this substance. As an
aid to the action of these common indicators the following table may be helpful: [Pg 136]

Indicator. Color in Acid Solution. Color in Alkaline Solution. Action of CO2.

Methyl orange Red Yellow Very slightly acid
Phenolphthalein Colorless Red Acid
Litmus Red Blue Acid

It may be further stated that methyl orange at the neutral point is orange in color.
To calculate the percentage of effective alkali from the above titrations, it must be first
pointed out that in the case of caustic potash or soda aliquot portions are taken. This is
done to reduce the error necessarily involved by weighing, as the absorption of water is
decided. Thus we had, say, exactly 5 grams which weighed 5.05 grams by the time it was
balanced. This was dissolved in 500 cubic centimeters of water and 50 cubic centimeters
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or one tenth of the amount of the solution was taken, or in each 50 cubic centimeters
there were 0.505 grams of the sample. We thus reduced the error of weighing by one
tenth provided other conditions introduce no error. In the case of the carbonates the
weight is taken directly.
One cubic centimeter of a normal acid solution is the equivalent of:

Grams.
Sodium Carbonate, Na2CO3 0.05305
Sodium Hydroxide, NaOH 0.04006
Sodium Oxide, Na2O 0.02905
Carbonate K2CO3 0.06908
Potassium Hydroxide, KOH 0.05616
Potassium Oxide, K2O 0.04715

Hence to arrive at the alkalinity we multiply the number of cubic centimeters, read on the
burette, by the factor opposite the terms in which we desire to express the alkalinity,
divide the weight in grams thus obtained by the original weight taken, and multiply the
result by 100, which gives the percentage of alkali in the proper terms. For example, say, [Pg 137]
we took the 0.505 grams of caustic potash as explained above and required 8.7 cubic
centimeter normal acid to neutralize the solution, then
8.7 × .05616 = .4886 grams KOH in sample
.4886
----- × 100 = 96.73% KOH in sample.
.505
Caustic potash often contains some caustic soda, and while it is possible to express the
results in terms of KOH, regardless of any trouble that may be caused by this mixture in
soap making, an error is introduced in the results, not all the alkali being caustic potash.
In such cases it is advisable to consult a book on analysis as the analysis is far more
complicated than those given we will not consider it. The presence of carbonates, as
already stated, also causes an error. To overcome this the alkali is titrated in absolute
alcohol, filtering off the insoluble carbonate. The soluble portion is caustic hydrate and
may be titrated as such. The carbonate remaining on the filter paper is dissolved in water
and titrated as carbonate.

SOAP ANALYSIS.

To obtain a sample of a cake of soap for analysis is a rather difficult matter as the
moisture content of the outer and inner layer varies considerably. To overcome this
difficulty a borer or sampler may be run right through the cake of soap, or slices may be
cut from various parts of the cake, or the cake may be cut and run through a meat
chopper several times and mixed. A sufficient amount of a homogeneous sample obtained
by any of these methods is preserved for the entire analysis by keeping the soap in a
securely stoppered bottle.
The more important determinations of soap are moisture, free alkali, or fatty acid,
combined alkali and total fatty matter. Besides these it is often necessary to determine [Pg 138]
insoluble matter, glycerine, unsaponifiable matter, rosin and sugar.

MOISTURE.

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The analysis of soap for moisture, at its best, is most unsatisfactory, for by heating it is
impossible to drive off all the water, and on the other hand volatile oils driven off by heat
are a part of the loss represented as moisture.
The usual method of determining moisture is to weigh 2 to 3 grams of finely shaved soap
on a watch glass and heat in an oven at 105 degrees C. for 2 to 3 hours. The loss in
weight is represented as water, although it is really impossible to drive off all the water in
this way.
To overcome the difficulties just mentioned either the Smith or Fahrion method may be
used. Allen recommends Smith's method which is said to be truthful to within 0.25 per
cent. Fahrion's method, according to the author, gives reliable results to within 0.5 per
cent. Both are more rapid than the above manipulation. To carry out the method of Smith,
5 to 10 grams of finely ground soap are heated over a sand bath with a small Bunsen
flame beneath it, in a large porcelain crucible. The heating takes 20 to 30 minutes, or
until no further evidence is present of water being driven off. This may be tested by the
fogging of a cold piece of glass held over the crucible immediately upon removing the
burner. When no fog appears the soap is considered dry. Any lumps of soap may be
broken up by a small glass rod, weighed with the crucible, and with a roughened end to
more easily separate the lumps. Should the soap burn, this can readily be detected by the
odor, which, of course, renders the analysis useless. The loss in weight is moisture. [Pg 139]

By Fahrion's method[13], 2 to 4 grams of soap are weighed in a platinum crucible and

about three times its weight of oleic acid, which has been heated at 120 degrees C. until
all the water is driven off and preserved from moisture, is added and reweighed. The dish
is then cautiously heated with a small flame until all the water is driven off and all the
soap is dissolved. Care must be exercised not to heat too highly or the oleic acid will
decompose. The moment the water is all driven off a clear solution is formed, provided
no fillers are present in the soap. The dish is then cooled in a dessicator and reweighed.
The loss in weight of acid plus soap is moisture and is calculated on the weight of soap
taken. This determination takes about fifteen minutes.

FREE ALKALI OR ACID.

(a) Alcoholic Method.

Test a freshly cut surface of the soap with a few drops of an alcoholic phenolphthalein
solution. If it does not turn red it may be assumed free fat is present; should a red color
appear, free alkali is present. In any case dissolve 2 to 5 grams of soap in 100 cubic
centimeters of neutralized alcohol and heat to boiling until in solution. Filter off the
undissolved portion containing carbonate, etc., and wash with alcohol. Add
phenolphthalein to the filtrate and titrate with N/10 acid and calculate the per cent. of free
alkali as sodium or potassium hydroxide. Should the filtrate be acid instead of alkaline,
titrate with N/10 alkali and calculate the percentage of free fatty acid as oleic acid.
The insoluble portion remaining on the filter paper is washed with water until all the
carbonate is dissolved. The washings are then titrated with N/10 sulfuric acid and [Pg 140]
expressed as sodium or potassium carbonate. Should borates or silicates be present it is
possible to express in terms of these. If borax is present the carbon dioxide is boiled off
after neutralizing exactly to methyl orange; cool, add mannite and phenolphthalein and
titrate the boric acid with standard alkali.

(b) Bosshard and Huggenberg Method.[14]

In using the alcoholic method for the determination of the free alkali or fat in soap there
is a possibility of both free fat and free alkali being present. Upon boiling in an alcoholic
solution the fat will be saponified, thus introducing an error in the analysis. The method

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of Bosshard and Huggenberg overcomes this objection. Their method is briefly as

follows:

Reagents.

1. N/10 hydrochloric acid to standardize N/10 alcoholic sodium hydroxide.

2. Approximately N/10 alcoholic sodium hydroxide to fix and control the N/40 stearic
acid.
3. N/40 stearic acid. Preparation: About 7.1 grams of stearic acid are dissolved in one
liter of absolute alcohol, the solution filtered, the strength determined by titration against
N/10 NaOH and then protected in a well stoppered bottle, or better still connected
directly to the burette.
4. A 10 per cent. solution of barium chloride. Preparation: 100 grams of barium chloride
are dissolved in one liter of distilled water and filtered. The neutrality of the solution
should be proven as it must be neutral.
5. α naphtholphthalein indicator according to Sorenson. Preparation: 0.1 gram of α
naphtholphthalein is dissolved in 150 cubic centimeters of alcohol and 100 cubic [Pg 141]
centimeters of water. For every 10 cubic centimeters of liquid use at least 12 drops of
indicator.
6. Phenolphthalein solution 1 gram to 100 cubic centimeter 96 per cent. alcohol.
7. Solvent, 50 per cent. alcohol neutralized.

MANIPULATION.

First—Determine the strength of the N/10 alcoholic sodium hydroxide in terms of N/10
hydrochloric acid and calculate the factor, e. g.:

10 c.c. N/10 alcoholic NaOH = 9.95 N/10 HCl}

9.96
10 c.c. N/10 alcoholic NaOH = 9.96 N/10 HCl}

The alcoholic N/10 NaOH has a factor of 0.996.

Second—Control the N/40 stearic acid with the above alkali to obtain its factor, e. g.:

40 c.c. N/40 alcoholic stearic acid = 10.18 c.c. N/10 NaOH }

} 10.2
40 c.c. N/40 alcoholic stearic acid = 10.22 c.c. N/10 NaOH }

10.2 × F N/10 NaOH (0.996) = Factor N/40 stearic acid

∴Factor N/40 stearic acid = 1.016.
Third—About 5 grams of soap are weighed and dissolved in 100 cubic centimeters of 50
per cent. neutralized alcohol in a 250 cubic centimeter Erlenmeyer flask over a water
bath and connected with a reflux condensor. When completely dissolved, which takes but
a few moments, it is cooled by allowing a stream of running water to run over the outside
of the flask.
Fourth—The soap is precipitated with 15 to 20 cubic centimeters of the 10 per cent.
barium chloride solution.
Fifth—After the addition of 2 to 5 cubic centimeters of α naphtholphthalein solution the
solution is titrated with N/40 alcoholic stearic acid. α naphtholphthalein is red with an
excess of stearic acid. To mark the color changes it is advisable to first run a few blanks [Pg 142]

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until the eye has become accustomed to the change in the indicator in the same way. The
change from green to red can then be carefully observed.
Let us presume 5 grams of soap were taken for the analysis and 20 cubic centimeters of
N/40 stearic acid were required for the titration then to calculate the amount of NaOH
since the stearic factor is 1.016.
20 × 1.016 = 20.32 N/40 stearic acid really required.
1 cubic centimeter N/40 stearic acid = 0.02 per cent. NaOH for 5 grams soap.
Δ 20.32 cubic centimeters N/40 stearic acid = 0.02 × 20.32 per cent. NaOH for 5 grams
soap.
Hence the soap contains 0.4064 per cent. NaOH.
It is necessary, however, to make a correction by this method. When the free alkali
amounts to over 0.1 per cent. the correction is + 0.01, and when the free alkali exceeds
0.4 per cent. the correction is + 0.04, hence in the above case we multiply 0.004064 by
0.04, add this amount to 0.004064 and multiply by 100 to obtain the true percentage.
Should the alkalinity have been near 0.1 per cent. we would have multiplied by 0.01 and
added this.
If carbonate is also present in the soap, another 5 grams of soap is dissolved in 100 cubic
centimeters of 50 per cent. alcohol and the solution titrated directly after cooling with
N/40 stearic acid, using α naphtholphthalein or phenolphthalein as an indicator, without
the addition of barium chloride. From the difference of the two titrations the alkali
present as carbonate is determined.
If the decomposed soap solution is colorless with phenolphthalein, free fatty acids are
present, which may be quickly determined with alcoholic N/10 sodium hydroxide. [Pg 143]

INSOLUBLE MATTER.
The insoluble matter in soap may consist of organic or inorganic substances. Among the
organic substances which are usually present in soap are oat meal, bran, sawdust, etc.,
while among the common inorganic or mineral compounds are pumice, silex, clay, talc,
zinc oxide, infusorial earth, sand or other material used as fillers.
To determine insoluble matter, 5 grams of soap are dissolved in 75 cubic centimeters of
hot water. The solution is filtered through a weighed gooch crucible or filter paper. The
residue remaining on the filter is washed with hot water until all the soap is removed, is
then dried to constant weight at 105 degrees C. and weighed. From the difference in
weight of the gooch or filter paper and the dried residue remaining thereon after filtering
and drying, the total percentage of insoluble matter may easily be calculated. By igniting
the residue and reweighing the amount of insoluble mineral matter can be readily
determined.

STARCH AND GELATINE.

Should starch or gelatine be present in soap it is necessary to extract 5 grams of the soap
with 100 cubic centimeters of 95 per cent. neutralized alcohol in a Soxhlet extractor until
the residue on the extraction thimble is in a powder form. If necessary the apparatus
should be disconnected and any lumps crushed, as these may contain soap. The residue
remaining on the thimble consists of all substances present in soap, insoluble in alcohol.
This is dried and weighed so that any percentage of impurities not actually determined
can be found by difference. Starch and gelatine are separated from carbonate, sulfate and
borate by dissolving the latter out through a filter with cold water. The starch and gelatine
thus remaining can be determined by known methods, starch by the method of direct [Pg 144]

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hydrolysis[15] and gelatine by Kjeldahling and calculating the corresponding amount of

gelatine from the percentage of nitrogen (17.9%) therein.[16]

TOTAL FATTY AND RESIN ACIDS.

To the filtrate from the insoluble matter add 40 cubic centimeters of half normal sulfuric
acid, all the acid being added at once. Boil, stir thoroughly for some minutes and keep
warm on a water bath until the fatty acids have collected as a clear layer on the surface.
Cool by placing the beaker in ice and syphon off the acid water through a filter. Should
the fatty acids not readily congeal a weighed amount of dried bleached bees-wax or
stearic acid may be added to the hot mixture. This fuses with the hot mass and forms a
firm cake of fatty acids upon cooling. Without removing the fatty acids from the beaker,
add about 300 cubic centimeters of hot water, cool, syphon off the water through the
same filter used before and wash again. Repeat washing, cooling and syphoning
processes until the wash water is no longer acid. When this stage is reached, dissolve any
fatty acid which may have remained on the filter with hot 95 per cent. alcohol into the
beaker containing the fatty acids. Evaporate the alcohol and dry the beaker to constant
weight over a water bath. The fatty acids thus obtained represent the combined fatty
acids, uncombined fat and hydrocarbons.

DETERMINATION OF ROSIN.

If resin acids are present, this may be determined by the Liebermann-Storch reaction. To
carry out this test shake 2 cubic centimeters of the fatty acids with 5 cubic centimeters of [Pg 145]
acetic anhydride; warm slightly; cool; draw off the anhydride and add 1:1 sulfuric acid. A
violet color, which is not permanent, indicates the presence of rosin in the soap. The
cholesterol in linseed or fish oil, which of course may be present in the soap, also give
this reaction.
Should resin acids be present, these may be separated by the Twitchell method, which
depends upon the difference in the behavior of the fatty and resin acids when converted
into their ethyl esters through the action of hydrochloric acid. This may be carried out as
follows:
Three grams of the dried mixed acids are dissolved in 25 cubic centimeters of absolute
alcohol in a 100 cubic centimeter stoppered flask; the flask placed in cold water and
shaken. To this cooled solution 25 cubic centimeters of absolute alcohol saturated with
dry hydrochloric acid is added. The flask is shaken occasionally and the action allowed to
continue for twenty minutes, then 10 grams of dry granular zinc chloride are added, the
flask shaken and again allowed to stand for twenty minutes. The contents of the flask are
then poured into 200 cubic centimeters of water in a 500 cubic centimeter beaker and the
flask rinsed out with alcohol. A small strip of zinc is placed in the beaker and the alcohol
evaporated. The beaker is then cooled and transferred to a separatory funnel, washing out
the beaker with 50 cubic centimeters of gasoline (boiling below 80 degrees C.) and
extracting by shaking the funnel well. Draw off the acid solution after allowing to
separate and wash the gasoline with water until free from hydrochloric acid. Draw off the
gasoline solution and evaporate the gasoline. Dissolve the residue in neutral alcohol and
titrate with standard alkali using phenolphthalein as an indicator. One cubic centimeter of
normal alkali equals 0.346 grams of rosin. The rosin may be gravimetrically determined [Pg 146]
by washing the gasoline extract with water, it not being necessary to wash absolutely free
from acid, then adding 0.5 gram of potassium hydroxide and 5 cubic centimeters of
alcohol in 50 cubic centimeters of water. Upon shaking the resin acids are rapidly
saponified and extracted by the dilute alkaline solution as rosin soaps, while the ethyl
esters remain in solution in the gasoline. Draw off the soap solution, wash the gasoline
solution again with dilute alkali and unite the alkaline solutions. Decompose the alkaline
soap solution with an excess of hydrochloric acid and weigh the resin acids liberated as
in the determination of total fatty acids.

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According to Lewkowitsch, the results obtained by the volumetric method which

assumes a combining weight of 346 for resin acids, are very likely to be high. On the
other hand those obtained by the gravimetric method are too low.

Leiste and Stiepel[17] have devised a simpler method for the determination of rosin. They
make use of the fact that the resin acids as sodium soaps are soluble in acetone and
particularly acetone containing two per cent. water, while the fatty acid soaps are soluble
in this solvent to the extent of only about 2 per cent. First of all it is necessary to show
that the sample to be analyzed contains a mixture of resin and fatty acids. This may be
done by the Liebermann-Storch reaction already described. Glycerine interferes with the
method. Two grams of fatty acids or 3 grams of soap are weighed in a nickel crucible and
dissolved in 15-20 cubic centimeters of alcohol. The solution is then neutralized with
alcoholic sodium hydroxide, using phenolphthalein as an indicator. The mass is
concentrated by heat over an asbestos plate until a slight film forms over it. Then about [Pg 147]
10 grams of sharp, granular, ignited sand are stirred in by means of a spatula, the alcohol
further evaporated, the mixture being constantly stirred and then thoroughly dried in a
drying oven. The solvent for the cooled mass is acetone containing 2 per cent. water. It is
obtained from acetone dried by ignited sodium sulfate and adding 2 per cent. water by
volume. One hundred cubic centimeters of this solvent are sufficient for extracting the
above. The extraction of the rosin soap is conducted by adding 10 cubic centimeters of
acetone eight times, rubbing the mass thoroughly with a spatula and decanting. The
decanted portions are combined in a beaker and the suspended fatty soaps allowed to
separate. The mixture is then filtered into a previously weighed flask and washed several
times with the acetone remaining. The solution of rosin soap should show no separation
of solid matter after having evaporated to half the volume and allowing to cool. If a
separation should occur another filtration and the slightest possible washing is necessary.
To complete the analysis, the acetone is completely evaporated and the mass dried to
constant weight in a drying oven. The weight found gives the weight of the rosin soap. In
conducting the determination, it is important to dry the mixture of soap and sand
thoroughly. In dealing with potash soaps it is necessary to separate the fatty acids from
these and use them as acetone dissolves too great a quantity of a potash soap.

TOTAL ALKALI.

In the filtrate remaining after having washed the fatty acids in the determination of total
fatty and resin acids all the alkali present as soap, as carbonate and as hydroxide remains
in solution as sulfate. Upon titrating this solution with half normal alkali the difference
between the half normal acid used in decomposing the soap and alkali used in titrating [Pg 148]
the excess of acid gives the amount of total alkali in the soap. By deducting the amount
of free alkali present as carbonate or hydroxide previously found the amount of combined
alkali in the soap may be calculated.
To quickly determine total alkali in soap a weighed portion of the soap may be ignited to
a white ash and the ash titrated for alkalinity using methyl orange as an indicator.

UNSAPONIFIED MATTER.

Dissolve 5 grams of soap in 50 cubic centimeters of 50 per cent. alcohol. Should any free
fatty acids be present neutralize them with standard alkali. Wash into a separatory funnel
with 50 per cent. alcohol and extract with 100 cubic centimeters of gasoline, boiling at 50
degrees to 60 degrees C. Wash the gasoline with water, draw off the watery layer. Run the
gasoline into a weighed dish, evaporate the alcohol, dry and weigh the residue as
unsaponified matter. The residue contains any hydrocarbon oils or fats not converted into
soap.

SILICA AND SILICATES.

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The insoluble silicates, sand, etc., are present in the ignited residue in the determination
of insoluble matter. Sodium silicate, extensively used as a filler, however, will only show
itself in forming a pasty liquid. Where it is desired to determine sodium silicate, 10 grams
of soap are ashed by ignition, hydrochloric acid added to the ash in excess and
evaporated to dryness. More hydrochloric acid is then added and the mass is again
evaporated until dry; then cooled; moistened with hydrochloric acid; dissolved in water;
filtered; washed; the filtrate evaporated to dryness and again taken up with hydrochloric
acid and water; filtered and washed. The precipitates are then combined and ignited. [Pg 149]
Silicon dioxide (SiO2) is thus formed, which can be calculated to sodium silicate
(Na2Si4O9). Should other metals than alkali metals be suspected present the filtrate from
the silica determinations should be examined.

GLYCERINE IN SOAP.

To determine the amount of glycerine contained in soap dissolve 25 grams in hot water,
add a slight excess of sulfuric acid and keep hot until the fatty acids form as a clear layer
on top. Cool the mass and remove the fatty acids. Filter the acid solution into a 25 cubic
centimeter graduated flask; bring to the mark with water and determine the glycerine by
the bichromate method as described under glycerine analysis.
When sugar is present the bichromate would be reduced by the sugar, hence this method
is not applicable. In this case remove the fatty acids as before, neutralize an aliquot
portion with milk of lime, evaporate to 10 cubic centimeters, add 2 grams of sand and
milk of lime containing about 2 grams of calcium hydroxide and evaporate almost to
dryness. Treat the moist residue with 5 cubic centimeters of 96 per cent. alcohol, rub the
whole mass into a paste, then constantly stirring, heat on a water bath and decant into a
250 cubic centimeter graduated flask. Repeat the washing with 5 cubic centimeters of
alcohol five or six times, each time pouring the washings into the flask; cool the flask to
room temperature and fill to the mark with 96 per cent. alcohol, agitate the flask until
well mixed and filter through a dry filter paper. Take 200 cubic centimeters of the nitrate
and evaporate to a syrupy consistency over a safety water bath. Wash the liquor into a
stoppered flask with 20 cubic centimeters of absolute alcohol, add 30 cubic centimeters
of absolute ether 10 cubic centimeters at a time, shaking well after each addition and let [Pg 150]
stand until clear. Pour off the solution through a filter into a weighed dish and wash out
the flask with a mixture of three parts absolute ether and two parts absolute alcohol.
Evaporate to a syrup, dry for one hour at the temperature of boiling water, weigh, ignite
and weigh again. The loss is glycerine. This multiplied by 5/4 gives the total loss for the
aliquot portion taken. The glycerine may also be determined by the acetin or bichromate
methods after driving off the alcohol and ether if so desired.

SUGAR IN SOAP.
To determine sugar in soap, usually present in transparent soaps, decompose a soap
solution of 5 grams of soap dissolved in 100 cubic centimeters of hot water with an
excess of hydrochloric acid and separate the fatty acids as usual. Filter the acid solution
into a graduated flask and make up to the mark. Take an aliquot containing approximately
1 per cent. of reducing sugar and determine the amount of sugar by the Soxhlet method.
[18]

GLYCERINE ANALYSIS.

The methods of analyzing glycerine varied so greatly due to the fact that glycerine
contained impurities which acted so much like glycerine as to introduce serious errors in
the determinations of crude glycerine. This led to the appointment of committees in the
United States and Europe to investigate the methods of glycerine analysis. An
international committee met after their investigations and decided the acetin method

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should control the buying and selling of glycerine, but the more convenient bichromate
method in a standardized form might be used in factory control and other technical [Pg 151]
purposes. The following are the methods of analysis and sampling as suggested by the
international committee:

SAMPLING.
The most satisfactory method available for sampling crude glycerine liable to contain
suspended matter, or which is liable to deposit salt on settling, is to have the glycerine
sampled by a mutually approved sampler as soon as possible after it is filled into drums,
but in any case before any separation of salt has taken place. In such cases he shall
sample with a sectional sampler (see appendix) then seal the drums, brand them with a
number for identification, and keep a record of the brand number. The presence of any
visible salt or other suspended matter is to be noted by the sampler, and a report of the
same made in his certificate, together with the temperature of the glycerine. Each drum
must be sampled. Glycerine which has deposited salt or other solid matter cannot be
accurately sampled from the drums, but an approximate sample can be obtained by
means of the sectional sampler, which will allow a complete vertical section of the
glycerine to be taken including any deposit.

ANALYSIS.

1. Determination of Free Caustic Alkali.—Put 20 grams of the sample into a 100 cc.
flask, dilute with approximately 50 cc. of freshly boiled distilled water, add an excess of
neutral barium chloride solution, 1 cc. of phenolphthalein solution, make up to the mark
and mix. Allow the precipitate to settle, draw off 50 cc. of the clear liquid and titrate with
normal acid (N/1). Calculate the percentage of Na2O existing as caustic alkali.

2. Determination of Ash and Total Alkalinity.—Weigh 2 to 5 grams of the sample in a [Pg 152]
platinum dish, burn off the glycerine over a luminous Argand burner or other source of
heat,[19] giving a low temperature, to avoid volatilization and the formation of sulphides.
When the mass is charred to the point that water will not be colored by soluble organic
matter, lixiviate with hot distilled water, filter, wash and ignite the residue in the platinum
dish. Return the filtrate and washings to the dish, evaporate the water, and carefully ignite
without fusion. Weigh the ash.
Dissolve the ash in distilled water and titrate total alkalinity, using as indicator methyl
orange cold or litmus boiling.
3. Determination of Alkali Present as Carbonate.—Take 10 grams of the sample, dilute
with 50 cc. distilled water, add sufficient N/1 acid to neutralize the total alkali found at
(2), boil under a reflux condenser for 15 to 20 minutes, wash down the condenser tube
with distilled water, free from carbon dioxide, and then titrate back with N/1 NaOH,
using phenolphthalein as indicator. Calculate the percentage of Na2O. Deduct the Na2O
found in (1). The difference is the percentage of Na2O existing as carbonate.

4. Alkali Combined with Organic Acids.—The sum of the percentages of Na2O found at
(1) and (3) deducted from the percentage found at (2) is a measure of the Na2O or other
alkali combined with organic acids.
5. Determination of Acidity.—Take 10 grams of the sample, dilute with 50 cc. distilled
water free from carbon dioxide, and titrate with N/1 NaOH and phenolphthalein. Express
in terms of Na2O required to neutralize 100 grams.

6. Determination of Total Residue at 160° C.—For this determination the crude glycerine
should be slightly alkaline with Na2CO3 not exceeding 0.2 per cent. Na2O, in order to [Pg 153]

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prevent loss of organic acids. To avoid the formation of polyglycerols this alkalinity must
not be exceeded.
Ten grams of the sample are put into a 100 cc. flask, diluted with water and the calculated
quantity of N/1 HCl or Na2CO3 added to give the required degree of alkalinity. The flask
is filled to 100 cc., the contents mixed, and 10 cc. measured into a weighed Petrie or
similar dish 2.5 in. in diameter and 0.5 in. deep, which should have a flat bottom. In the
case of crude glycerine abnormally high in organic residue a smaller amount should be
taken, so that the weight of the organic residue does not materially exceed 30 to 40
milligrams.
The dish is placed on a water bath (the top of the 160° oven acts equally well) until most
of the water has evaporated. From this point the evaporation is effected in the oven.
Satisfactory results are obtained in an oven[20] measuring 12 ins. cube, having an iron
plate 0.75 in. thick lying on the bottom to distribute the heat. Strips of asbestos millboard
are placed on a shelf half way up the oven. On these strips the dish containing the
glycerine is placed.
If the temperature of the oven has been adjusted to 160° C. with the door closed, a
temperature of 130° to 140° can be readily maintained with the door partially open, and
the glycerine, or most of it, should be evaporated off at this temperature. When only a
slight vapor is seen to come off, the dish is removed and allowed to cool.
An addition of 0.5 to 1.0 cc. of water is made, and by a rotary motion the residue brought [Pg 154]
wholly or nearly into solution. The dish is then allowed to remain on a water bath or top
of the oven until the excess water has evaporated and the residue is in such a condition
that on returning to the oven at 160° C. it will not spurt. The time taken up to this point
cannot be given definitely, nor is it important. Usually two or three hours are required.
From this point, however, the schedule of time must be strictly adhered to. The dish is
allowed to remain in the oven, the temperature of which is carefully maintained at 160°
C. for one hour, when it is removed, cooled, the residue treated with water, and the water
evaporated as before. The residue is then subjected to a second baking of one hour, after
which the dish is allowed to cool in a desiccator over sulphuric acid and weighed. The
treatment with water, etc., is repeated until a constant loss of 1 to 1.5 mg. per hour is
obtained.
In the case of acid glycerine a correction must be made for the alkali added 1 cc. N/1
alkali represents an addition of 0.03 gram. In the case of alkaline crudes a correction
should be made for the acid added. Deduct the increase in weight due to the conversion
of the NaOH and Na2CO3 to NaCl. The corrected weight multiplied by 100 gives the
percentage of total residue at 160° C.
This residue is taken for the determination of the non-volatile acetylizable impurities (see
acetin method).
7. Organic residue.—Subtract the ash from the total residue at 160° C. Report as organic
residue at 160° C. (it should be noted that alkaline salts of fatty acids are converted to
carbonates on ignition and that the CO3 thus derived is not included in the organic
residue). [Pg 155]

ACETIN PROCESS FOR THE DETERMINATION OF GLYCEROL.

This process is the one agreed upon at a conference of delegates from the British, French,
German and American committees, and has been confirmed by each of the above
committees as giving results nearer to the truth than the bichromate method on crudes in
general. It is the process to be used (if applicable) whenever only one method is
employed. On pure glycerines the results are identical with those obtained by the
bichromate process. For the application of this method the crude glycerine should not
contain over 60 per cent. water.
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REAGENTS REQUIRED.

(A) Best Acetic Anhydride.—This should be carefully selected. A good sample must not
require more than 0.1 cc. normal NaOH for saponification of the impurities when a blank
is run on 7.5 cc. Only a slight color should develop during digestion of the blank.
The anhydride may be tested for strength by the following method: Into a weighed
stoppered vessel, containing 10 to 20 cc. of water, run about 2 cc. of the anhydride,
replace the stopper and weigh. Let stand with occasional shaking, for several hours, to
permit the hydrolysis of all the anhydride; then dilute to about 200 cc., add
phenolphthalein and titrate with N/1 NaOH. This gives the total acidity due to free acetic
acid and acid formed from the anhydride. It is worthy of note that in the presence of
much free anhydride a compound is formed with phenolphthalein, soluble in alkali and
acetic acid, but insoluble in neutral solutions. If a turbidity is noticed toward the end of
the neutralization it is an indication that the anhydride is incompletely hydrolyzed and
inasmuch as the indicator is withdrawn from the solution, results may be incorrect. [Pg 156]

Into a stoppered weighing bottle containing a known weight of recently distilled aniline
(from 10 to 20 cc.) measure about 2 cc. of the sample, stopper, mix, cool and weigh.
Wash the contents into about 200 cc. of cold water, and titrate the acidity as before. This
yields the acidity due to the original, preformed, acetic acid plus one-half the acid due to
anhydride (the other half having formed acetanilide); subtract the second result from the
first (both calculated to 100 grams) and double the result, obtaining the cc. N/1 NaOH per
100 grams of the sample. 1 cc. N/NaOH equals 0.0510 anhydride.
(B) Pure Fused Sodium Acetate.—The purchased salt is again completely fused in a
platinum, silica or nickel dish, avoiding charring, powdered quickly and kept in a
stoppered bottle or desiccator. It is most important that the sodium acetate be anhydrous.
(C) A Solution of Caustic Soda for Neutralizing, of about N/1 Strength, Free from
Carbonate.—This can be readily made by dissolving pure sodium hydroxide in its own
weight of water (preferably water free from carbon dioxide) and allowing to settle until
clear, or filtering through an asbestos or paper filter. The clear solution is diluted with
water free from carbon dioxide to the strength required.
(D) N/1 Caustic Soda Free from Carbonate.—Prepared as above and carefully
standardized. Some caustic soda solutions show a marked diminution in strength after
being boiled; such solutions should be rejected.
(E) N/1 Acid.—Carefully standardized.
(F) Phenolphthalein Solution.—0.5 per cent. phenolphthalein in alcohol and neutralized.

THE METHOD.

In a narrow-mouthed flask (preferably round-bottomed), capacity about 120 cc., which [Pg 157]
has been thoroughly cleaned and dried, weigh accurately and as rapidly as possible 1.25
to 1.5 grams of the glycerine. A Grethan or Lunge pipette will be found convenient. Add
about 3 grams of the anhydrous sodium acetate, then 7.5 cc. of the acetic anhydride, and
connect the flask with an upright Liebig condenser. For convenience the inner tube of this
condenser should not be over 50 cm. long and 9 to 10 mm. inside diameter. The flask is
connected to the condenser by either a ground glass joint (preferably) or a rubber stopper.
If a rubber stopper is used it should have had a preliminary treatment with hot acetic
anhydride vapor.
Heat the contents and keep just boiling for one hour, taking precautions to prevent the
salts drying on the sides of the flask.
Allow the flask to cool somewhat, and through the condenser tube add 50 cc. of distilled
water free from carbon dioxide at a temperature of about 80° C., taking care that the flask
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is not loosened from the condenser. The object of cooling is to avoid any sudden rush of
vapors from the flask on adding water, and to avoid breaking the flask. Time is saved by
adding the water before the contents of the flask solidify, but the contents may be allowed
to solidify and the test proceeded with the next day without detriment, bearing in mind
that the anhydride in excess is much more effectively hydrolyzed in hot than in cold
water. The contents of the flask may be warmed to, but must not exceed, 80° C., until the
solution is complete, except a few dark flocks representing organic impurities in the
crude. By giving the flask a rotary motion, solution is more quickly effected.
Cool the flask and contents without loosening from the condenser. When quite cold wash
down the inside of the condenser tube, detach the flask, wash off the stopper or ground [Pg 158]
glass connection into the flask, and filter the contents through an acid-washed filter into a
Jena glass flask of about 1 litre capacity. Wash thoroughly with cold distilled water free
from carbon dioxide. Add 2 cc. of phenolphthalein solution (F), then run in caustic soda
solution (C) or (D) until a faint pinkish yellow color appears throughout the solution.
This neutralization must be done most carefully; the alkali should be run down the sides
of the flask, the contents of which are kept rapidly swirling with occasional agitation or
change of motion until the solution is nearly neutralized, as indicated by the slower
disappearance of the color developed locally by the alkali running into the mixture. When
this point is reached the sides of the flask are washed down with carbon dioxide-free
water and the alkali subsequently added drop by drop, mixing after each drop until the
desired tint is obtained.
Now run in from a burette 50 cc. or a calculated excess of N/1 NaOH (D) and note
carefully the exact amount. Boil gently for 15 minutes, the flask being fitted with a glass
tube acting as a partial condenser. Cool as quickly as possible and titrate the excess of
NaOH with N/1 acid (E) until the pinkish yellow or chosen end-point color just remains.
[21] A further addition of the indicator at this point will cause an increase of the pink
color; this must be neglected, and the first end-point taken.
From the N/1 NaOH consumed calculate the percentage of glycerol (including
acetylizable impurities) after making the correction for the blank test described below.
1 cc. N/1 NaOH = 0.03069 gram glycerol.
The coefficient of expansion for normal solutions is 0.00033 per cc. for each degree [Pg 159]
centigrade. A correction should be made on this account if necessary.
Blank Test.—As the acetic anhydride and sodium acetate may contain impurities which
affect the result, it is necessary to make a blank test, using the same quantities of acetic
anhydride, sodium acetate and water as in the analysis. It is not necessary to filter the
solution of the melt in this case, but sufficient time must be allowed for the hydrolysis of
the anhydride before proceeding with the neutralization. After neutralization it is not
necessary to add more than 10 cc. of the N/1 alkali (D), as this represents the excess
usually present after the saponification of the average soap lye crude. In determining the
acid equivalent of the N/1 NaOH, however, the entire amount taken in the analysis, 50
cc., should be titrated after dilution with 300 cc. water free from carbon dioxide and
without boiling.
Determination of the Glycerol Value of the Acetylizable Impurities.—The total residue at
160° C. is dissolved in 1 or 2 cc. of water, washed into the acetylizing flask and
evaporated to dryness. Then add anhydrous sodium acetate and acetic anhydride in the
usual amounts and proceed as described in the regular analysis. After correcting for the
blank, calculate the result to glycerol.

WAYS OF CALCULATING ACTUAL GLYCEROL CONTENT.

(1) Determine the apparent percentage of glycerol in the sample by the acetin process as
described. The result will include acetylizable impurities if any are present.

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(2) Determine the total residue at 160° C.

(3) Determine the acetin value of the residue at (2) in terms of glycerol.
(4) Deduct the result found at (3) from the percentage obtained at (1) and report this
corrected figure as glycerol. If volatile acetylizable impurities are present these are [Pg 160]
included in this figure.
Trimethyleneglycol is more volatile than glycerine and can therefore be concentrated by
fractional distillation. An approximation to the quantity can be obtained from the spread
between the acetin and bichromate results on such distillates. The spread multiplied by
1.736 will give the glycol.

BICHROMATE PROCESS FOR GLYCEROL DETERMINATION.

REAGENTS REQUIRED.
(A) Pure potassium bichromate powdered and dried in air free from dust or organic
vapors, at 110° to 120° C. This is taken as the standard.
(B) Dilute Bichromate Solution.—7.4564 grams of the above bichromate are dissolved in
distilled water and the solution made up to one liter at 15.5° C.
(C) Ferrous Ammonium Sulphate.—It is never safe to assume this salt to be constant in
composition and it must be standardized against the bichromate as follows: dissolve
3.7282 grams of bichromate (A) in 50 cc. of water. Add 50 cc. of 50 per cent. sulphuric
acid (by volume), and to the cold undiluted solution add from a weighing bottle a
moderate excess of the ferrous ammonium sulphate, and titrate back with the dilute
bichromate (B). Calculate the value of the ferrous salt in terms of bichromate.
(D) Silver Carbonate.—This is prepared as required for each test from 140 cc. of 0.5 per
cent. silver sulphate solution by precipitation, with about 4.9 cc. N/1 sodium carbonate
solution (a little less than the calculated quantity of N/1 sodium carbonate should be used
as an excess to prevent rapid settling). Settle, decant and wash one by decantation.
(E) Subacetate of Lead.—Boil a 10 per cent. solution of pure lead acetate with an excess [Pg 161]
of litharge for one hour, keeping the volume constant, and filter while hot. Disregard any
precipitate which subsequently forms. Preserve out of contact with carbon dioxide.
(F) Potassium Ferricyanide.—A very dilute, freshly prepared solution containing about
0.1 per cent.

THE METHOD.

Weigh 20 grams of the glycerine, dilute to 250 cc. and take 25 cc. Add the silver
carbonate, allow to stand, with occasional agitation, for about 10 minutes, and add a
slight excess (about 5 cc. in most cases) of the basic lead acetate (E), allow to stand a few
minutes, dilute with distilled water to 100 cc., and then add 0.15 cc. to compensate for
the volume of the precipitate, mix thoroughly, filter through an air-dry filter into a
suitable narrow-mouthed vessel, rejecting the first 10 cc., and return the filtrate if not
clear and bright. Test a portion of the filtrate with a little basic lead acetate, which should
produce no further precipitate (in the great majority of cases 5 cc. are ample, but
occasionally a crude will be found requiring more, and in this case another aliquot of 25
cc. of the dilute glycerine should be taken and purified with 6 cc. of the basic acetate).
Care must be taken to avoid a marked excess of basic acetate.
Measure off 25 cc. of the clear filtrate into a flask or beaker (previously cleaned with
potassium bichromate and sulphuric acid). Add 12 drops of sulphuric acid (1: 4) to
precipitate the small excess of lead as sulphate. Add 3.7282 grams of the powdered
potassium bichromate (A). Rinse down the bichromate with 25 cc. of water and let stand

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with occasional shaking until all the bichromate is dissolved (no reduction will take place
in the cold).
Now add 50 cc. of 50 per cent. sulphuric acid (by volume) and immerse the vessel in [Pg 162]
boiling water for two hours and keep protected from dust and organic vapors, such as
alcohol, till the titration is completed. Add from a weighing bottle a slight excess of the
ferrous ammonium sulphate (C), making spot tests on a porcelain plate with the
potassium ferricyanide (F). Titrate back with the dilute bichromate. From the amount of
bichromate reduced calculate the percentage of glycerol.
1 gram glycerol = 7.4564 grams bichromate.
1 gram bichromate = 0.13411 gram glycerol.
The percentage of glycerol obtained above includes any oxidizable impurities present
after the purification. A correction for the non-volatile impurities may be made by
running a bichromate test on the residue at 160° C.

NOTES.
(1) It is important that the concentration of acid in the oxidation mixture and the time of
oxidation should be strictly adhered to.
(2) Before the bichromate is added to the glycerine solution it is essential that the slight
excess of lead be precipitated with sulphuric acid, as stipulated.
(3) For crudes practically free from chlorides the quantity of silver carbonate may be
reduced to one-fifth and the basic lead acetate to 0.5 cc.
(4) It is sometimes advisable to add a little potassium sulphate to insure a clear filtrate.

SAMPLING CRUDE GLYCERINE.

The usual method of sampling crude glycerine hitherto has been by means of a glass
tube, which is slowly lowered into the drum with the object of taking as nearly as
possible a vertical section of the glycerine contained in the drum. This method has been [Pg 163]
found unsatisfactory, owing to the fact that in cold climates glycerine runs into the tube
very slowly, so that, owing to the time occupied, it is impossible to take a complete
section of the crude. Another objection to the glass tube is that it fails to take anything
approaching a correct proportion of any settled salt contained in the drum.
The sampler which is illustrated herewith has been devised with the object of overcoming
the objections to the glass tube as far as possible. It consists of two brass tubes, one
fitting closely inside the other. A number of ports are cut out in each tube in such a way
that when the ports are opened a continuous slot is formed which enables a complete
section to be taken throughout the entire length of the drum. By this arrangement the
glycerine fills into the sampler almost instantaneously. There are a number of ports cut at
the bottom of the sampler which render it possible to take a proportion of the salt at the
bottom of the drum. The instrument is so constructed that all the ports, including the
bottom ones, can be closed simultaneously by the simple action of turning the handle at
the top; a pointer is arranged which indicates on a dial when the sampler is open or
closed. In samplers of larger section (1 in.) it is possible to arrange a third motion
whereby the bottom ports only are open for emptying, but in samplers of smaller
dimensions (5/8 in.) this third motion must be dispensed with, otherwise the dimensions
of the ports have to be so small that the sampler would not be efficient.
In using the sampler it is introduced into the drum with the ports closed, and when it has
touched the bottom, the ports are opened for a second or two, then closed and withdrawn,
and the sample discharged into the receiving vessel by opening the ports. When the drum
contains salt which has deposited, the ports must be opened before the sampler is pushed [Pg 164]
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through the salt, thus enabling a portion to be included in the sample. It is, however,
almost impossible to obtain a correct proportion of salt after it has settled in the drum and
it is therefore recommended that the drum be sampled before any salt has deposited. A
sampler 1 in. in diameter withdraws approximately 10 oz. from a 110-gal. drum. A
sampler 5/8 in. in diameter will withdraw about 5 oz.

FOOTNOTES:
[13] Zeit. Angew. Chem. 19, 385 (1906).
[14] Zeit. Angew. Chem. 27, 11-20 (1914).
[15] Bull. 107, Bur. Chem. U. S. Dept. Agriculture.
[16] Richards and Gies, Am. J. Physiol. (1902) 7, 129.
[17] Seifensieder Ztg. (1913) No. 46.
[18] Bull 107, Bur. Chem. U. S. Dept. Agriculture.
[19] Carbon is readily burned off completely, without loss of chlorides, in a gas-
heated muffle furnace adjusted to a dull red heat.
[20] An electric oven suitable for this work, which is readily adjusted to 160 degs.
C., has been made for Mr. Low and the chairman, by the Apparatus and
Specialty Company, Lansing, Mich. Its size is 9-1/2 × 10 × 16 inches, and
capacity 8 Petrie dishes. It gives a strong draft at constant temperature.
[21] A precipitate at this point is an indication of the presence of iron or alumina,
and high results will be obtained unless a correction is made as described
below.

CHAPTER VII [Pg 165]

Standard Methods for the Sampling and Analysis of Commercial Fats

and Oils[22]
The following report of the Committee on Analysis of Commercial Fats and Oils of the
Division of Industrial Chemists and Chemical Engineers of the American Chemical
Society was adopted April 14, 1919, by unanimous vote:
W. D. Richardson, Chairman, Swift and Co., Chicago, Ill.
R. W. Bailey, Stillwell and Gladding, New York City.
W. J. Gascoyne, W. J. Gascoyne and Co., Baltimore, Md.
I. Katz,[A] Wilson and Co., Chicago, Ill.
A. Lowenstein,[A] Morris and Co., Chicago, Ill.
H. J. Morrison, Proctor and Gamble Co., Ivorydale, Ohio.
J. R. Powell, Armour Soap Works, Chicago, Ill.
R. J. Quinn,[A] Midland Chemical Co., Argo, Ill.
Paul Rudnick, Armour and Co., Chicago, Ill.

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L. M. Tolman, Wilson and Co., Chicago, Ill.

E. Twitchell,[A] Emery Candle Co., Cincinnati, Ohio.
J. J. Vollertsen, Morris and Co., Chicago, Ill.
[Note A: Resigned.]

Scope, Applicability and Limitations of the Methods.

SCOPE.

These methods are intended to aid in determining the commercial valuation of fats and
fatty oils in their purchase and sale, based on the fundamental assumption commonly
recognized in the trade, namely, that the product is true to name and is not adulterated.
For methods for determining the identity of oils and fats, the absence of adulterants
therein and for specific tests used in particular industries, the chemist is referred to
standard works on the analysis of fats and oils. [Pg 166]

APPLICABILITY.

The methods are applicable in commercial transactions involving fats and fatty oils used
in the soap, candle and tanning industries, to edible fats and oils and to fats and fatty oils
intended for lubricating and burning purposes. The methods are applicable to the raw oils
used in the varnish and paint industry with the exceptions noted under limitations, but
special methods have not been included.

LIMITATIONS.

The methods have not been developed with special reference to waxes (beeswax,
carnauba wax, wool wax, etc.) although some of them may be found applicable to these
substances. The Committee considers the Wijs method superior to the Hanus method for
the determination of iodine number of linseed oil as well as other oils, although the
Hanus method has been considered standard for this work for some time and has been
adopted by the American Society for Testing Materials and in various specifications. It
has been customary to use the Hübl method for the determination of iodine value of tung
oil (China wood oil) but the Committee's work indicates that the Wijs method is
satisfactory for this determination.

Sampling.

TANK CARS.

1. Sampling While Loading—Sample shall be taken at discharge of pipe where it enters

tank car dome. The total sample taken shall be not less than 50 lbs. and shall be a
composite of small samples of about 1 pound each, taken at regular intervals during the
entire period of loading.
The sample thus obtained is thoroughly mixed and uniform 3-lb. portions placed in air-
tight 3-lb. metal containers. At least three such samples shall be put up, one for the buyer,
one for the seller, and the third to be sent to a referee chemist in case of dispute. All [Pg 167]
samples are to be promptly and correctly labeled and sealed.

2. Sampling from Car on Track[23]—(a) When contents are solid.[24] In this case the
sample is taken by means of a large tryer measuring about 2 in. across and about 1-1/2
times the depth of the car in length. Several tryerfuls are taken vertically and obliquely
toward the ends of the car until 50 lbs. are accumulated, when the sample is softened,
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mixed and handled as under (1). In case the contents of the tank car have assumed a very
hard condition, as in Winter weather, so that it is impossible to insert the tryer, and it
becomes necessary to soften the contents of the car by means of the closed steam coil (in
nearly all tank cars the closed steam coil leaks) or by means of open steam in order to
draw a proper sample, suitable arrangements must be made between buyer and seller for
the sampling of the car after it is sufficiently softened, due consideration being given to
the possible presence of water in the material in the car as received and also to the
possible addition of water during the steaming. The Committee knows of no direct
method for sampling a hard-frozen tank car of tallow in a satisfactory manner.
(b) When contents are liquid. The sample taken is to be a 50-lb. composite made up of
numerous small samples taken from the top, bottom and intermediate points by means of
a bottle or metal container with removable stopper or top. This device attached to a
suitable pole is lowered to the various desired depths, when the stopper or top is removed
and the container allowed to fill. The 50-lb. sample thus obtained is handled as under (1). [Pg 168]
In place of the device described above, any sampler capable of taking a sample from the
top, bottom, and center, or from a section through car, may be used.
(c) When contents are in semi-solid condition, or when stearine has separated from liquid
portions. In this case, a combination of (a) and (b) may be used or by agreement of the
parties the whole may be melted and procedure (b) followed.

BARRELS, TIERCES, CASKS, DRUMS, AND OTHER PACKAGES.

All packages shall be sampled, unless by special agreement the parties arrange to sample
a lesser number; but in any case not less than 10 per cent of the total number shall be
sampled. The total sample taken shall be at least 20 lbs. in weight for each 100 barrels, or
equivalent.
1. Barrels, Tierces and Casks—(a) When contents are solid. The small samples shall
be taken by a tryer through the bunghole or through a special hole bored in the head or
side for the purpose, with a 1-in. or larger auger. Care should be taken to avoid and
eliminate all borings and chips from the sample. The tryer is inserted in such a way as to
reach the head of the barrel, tierce, or cask. The large sample is softened, mixed and
handled according to tank cars (1).
(b) When contents are liquid. In this case use is made of a glass tube with constricted
lower end. This is inserted slowly and allowed to fill with the liquid, when the upper end
is closed and the tube withdrawn, the contents being allowed to drain into the sample
container. After the entire sample is taken it is thoroughly mixed and handled according
to tank cars (1).
(c) When contents are semi-solid. In this case the tryer or a glass tube with larger outlet is
used, depending on the degree of fluidity. [Pg 169]

(d) Very hard materials, such as natural and artificial stearines. By preference the barrels
are stripped and samples obtained by breaking up contents of at least 10 per cent of the
packages. This procedure is to be followed also in the case of cakes shipped in sacks.
When shipped in the form of small pieces in sacks they can be sampled by grab sampling
and quartering. In all cases the final procedure is as outlined under tank cars (1).
2. Drums—Samples are to be taken as under (1), use being made of the bunghole. The
tryer or tube should be sufficiently long to reach to the ends of the drum.
3. Other Packages—Tubs, pails and other small packages not mentioned above are to
be sampled by tryer or tube (depending on fluidity) as outlined above, the tryer or tube
being inserted diagonally whenever possible.
4. Mixed Lots and Packages—When lots of tallow or other fats are received in
packages of various shapes and sizes, and especially wherein the fat itself is of variable
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composition, such must be left to the judgment of the sampler. If variable, the contents of
each package should be mixed as thoroughly as possible and the amount of the individual
samples taken made proportional to the sizes of the packages.

Analysis.

SAMPLE.

The sample must be representative and at least three pounds in weight and taken in
accordance with the standard methods for the sampling of commercial fats and
oils. It must be kept in an air-tight container, in a dark, cool place.
Soften the sample if necessary by means of a gentle heat, taking care not to melt it. When
sufficiently softened, mix the sample thoroughly by means of a mechanical egg beater or
other equally effective mechanical mixer. [Pg 170]

MOISTURE AND VOLATILE MATTER.

Apparatus: Vacuum Oven—The Committee Standard Oven.

Description—The Standard F. A. C. Vacuum Oven has been designed with the idea of
affording a simple and compact vacuum oven which will give as uniform temperatures as
possible on the shelf. As the figure shows, it consists of an iron casting of rectangular
sections with hinged front door made tight by means of a gasket and which can be
lowered on opening the oven so as to form a shelf on which samples may be rested. The
oven contains but one shelf which is heated from above as well as below by means of
resistance coils. Several thermometer holes are provided in order to ascertain definitely
the temperature at different points on the shelf. In a vacuum oven where the heating is
done almost entirely by radiation it is difficult to maintain uniform temperatures at all
points, but the F. A. C. oven accomplishes this rather better than most vacuum ovens.
Larger ovens containing more than one shelf have been tried by the Committee, but have
been found to be lacking in temperature uniformity and means of control. The entire oven
is supported by means of a 4-in. standard pipe which screws into the base of the oven and
which in turn is supported by being screwed into a blind flange of suitable diameter
which rests on the floor or work table.
Moisture Dish—A shallow, glass dish, lipped, beaker form, approximately 6 to 7 cm.
diameter and 4 cm. deep, shall be standard.
Determination—Weigh out 5 grams (= 0.2 g. of the prepared sample) into a moisture
dish. Dry to constant weight in vacuo at a uniform temperature, not less than 15° C. nor
more than 20° C. above the boiling point of water at the working pressure, which must
not exceed 100 mm. of mercury.[25] Constant weight is attained when successive dryings
for 1-hr. periods show an additional loss of not more that 0.05 per cent. Report loss in
weight as moisture and volatile matter.[26] [Pg 171]

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Standard Vacuum Oven

The vacuum-oven method cannot be considered accurate in the case of fats of the [Pg 172]
coconut oil group containing free acid and the Committee recommends that it be used
only for oils of this group when they contain less than 1 per cent free acid. In the case of
oils of this group containing more than 1 per cent free acid, recourse should be had
temporarily to the routine control method for moisture and volatile matter[27] until the
Committee develops a more satisfactory method.
The air-oven method cannot be considered even approximately accurate in the case of the
drying and semi-drying oils and those of the coconut oil group. Therefore, in the case of
such oils as cottonseed oil, maize oil (corn oil), soy bean oil, linseed oil, coconut oil,
palm kernel oil, etc., the vacuum-oven method should always be used, except in the case
of fats of the coconut group containing more than 1 per cent free acid, as noted above.

INSOLUBLE IMPURITIES.

Dissolve the residue from the moisture and volatile matter determination by heating it on
a steam bath with 50 cc. of kerosene. Filter the solution through a Gooch crucible
properly prepared with asbestos,[28] wash the insoluble matter five times with 10-cc.
portions of hot kerosene, and finally wash the residual kerosene out thoroughly with
petroleum ether. Dry the crucible and contents to constant weight, as in the determination
of moisture and volatile matter and report results as insoluble impurities. [Pg 173]

SOLUBLE MINERAL MATTER.

Place the combined kerosene filtrate and kerosene washings from the insoluble impurities
determination in a platinum dish. Place in this an ashless filter paper folded in the form of
a cone, apex up. Light the apex of the cone, whereupon the bulk of the kerosene burns
quietly. Ash the residue in a muffle, to constant weight, taking care that the

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decomposition of alkaline earth carbonates is complete, and report the result as soluble
mineral matter.[29] When the percentage of soluble mineral matter amounts to more
than 0.1 per cent, multiply the percentage by 10 and add this amount to the percentage of
free fatty acids as determined.[30] [Pg 174]

FREE FATTY ACIDS.

The alcohol[31] used shall be approximately 95 per cent ethyl alcohol, freshly distilled
from sodium hydroxide, which with phenolphthalein gives a definite and distinct end-
point.
Determination—Weigh 1 to 15 g. of the prepared sample into an Erlenmeyer flask,
using the smaller quantity in the case of dark-colored, high acid fats. Add 50 to 100 cc.
hot, neutral alcohol, and titrate with N/2, N/4 or N/10 sodium hydroxide depending on the
fatty acid content, using phenolphthalein as indicator. Calculate to oleic acid, except that
in the case of palm oil the results may also be expressed in terms of palmitic acid, clearly
indicating the two methods of calculation in the report. In the case of coconut and palm
kernel oils, calculate to and report in terms of lauric acid in addition to oleic acid, clearly
indicating the two methods of calculation in the report. In the case of fats or greases
containing more than 0.1 per cent of soluble mineral matter, add to the percentages of
free fatty acids as determined 10 times the percentage of bases in the soluble mineral
matter as determined.[30] This addition gives the equivalent of fatty acids combined with
the soluble mineral matter. [Pg 175]

TITER.

Standard Thermometer—The thermometer is graduated at zero and in tenth degrees

from 10° C. to 65° C., with one auxiliary reservoir at the upper end and another between
the zero mark and the 10° mark. The cavity in the capillary tube between the zero mark
and the 10° mark is at least 1 cm. below the 10° mark, the 10° mark is about 3 or 4 cm.
above the bulb, the length of the thermometer being about 37 cm. over all. The
thermometer has been annealed for 75 hrs. at 450° C. and the bulb is of Jena normal 16'''
glass, or its equivalent, moderately thin, so that the thermometer will be quick-acting.
The bulb is about 3 cm. long and 6 mm. in diameter. The stem of the thermometer is 6
mm. in diameter and made of the best thermometer tubing, with scale etched on the stem,
the graduation is clear-cut and distinct, but quite fine. The thermometer must be certified
by the U. S. Bureau of Standards.
Glycerol Caustic Solution—Dissolve 250 g. potassium hydroxide in 1900 cc.
dynamite glycerin with the aid of heat.
Determination—Heat 75 cc. of the glycerol-caustic solution to 150° C. and add 50 g. of
the melted fat. Stir the mixture well and continue heating until the melt is homogeneous,
at no time allowing the temperature to exceed 150° C. Allow to cool somewhat and
carefully add 50 cc. 30 per cent sulfuric acid. Now add hot water and heat until the fatty
acids separate out perfectly clear. Draw off the acid water and wash the fatty acids with
hot water until free from mineral acid, then filter and heat to 130° C. as rapidly as
possible while stirring. Transfer the fatty acids, when cooled somewhat, to a 1-in. by 4-in.
titer tube, placed in a 16-oz. salt-mouth bottle of clear glass, fitted with a cork that is
perforated so as to hold the tube rigidly when in position. Suspend the titer thermometer
so that it can be used as a stirrer and stir the fatty acids slowly (about 100 revolutions per [Pg 176]
minute) until the mercury remains stationary for 30 seconds. Allow the thermometer to
hang quietly with the bulb in the center of the tube and report the highest point to which
the mercury rises as the titer of the fatty acids. The titer should be made at about 20° C.
for all fats having a titer above 30° C. and at 10° C. below the titer for all other fats. Any
convenient means may be used for obtaining a temperature of 10° below the titer of the
various fats. The committee recommends first of all a chill room for this purpose; second,

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an artificially chilled small chamber with glass window; third, immersion of the salt-
mouth bottle in water or other liquid of the desired temperature.

UNSAPONIFIABLE MATTER.

Extraction Cylinder—The cylinder shall be glass-stoppered, graduated at 40 cc., 80

cc. and 130 cc., and of the following dimensions: diameter about 1-3/8 in., height about
12 in.
Petroleum Ether—Redistilled petroleum ether, boiling under 75° C., shall be used. A
blank must be made by evaporating 250 cc. with about 0.25 g. of stearine or other hard
fat (previously brought to constant weight by heating) and drying as in the actual
determination. The blank must not exceed a few milligrams.
Determination—Weigh 5 g. (±0.20 g.) of the prepared sample into a 200-cc. Erlenmeyer
flask, add 30 cc. of redistilled 95 per cent (approximately) ethyl alcohol and 5 cc. of 50
per cent aqueous potassium hydroxide, and boil the mixture for one hour under a reflux
condenser. Transfer to the extraction cylinder and wash to the 40-cc. mark with redistilled
95 per cent ethyl alcohol. Complete the transfer, first with warm, then with cold water, till
the total volume amounts to 80 cc. Cool the cylinder and contents to room temperature [Pg 177]
and add 50 cc. of petroleum ether. Shake vigorously for one minute and allow to settle
until both layers are clear, when the volume of the upper layer should be about 40 cc.
Draw off the petroleum ether layer as closely as possible by means of a slender glass
siphon into a separatory funnel of 500 cc. capacity. Repeat extraction at least four more
times, using 50 cc. of petroleum ether each time. More extractions than five are necessary
where the unsaponifiable matter runs high, say over 5 per cent, and also in some cases
where it is lower than 5 per cent, but is extracted with difficulty. Wash the combined
extracts in a separatory funnel three times with 25-cc. portions of 10 per cent alcohol,
shaking vigorously each time. Transfer the petroleum ether extract to a wide-mouth tared
flask or beaker, and evaporate the petroleum ether on a steam bath in an air current. Dry
as in the method for moisture and volatile matter. Any blank must be deducted from
the weight before calculating unsaponifiable matter. Test the final residue for solubility in
50 cc. petroleum ether at room temperature. Filter and wash free from the insoluble
residue, if any, evaporate and dry in the same manner as before. The Committee wishes
to emphasize the necessity of thorough and vigorous shaking in order to secure accurate
results. The two phases must be brought into the most intimate contact possible,
otherwise low and disagreeing results may be obtained.

IODINE NUMBER—WIJS METHOD.

Preparation of Reagents—Wijs Iodine Solution—Dissolve 13.0 g. of resublimed iodine

in one liter of C. P. glacial acetic acid and pass in washed and dried chlorine gas until the
original thiosulfate titration of the solution is not quite doubled. The solution is then
preserved in amber glass-stoppered bottles, sealed with paraffin until ready for use.
Mark the date on which the solution is prepared on the bottle or bottles and do not use [Pg 178]
Wijs solution which is more than 30 days old.
There should be no more than a slight excess of iodine, and no excess of chlorine. When
the solution is made from iodine and chlorine, this point can be ascertained by not quite
doubling the titration.[32]
The glacial acetic acid used for preparation of the Wijs solution should be of 99.0 to 99.5
per cent strength. In case of glacial acetic acids of somewhat lower strength, the
Committee recommends freezing and centrifuging or draining as a means of purification.
N/10 Sodium Thiosulfate Solution—Dissolve 24.8 g. of C. P. sodium thiosulfate in
recently boiled distilled water and dilute with the same to one liter at the temperature at
which the titrations are to be made.
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Starch Paste—Boil 1 g. of starch in 200 cc. of distilled water for 10 min. and cool to
room temperature.
An improved starch solution may be prepared by autoclaving 2 g. of starch and 6 g. of
boric acid dissolved in 200 cc. water at 15 lbs. pressure for 15 min. This solution has
good keeping qualities. [Pg 179]

Potassium Iodide Solution—Dissolve 150 g. of potassium iodide in water and make up to

one liter.
N/10 Potassium Bichromate—Dissolve 4.903 g. of C. P. potassium bichromate in water
and make the volume up to one liter at the temperature at which titrations are to be made.
The Committee calls attention to the fact that occasionally potassium bichromate is found
containing sodium bichromate, although this is of rare occurrence. If the analyst suspects
that he is dealing with an impure potassium bichromate, the purity can be ascertained by
titration against re-sublimed iodine. However, this is unnecessary in the great majority of
cases.
Standardization of the Sodium Thiosulfate Solution—Place 40 cc. of the potassium
bichromate solution, to which has been added 10 cc. of the solution of potassium iodide,
in a glass-stoppered flask. Add to this 5 cc. of strong hydro-chloric acid. Dilute with 100
cc. of water, and allow the N/10 sodium thiosulfate to flow slowly into the flask until the
yellow color of the liquid has almost disappeared. Add a few drops of the starch paste,
and with constant shaking continue to add the N/10 sodium thiosulfate solution until the
blue color just disappears.
Determination—Weigh accurately from 0.10 to 0.50 g. (depending on the iodine
number) of the melted and filtered sample into a clean, dry, 16-oz. glass-stoppered bottle
containing 15-20 cc. of carbon tetrachloride or chloroform. Add 25 cc. of iodine solution
from a pipette, allowing to drain for a definite time. The excess of iodine should be from
50 per cent to 60 per cent of the amount added, that is, from 100 per cent to 150 per cent
of the amount absorbed. Moisten the stopper with a 15 per cent potassium iodide solution
to prevent loss of iodine or chlorine but guard against an amount sufficient to run down
inside the bottle. Let the bottle stand in a dark place for 1/2 hr. at a uniform temperature. [Pg 180]
At the end of that time add 20 cc. of 15 per cent potassium iodide solution and 100 cc. of
distilled water. Titrate the iodine with N/10 sodium thiosulfate solution which is added
gradually, with constant shaking, until the yellow color of the solution has almost
disappeared. Add a few drops of starch paste and continue titration until the blue color
has entirely disappeared. Toward the end of the reaction stopper the bottle and shake
violently so that any iodine remaining in solution in the tetrachloride or chloroform may
be taken up by the potassium iodide solution. Conduct two determinations on blanks
which must be run in the same manner as the sample except that no fat is used in the
blanks. Slight variations in temperature quite appreciably affect the titer of the iodine
solution, as acetic acid has a high coefficient of expansion. It is, therefore, essential that
the blanks and determinations on the sample be made at the same time. The number of
cc. of standard thiosulfate solution required by the blank, less the amount used in the
determination, gives the thiosulfate equivalent of the iodine absorbed by the amount of
sample used in the determination. Calculate to centigrams of iodine absorbed by 1 g. of
sample (= per cent iodine absorbed).
Determination, Tung Oil—Tung oil shows an erratic behavior with most iodine
reagents and this is particularly noticeable in the case of the Hanus reagent which is
entirely unsuitable for determining the iodine number of this oil since extremely high and
irregular results are obtained. The Hübl solution shows a progressive absorption up to 24
hrs. and probably for a longer time but the period required is entirely too long for a
chemical determination. The Wijs solution gives good results if the following precautions
are observed:

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Weigh out 0.15 ± 0.05 g., use an excess of 55 ± 3 per cent Wijs solution. Conduct the [Pg 181]
absorption at a temperature of 20-25° C. for 1 hr. In other respects follow the instructions
detailed above.

SAPONIFICATION NUMBER (KOETTSTORFER NUMBER).

Preparation of Reagents. N/2 Hydrochloric Acid—Carefully standardized.

Alcoholic Potassium Hydroxide Solution—Dissolve 40 g. of pure potassium hydroxide in
one liter of 95 per cent redistilled alcohol (by volume). The alcohol should be redistilled
from potassium hydroxide over which it has been standing for some time, or with which
it has been boiled for some time, using a reflux condenser. The solution must be clear and
the potassium hydroxide free from carbonates.
Determination—Weigh accurate about 5 g. of the filtered sample into a 250 to 300 cc.
Erlenmeyer flask. Pipette 50 cc. of the alcoholic potassium hydroxide solution into the
flask, allowing the pipette to drain for a definite time. Connect the flask with an air
condenser and boil until the fat is completely saponified (about 30 minutes). Cool and
titrate with the N/2 hydrochloric acid, using phenolphthalein as an indicator. Calculate the
Koettstorfer number (mg. of potassium hydroxide required to saponify 1 g. of fat).
Conduct 2 or 3 blank determinations, using the same pipette and draining for the same
length of time as above.

MELTING POINT.

Apparatus—Capillary tubes made from 5 mm. inside diameter thin-walled glass tubing
drawn out to 1 mm. inside diameter. Length of capillary part of tubes to be about 5 cm.
Length of tube over all 8 cm.
Standard thermometer graduated in tenths of a degree.
600 cc. beaker.
Determination—The sample should be clear when melted and entirely free from [Pg 182]
moisture, or incorrect results will be obtained.
Melt and thoroughly mix the sample. Dip three of the capillary tubes above described in
the oil so that the fat in the tube stands about 1 cm. in height. Now fuse the capillary end
carefully by means of a small blast flame and allow to cool. These tubes are placed in a
refrigerator over night at a temperature of from 40 to 50° F. They are then fastened by
means of a rubber band or other suitable means to the bulb of a thermometer graduated in
tenths of a degree. The thermometer is suspended in a beaker of water (which is agitated
by air or other suitable means) so that the bottom of the bulb of the thermometer is
immersed to a depth of about 3 cm. The temperature of the water is increased gradually at
the rate of about 1° per minute.
The point at which the sample becomes opalescent is first noted and the heating
continued until the contents of the tube becomes uniformly transparent. The latter
temperature is reported as the melting point.
Before finally melting to a perfectly clear fluid, the sample becomes opalescent and
usually appears clear at the top, bottom, and sides before becoming clear at the center.
The heating is continued until the contents of the tube become uniformly clear and
transparent. This temperature is reported as the melting point.[33] It is usually only a
fraction of a degree above the opalescent point noted. The thermometer should be read to
the nearest 1/2° C., and in addition this temperature may be reported to the nearest degree
Fahrenheit if desired.

CLOUD TEST.

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Precautions—(1) The oil must be perfectly dry, because the presence of moisture will [Pg 183]
produce a turbidity before the clouding point is reached.
(2) The oil must be heated to 150° C. over a free flame, immediately before making the
test.
(3) There must not be too much discrepancy between the temperature of the bath and the
clouding point of the oil. An oil that will cloud at the temperature of hydrant water should
be tested in a bath of that temperature. An oil that will cloud in a mixture of ice and water
should be tested in such a bath. An oil that will not cloud in a bath of ice and water must
be tested in a bath of salt, ice, and water.
Determination—The oil is heated in a porcelain casserole over a free flame to 150° C.,
stirring with the thermometer. As soon as it can be done with safety, the oil is transferred
to a 4 oz. oil bottle, which must be perfectly dry. One and one-half ounces of the oil are
sufficient for the test. A dry centigrade thermometer is placed in the oil, and the bottle is
then cooled by immersion in a suitable bath. The oil is constantly stirred with the
thermometer, taking care not to remove the thermometer from the oil at any time during
the test, so as to avoid stirring air bubbles into the oil. The bottle is frequently removed
from the bath for a few moments. The oil must not be allowed to chill on the sides and
bottom of the bottle. This is effected by constant and vigorous stirring with the
thermometer. As soon as the first permanent cloud shows in the body of the oil, the
temperature at which this cloud occurs is noted.
With care, results concordant to within 1/2° C. can be obtained by this method. A
Fahrenheit thermometer is sometimes used because it has become customary to report
results in degrees Fahrenheit.
The oil must be tested within a short time after heating to 150° C. and a re-test must
always be preceded by reheating to that temperature. The cloud point should be [Pg 184]
approached as quickly as possible, yet not so fast that the oil is frozen on the sides or
bottom of the bottle before the cloud test is reached.

Notes on the Above Methods.

SAMPLING.

The standard size of sample adopted by the committee is at least 3 lbs. in weight. The
committee realizes that this amount is larger than any samples usually furnished even
when representing shipments of from 20,000 to 60,000 lbs. but it believes that the
requirement of a larger sample is desirable and will work toward uniform and more
concordant results in analysis. It will probably continue to be the custom of the trade to
submit smaller buyers' samples than required by the committee, but these are to be
considered only as samples for inspection and not for analysis. The standard analytical
sample must consist of 3 lbs. or more.
The reasons for keeping samples in a dark, cool place are obvious. This is to prevent any
increase in rancidity and any undue increase in free fatty acids. In the case of many fats
the committee has found in its co-operative analytical work that free acid tends to
increase very rapidly. This tendency is minimized by low temperatures.

MOISTURE AND VOLATILE MATTER.

After careful consideration the committee has decided that moisture is best determined in
a vacuum oven of the design which accompanies the above report. Numerous results on
check samples have confirmed the committee's conclusions. The oven recommended by
the committee is constructed on the basis of well-known principles and it is hoped that
this type will be adopted generally by chemists who are called upon to analyze fats and
oils. The experiments of the committee indicate that it is a most difficult matter to design
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a vacuum oven which will produce uniform temperatures throughout; and one of the [Pg 185]
principal ideas in the design adopted is uniformity of temperature over the entire single
shelf. This idea has not quite been realized in practice but, nevertheless, the present
design approaches much closer to the ideal than other vacuum ovens commonly used. In
the drawing the essential dimensions are those between the heating units and the shelf
and the length and breadth of the outer casting. The standard Fat Analysis Committee
Oven (F. A. C. Oven) can be furnished by Messrs. E. H. Sargent & Company, 125 West
Lake street, Chicago.
The committee realizes that for routine work a quicker method is desirable and has added
one such method and has also stated the conditions under which comparable results can
be obtained by means of the ordinary well-ventilated air oven held at 105 to 110° C.
However, in accordance with a fundamental principle adopted by the committee at its
first meeting, only one standard method is adopted and declared official for each
determination.
The committee realizes that in the case of all methods for determining moisture by means
of loss on heating there may be a loss due to volatile matter (especially fatty acids) other
than water. The title of the determination moisture and volatile matter indicates this
idea, but any considerable error from this source may occur only in the case of high acid
fats and oils and particularly those containing lower fatty acids such as coconut and palm
kernel oil. In the case of extracted greases which have not been properly purified, some
of the solvent may also be included in the moisture and volatile matter determination, but
inasmuch as the solvent, usually a petroleum product, can only be considered as foreign
matter, for commercial purposes, it is entirely proper to include it with the moisture.
The committee has also considered the various distillation methods for the determination
of moisture in fats and oils, but since according to the fundamental principles which it [Pg 186]
was endeavoring to follow it could only standardize one method, it was decided that the
most desirable one on the whole was the vacuum-oven method as given. There are cases
wherein a chemist may find it desirable to check a moisture determination or investigate
the moisture content of a fat or oil further by means of one of the distillation methods.
However, in co-operative work the distillation method in various types of apparatus has
not yielded satisfactory results. The difficulties appear to be connected with a proper
choice of solvent and particularly with the tendency of drops of water to adhere to
various parts of the glass apparatus instead of passing on to the measuring device. When
working on coconut oil containing a high percentage of free fatty acids, concordant
results could not be obtained by the various members of the committee when working
with identical samples, solvents and apparatus.
On the other hand, the committee found by individual work, co-operative work and
collaborative work by several members of the committee in one laboratory, that the old,
well-known direct heating method (which the committee has designated the hot plate
method) yielded very satisfactory results on all sorts of fats and oils including emulsions
such as butter and oleomargarine and even on coconut oil samples containing 15 to 20
per cent free fatty acids and 5 to 6 per cent of moisture. Unfortunately, this method
depends altogether on the operator's skill and while the method may be taught to any
person whether a chemist or not so that he can obtain excellent results with it, it is
difficult to give a sufficiently, complete description of it so that any chemist anywhere
after reading the description could follow it successfully. The method is undoubtedly
worthy of much confidence in careful hands. It is quick, accurate and reliable. It is [Pg 187]
probably the best single method for the determination of moisture in all sorts of samples
for routine laboratory work. On account of this fact the committee desires to announce its
willingness to instruct any person in the proper use of the method who desires to become
acquainted with it and who will visit any committee member's laboratory.

INSOLUBLE IMPURITIES.

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This determination, the title for which was adopted after careful consideration,
determines the impurities which have generally been known as dirt, suspended matter,
suspended solids, foreign solids, foreign matter, etc., in the past. The first solvent
recommended by the committee is hot kerosene to be followed by petroleum ether kept at
ordinary room temperature. Petroleum ether, cold or only slightly warm, is not a good fat
and metallic soap solvent, whereas hot kerosene dissolves these substances readily, and
for this reason the committee has recommended the double solvent method so as to
exclude metallic soaps which are determined below as soluble mineral matter.

SOLUBLE MINERAL MATTER.

Soluble mineral matter represents mineral matter combined with fatty acids in the form
of soaps in solution in the fat or oil. Formerly, this mineral matter was often determined
in combination by weighing the separated metallic soap or by weighing it in conjunction
with the insoluble impurities. Since the soaps present consist mostly of lime soap, it has
been customary to calculate the lime present therein by taking 0.1 the weight of the total
metallic soaps. The standard method as given above is direct and involves no calculation.
The routine method given in the note has been placed among the methods for the reason
that it is used in some laboratories, but has not been adopted as a standard method in
view of the fact that the committee has made it a rule to adopt only one standard method. [Pg 188]
It should be pointed out, however, that the method cannot be considered accurate for the
reason that insoluble impurities may vary from sample to sample to a considerable extent
and the error due to the presence of large particles of insoluble impurities is thus
transferred to the soluble mineral matter. The committee has found one type of grease
(naphtha bone grease) which shows most unusual characteristics. The type sample
contains 4.3 per cent soluble mineral matter by the committee method which would be
equivalent to 43.0 per cent free fatty acid. The kerosene and gasoline filtrate was
particularly clear, nevertheless the ash was found to contain 36.43 per cent P2O5
equivalent to 79.60 per cent of Ca3(PO4)2 and 9.63 per cent of Fe2O3. The method,
therefore, determines the soluble mineral matter in this case satisfactorily but the factor
10 is not applicable for calculating the fatty acids combined therewith. It is necessary,
therefore, in order to determine the fatty acids combined with soluble mineral matter in
the original sample to determine the actual bases in the soluble mineral matter as
obtained by ashing the kerosene and gasoline filtrate. To the bases so determined the
factor 10 can then be applied.

FREE FATTY ACID.

The fatty acid method adopted is sufficiently accurate for commercial purposes. In many
routine laboratories the fat or oil is measured and not weighed, but the committee
recommends weighing the sample in all cases. For scientific purposes the result is often
expressed as "acid number," meaning the number of milligrams of KOH required to
neutralize the free acids in one gram of fat, but the commercial practice has been, and is,
to express the fatty acids as oleic acid or in the case of palm oil, as palmitic acid, in some
instances. The committee sees no objection to the continuation of this custom so long as [Pg 189]
the analytical report clearly indicates how the free acid is expressed. For a more exact
expression of the free acid in a given fat, the committee recommends that the ratio of acid
number to saponification number be used. This method of expressing results is subject to
error when unsaponifiable fatty matter is present, since the result expresses the ratio of
free fatty acid to total saponifiable fatty matter present.

TITER.

At the present time the prices of glycerol and caustic potash are abnormally high, but the
committee has considered that the methods adopted are for normal times and normal

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prices. For routine work during the period of high prices the following method may be
used for preparing the fatty acids and is recommended by the committee:
Fifty grams of fat are saponified with 60 cc. of a solution of 2 parts of methyl alcohol to 1
of 50 per cent NaOH. The soap is dried, pulverized and dissolved in 1000 cc. of water in
a porcelain dish and then decomposed with 25 cc. of 75 per cent sulphuric acid. The fatty
acids are boiled until clear oil is formed and then collected and settled in a 150-cc. beaker
and filtered into a 50-cc. beaker. They are then heated to 130° C. as rapidly as possible
with stirring, and transferred, after they have cooled somewhat, to the usual 1-in. by 4-in.
titer tube.
The method of taking the titer, including handling the thermometer, to be followed is the
same as that described in the standard method. Even at present high prices many
laboratories are using the glycerol-caustic potash method for preparing the fatty acids,
figuring that the saving of time more than compensates for the extra cost of the reagents.
Caustic soda cannot be substituted for caustic potash in the glycerol method. [Pg 190]

UNSAPONIFIABLE MATTER.

The committee has considered unsaponifiable matter to include those substances

frequently found dissolved in fats and oils which are not saponified by the caustic
alkalies and which at the same time are soluble in the ordinary fat solvents. The term
includes such substances as the higher alcohols, such as cholesterol which is found in
animal fats, phytosterol found in some vegetable fats, paraffin and petroleum oils, etc.
Unsaponifiable matter should not be confused in the lay mind with insoluble
impurities or soluble mineral matter.
The method adopted by the committee has been selected only after the most careful
consideration of other methods, such as the dry extraction method and the wet method
making use of the separatory funnel. At first consideration the dry extraction process
would seem to offer the best basis for an unsaponifiable matter method, but in practice it
has been found absolutely impossible for different analysts to obtain agreeing results
when using any of the dry extraction methods proposed. Therefore, this method had to be
abandoned after numerous trials, although several members of the committee strongly
favored it in the beginning.
Iodine Number—The iodine number adopted by the committee is that determined by the
well-known Wijs method. This method was adopted after careful comparison with the
Hanus and Hübl methods. The Hübl method was eliminated from consideration almost at
the beginning of the committee's work for the reason that the time required for complete
absorption of the iodine is unnecessarily long and, in fact, even after absorption has gone
on over night, it is apparently not complete. In the case of the Hanus and Wijs methods
complete absorption takes place in from 15 minutes to an hour, depending on conditions.
Formerly, many chemists thought the Hanus solution rather easier to prepare than the [Pg 191]
Wijs solution, but the experience of the committee was that the Wijs solution was no
more difficult to prepare than the Hanus. Furthermore, absorption of iodine from the Wijs
solution appeared to take place with greater promptness and certainty than from the
Hanus and was complete in a shorter time. Results by the Wijs method were also in better
agreement in the case of oils showing high iodine absorption than with the Hanus
solution and showed a slightly higher iodine absorption for the same length of time.
However, the difference was not great. The committee investigated the question of
substitution since it has been suggested that in case of the Wijs solution substitution of
iodine in the organic molecule might occur, and found no evidence of this in the time
required for the determination, namely, 1/2 hr., or even for a somewhat longer period.
One member of the committee felt that it was not desirable to introduce the Wijs method
into these standard methods since the Hanus method was already standardized by the
Association of Official Agricultural Chemists, but the committee felt that it must follow
the principle established at the commencement of its work, namely, that of adopting the
method which appeared to be the best from all standpoints, taking into consideration
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accuracy, convenience, simplicity, time, expense, etc., without allowing precedent to have
the deciding vote.
Iodine Number, Tung Oil—The committee has made an extensive study of the
application of the Wijs method to the determination of iodine value in the case of tung oil
with the result that it recommends the method for this oil but has thought it desirable to
limit the conditions under which the determination is conducted rather narrowly, although
reasonably good results are obtained by the committee method without making use of the
special limitations.
The co-operative work of the committee and the special investigations conducted by [Pg 192]
individual members bring out the following points:
Influence of Temperature—From 16° C. to 30° C. there is a moderate increase in the
absorption, but above 30° the increase is rather rapid so that it was thought best to limit
the temperature in the case of tung oil to 20° to 25° C.
Influence of Time—The absorption increases with the time but apparently complete
absorption, so far as unsaturated bonds are concerned, occurs well within one hour's time.
Consequently, one hour was set as the practical limit.
Influence of Excess—The excess of iodine solution also tends to increase the iodine
number, hence the Committee thought it necessary to limit the excess rather rigidly to 55
± 3 per cent, although with greater latitude results were reasonably good.
Influence of Age of Solution—Old solutions tend to give low results although up to 2 mo.
no great differences were observed. Nevertheless, it was thought best to limit the age of
the solution to 30 days—long enough for all practical purposes.
Amount of Sample—As a practical amount of sample to be weighed out the Committee
decided on 0.15 g. with a tolerance of 0.05 g. in either direction according to preference.
In other words, the amount of sample to be taken for the determination to be from 0.1 to
0.2 g. in the discretion of the analyst.
The Committee's study of the Hübl method which has been adopted by the Society for
Testing Materials in the case of tung oil indicates that this method when applied to tung
oil is subject to the same influences as the Wijs method and it has the additional very
serious disadvantage of requiring a long period of time for absorption which cannot be
considered reasonable for a modern analytical method. When using the Hübl solution, the
absorption is not complete in the case of tung oil at 3, 7, 18 or even 24 hrs. [Pg 193]

The Hanus method in the case of tung oil gives very high and erratic results, as high as
180 to 240 in ordinary cases for an oil whose true iodine number is about 165.

MELTING POINT.

A melting point is the temperature at which a solid substance assumes the liquid
condition. If the solid is a pure substance in the crystalline condition the melting point is
sharp and well defined for any given pressure. With increased pressure the melting point
is lowered or raised, depending on whether the substance contracts or expands in melting.
The lowering or raising of the melting point with pressure is very slight and ordinarily is
not taken into consideration. Melting-point determinations are commonly carried out
under ordinary atmospheric pressures without correction. The general effect of soluble
impurities is to lower the melting point, and this holds true whether the impurity has a
higher or lower melting point than the pure substance (solvent). Thus if a small amount
of stearic acid be added to liquid palmitic acid and the solution frozen, the melting point
of this solid will be lower than that of palmitic acid. Likewise the melting point of stearic
acid is lowered by the addition of a small amount of palmitic acid. A eutectic mixture
results when two components solidify simultaneously at a definite temperature. Such a
mixture has a constant melting point and because of this and also because both solid and

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liquid phases have the same composition, eutectic mixtures were formerly looked upon
as compounds. The phenomenon of double melting points has been observed in the case
of a number of glycerides. Such a glyceride when placed in the usual capillary tube and
subjected to increasing temperature quickly resolidifies only to melt again and remain [Pg 194]
melted at a still higher temperature. This phenomenon has not yet been sufficiently
investigated to afford a satisfactory explanation.
Non-crystalline substances such as glass, sealing wax and various other waxes and wax
mixtures, and most colloidal substances do not exhibit a sharp melting point, but under
the application of heat first soften very gradually and at a considerably higher
temperature melt sufficiently to flow. This phenomenon of melting through a long range
of temperature may be due to the amorphous nature of the substance or to the fact that it
consists of a very large number of components of many different melting points.
The fats and oils of natural origin, that is, the animal and vegetable fats and oils, consist
of mixtures of glycerides and, generally speaking, of a considerable number of such
components. These components are crystalline and when separated in the pure state have
definite melting points, although some exhibit the phenomenon of double melting point.
For the most part the naturally occurring glycerides are mixed glycerides. In the natural
fats and oils there are present also certain higher alcohols, of which cholesterol is
characteristic of the animal fats and oils and phytosterol of many of the vegetable fats
and oils. In addition to the crystalline glycerides and the higher alcohols present in
neutral fats, there are in fats of lower grade, fatty acids, which are crystalline, and also
various non-crystalline impurities of an unsaponifiable nature, and the presence of these
impurities tends to lower the melting point. They also tend to induce undercooling and
when the liquid fat or oil is being chilled for purposes of solidification or in
determination of titer.
The presence of water, especially when this is thoroughly mixed or emulsified with a fat
or oil, also influences the melting point to a marked extent, causing the mixture to melt [Pg 195]
through a longer range of temperatures than would be the case if the water were absent.
This is particularly true of emulsified fats and oils, such as butter and oleomargarine,
both of which contain, besides water, the solids naturally present in milk or cream and
including casein, milk sugar, and salts. The melting-point method recommended by the
Committee is not applicable to such emulsions or other watery mixtures and the
Committee has found it impossible to devise an accurate method for making softening-
point or melting-point determinations on products of this nature. Not only the amount of
water present but also the fineness of its particles, that is, its state of subdivision and
distribution, in a fat or oil influences the softening point or melting point and causes it to
vary widely in different samples.
As a consequence of the foregoing facts, natural fats and oils do not exhibit a definite
melting point, composed as they are of mixtures of various crystalline glycerides, higher
alcohols, fatty acids, and non-crystalline substances. Therefore, the term melting point
when applied to them requires further definition. They exhibit first a lower melting point
(the melting point of the lowest melting component) or what might be called the
softening point and following this the fat softens through a shorter or longer range of
temperature to the final melting point at which temperature the fat is entirely liquid. This
is the melting point determined by the Committee's melting-point method. The range
between the softening point and the final melting point varies greatly with the different
fats and oils depending on their chemical components, the water associated with them,
emulsification, etc. In the case of coconut oil the range between softening point and final
melting point is rather short; in the case of butter, long. Various methods have been
devised to determine the so-called melting point of fats and oils. Most of these methods,
however, determine, not the melting point, but the softening point or the flow point of the [Pg 196]
fat and the great difficulty has been in the past to devise a method which would
determine even this point with reasonable accuracy and so that results could be easily
duplicated. It has been the aim of the Committee to devise a simple method for the

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determination of the melting point of fats and oils, but it should be understood that the
term melting point in the scientific sense is not applicable to natural fats and oils.

FOOTNOTES:
[22] Approved by the Supervisory Committee on Standard Methods of Analysis of
the American Chemical Society.
[23] Live steam must not be turned into tank cars or coils before samples are drawn,
since there is no certain way of telling when coils are free from leaks.
[24] If there is water present under the solid material this must be noted and
estimated separately.
[25] Boiling point of water at reduced pressures.

Pressure Mm. Boiling Point to 1° Boiling Point +15° Boiling Point +20°
Hg. C. C. C.
100 52° C. 67° C. 72° C.
90 50 65 70
80 47 62 67
70 45 60 65
60 42 57 62
50 38 53 58
40 34 49 54

[26] Results comparable to those of the Standard Method may be obtained on most
fats and oils by drying 5-g. portions of the sample, prepared and weighed as
above, to constant weight in a well-constructed and well-ventilated air oven
held uniformly at a temperature of 105° to 110° C. The thermometer bulb
should be close to the sample. The definition of constant weight is the same as
for the Standard Method.
[27] The following method is suggested by the Committee for routine control work:
Weigh out 5- to 25-g. portions of prepared sample into a glass or aluminum
(Caution: Aluminum soap may be formed) beaker or casserole and heat on a
heavy asbestos board over burner or hot plate, taking care that the temperature
of the sample does not go above 130° C. at any time. During the heating rotate
the vessel gently on the board by hand to avoid sputtering or too rapid
evolution of moisture. The proper length of time of heating is judged by
absence of rising bubbles of steam, by the absence of foam or by other signs
known to the operator. Avoid overheating of sample as indicated by smoking or
darkening. Cool in desiccator and weigh.
By co-operative work in several laboratories, the Committee has demonstrated
that this method can be used and satisfactory results obtained on coconut oil
even when a considerable percentage of free fatty acids is present, and the
method is recommended for this purpose. Unfortunately on account of the very
great personal factor involved, the Committee cannot establish this method as a
preferred method. Nevertheless, after an operator has learned the technique of
the method, it gives perfectly satisfactory results for ordinary oils and fats,
butter, oleomargarine and coconut oil, and deserves more recognition than it
has heretofore received.
[28] For routine control work, filter paper is sometimes more convenient than the
prepared Gooch crucible, but must be very carefully washed, especially around
the rim, to remove the last traces of fat.

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[29] For routine work, an ash may be run on the original fat, and the soluble mineral
matter obtained by deducting the ash on the insoluble impurities from this. In
this case the Gooch crucible should be prepared with an ignited asbestos mat
so that the impurities may be ashed directly after being weighed. In all cases
ignition should be to constant weight so as to insure complete decomposition
of carbonates.
[30] See note on Soluble Mineral Matter following these methods. When the ash
contains phosphates the factor 10 cannot be applied, but the bases consisting of
calcium oxide, etc., must be determined, and the factor 10 applied to them.
[31] For routine work methyl or denatured ethyl alcohol of approximately 95 per
cent strength may be used. With these reagents the end-point is not sharp.
[32] P. C. McIlhiney, J. Am. Chem. Soc., 29 (1917), 1222, gives the following
details for the preparation of the iodine monochloride solution:
The preparation of the iodine monochloride solution presents no great
difficulty, but it must be done with care and accuracy in order to obtain
satisfactory results. There must be in the solution no sensible excess either of
iodine or more particularly of chlorine, over that required to form the
monochloride. This condition is most satisfactorily attained by dissolving in
the whole of the acetic acid to be used the requisite quantity of iodine, using a
gentle heat to assist the solution, if it is found necessary, setting aside a small
portion of this solution, while pure and dry chlorine is passed into the
remainder until the halogen content of the whole solution is doubled.
Ordinarily it will be found that by passing the chlorine into the main part of the
solution until the characteristic color of free iodine has just been discharged
there will be a slight excess of chlorine which is corrected by the addition of
the requisite amount of the unchlorinated portion until all free chlorine has
been destroyed. A slight excess of iodine does little or no harm, but excess of
chlorine must be avoided.
[33] The melting point of oils may be determined in general according to the above
procedure, taking into consideration the lower temperature required.

PLANT AND MACHINERY [Pg 198]

Illustrations of machinery and layouts of the plant of a modern soap-

making establishment.

[Pg 199]

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[Pg 218]

Appendix [Pg 219]

Tables marked * are taken from the German Year Book for Soap
Industry.

(U. S. BUREAU OF STANDARDS) [Pg 220]

THE METRIC SYSTEM.

The fundamental unit of the metric system is the meter (the unit of length). From this the
units of mass (gram) and capacity (liter) are derived. All other units are the decimal sub-
divisions or multiples of these. These three units are simply related, so that for all
practical purposes the volume of one kilogram of water (one liter) is equal to one cubic
decimeter.

Prefixes. Meaning. Units.

Milli- = one thousandth 1-1000 .001
Centi- = one hundredth 1-100 .01 Meter for length.
Deci- = one tenth 1-10 .1
Unit = one 1.
Gram for mass.
Deka- = ten 10-1 10.
Hecto- = one hundred 100-1 100.
Liter for capacity.
Kilo- = one thousand 1000-1 1000.

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The metric terms are formed by combining the words "Meter," "Gram" and "Liter" with
the six numerical prefixes.

Length

10 milli-meters mm = 1 centi-meter cm
10 centi-meters = 1 deci-meter dm
10 deci-meters = 1 meter (about 40 inches) m
10 meters = 1 deka-meter dkm
10 deka-meters = 1 hecto-meter hm
10 hecto-meters = 1 kilo-meter (about 5/8 mile) k m
[Pg 221]
Mass.

10 milli-grams. m g = 1 centi-gram cg
10 centi-grams = 1 deci-gram dg
10 deci-grams = 1 gram (about 15 grains) g
10 grams = 1 deka-gram dkg
10 Deka-grams = 1 hecto-gram hg
10 hecto-grams = 1 kilo-gram (about 2 pounds) k g

Capacity.

10 milli-liters. m l = 1 centi-liter cl
10 centi-liters = 1 deci-liter dl
10 deci-liters = 1 liter (about 1 quart) l
10 liters = 1 deka-liter dkl
10 deka-liters = 1 hecto-liter (about a barrel) h l
10 hecto-liters = 1 kilo-liter kl

The square and cubic units are the squares and cubes of the linear units.
The ordinary unit of land area is the Hectare (about 2-1/2 acres). [Pg 222]

U.S. BUREAU OF STANDARDS TABLE OF METRIC

EQUIVALENTS

Meter = 39.37 inches.

Legal Equivalent Adopted by Act of Congress July 28, 1866.

Length.

Centimeter = 0.3937 inch

Meter = 3.28 feet
Meter = 1.094 yards
Kilometer = 0.621 statute mile
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Kilometer = 0.5396 nautical mile

Inch = 2.540 centimeters
Foot = 0.305 meter
Yard = 0.914 meter
Statute mile = 1.61 kilometers
Nautical mile = 1.853 kilometers

Area.

Sq. centimeter = 0.155 sq. inch

Sq. meter = 10.76 sq. feet
Sq. meter = 1.196 sq. yards
Hectare = 2.47 acres
Sq. kilometer = 0.386 sq. mile
Sq. inch = 6.45 sq. centimeters
Sq. foot = 0.0929 sq. meter
Sq. yard = 0.836 sq. meter
Acre = 0.405 hectare
Sq. mile = 2.59 sq. kilometers

[Pg 223]
Weight.

Gram = 15.43 grains

Gram = 0.772 U. S. apoth. scruple
Gram = 0.2572 U. S. apoth. dram
Gram = 0.0353 avoir. ounce
Gram = 0.03215 troy ounce
Kilogram = 2.205 avoir. pounds
Kilogram = 2.679 troy pounds
Metric ton = 0.984 gross or long ton
Metric ton = 1.102 short or net tons
Grain = 0.064 gram
U. S. apoth. scruple = 1.296 grams
U. S. apoth. dram = 3.89 grams
Avoir. ounce = 28.35 grams
Troy ounce = 31.10 grams
Avoir. pound = 0.4536 kilogram
Troy pound = 0.373 kilogram
Gross or long ton = 1.016 metric tons
Short or net ton = 0.907 metric ton

Volume.
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Cu. centimeter = 0.0610 cu. inch

Cu. meter = 35.3 cu. feet
Cu. meter = 1.308 cu. yards
Cu. inch = 16.39 cu. centimeters
Cu. foot = 0.283 cu. meter
Cu. yard = 0.765 cu. meter
[Pg 224]
Capacity.

Millimeter = 0.0338 U. S. liq. ounce

Millimeter = 0.2705 U. S. apoth. dram
Liter = 1.057 U. S. liq. quarts
Liter = 0.2642 U. S. liq. gallon
Liter = 0.908 U. S. dry quart
Dekaliter = 1.135 U. S. pecks
Hectoliter = 2.838 U. S. bushels
U. S. liq. ounce = 29.57 millimeters
U. S. apoth. dram = 3.70 millimeters
U. S. liq. quarts = 0.946 liter
U. S. dry quarts = 1.101 liters
U. S. liq. gallon = 3.785 liters
U. S. peck = 0.881 dekaliter
U. S. bushel = 0.3524 hectoliter

AVOIRDUPOIS WEIGHT.

1 pound = 16 ounces = 256 drams

1 ounce = 16 "

TROY (APOTHECARIES') WEIGHT (U. S.)

1 pound = 12 ounces = 96 drams = 288 scruples = 5,760 grains

1 ounce = 8 drams = 24 scruples = 480 grains
1 dram = 3 scruples = 60 grains
1 scruple = 20 grains

WINE (APOTHECARIES) LIQUID MEASURE (U. S.)

1 gallon = 8 pints = 128 fl. ozs. = 1,024 fl. drams = 61,440 minims
1 pint = 16 fl. ozs. = 128 fl. drams = 7,689 minims
1 fl. oz. = 8 fl. drams = 480 minims
1 fl. dram = 60 minims

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To find diameter of a circle multiply circumference by .31831. [Pg 225]

To find circumference of a circle, multiply diameter by 3.1416.

To find area of a circle, multiply square of diameter by .7854.
To find surface of a ball, multiply square of diameter by 3.1416.
To find side of an equal square, multiply diameter by .8862.
To find cubic inches in a ball, multiply cube of diameter by .5236.
Doubling the diameter of a pipe, increases its capacity four times.
One cubic foot of anthracite coal weighs about 53 lbs.
One cubic foot of bituminous coal weighs from 47 to 50 pounds.
A gallon of water (U. S. standard) weighs 8-1/3 pounds and contains 231 cubic inches.
A cubic foot of water contains 7-1/2 gallons, 1728 cubic inches and weighs 62-1/2
pounds.
To find the number of pounds of water a cylindrical tank contains, square the diameter,
multiply by .785 and then by the height in feet. This gives the number of cubic feet which
multiplied by 62-1/2 gives the capacity in pounds of water. Divide by 7-1/2 and this gives
the capacity in gallons.
A horse-power is equivalent to raising 33,000 pounds 1 foot per minute, or 550 pounds 1
foot per second. [Pg 226]

The friction of water in pipes is as the square of velocity. The capacity of pipes is as the
square of their diameters; thus, doubling the diameter of a pipe increases its capacity four
times.
To find the diameter of a pump cylinder to move a given quantity of water per minute
(100 feet of piston being the standard of speed), divide the number of gallons by 4, then
extract the square root, and the product will be the diameter in inches of the pump
cylinder.
To find the horse-power necessary to elevate water to a given height, multiply the weight
of the water elevated per minute in pounds by the height in feet, and divide the product
by 33,000 (an allowance should be added for water friction, and a further allowance for
loss in steam cylinder, say from 20 to 30 per cent).
To compute the capacity of pumping engines, multiply the area of water piston, in inches,
by the distance it travels, in inches, in a given time. Deduct 3 per cent for slip and rod
displacement. The product divided by 231 gives the number of gallons in time named.
To find the velocity in feet per minute necessary to discharge a given volume of water in a
given time, multiply the number of cubic feet of water by 144 and divide the product by
the area of the pipe in inches.
To find the area of a required pipe, the volume and velocity of water being given,
multiply the number of cubic feet of water by 144 and divide the product by the velocity
in feet per minute. The area being found, the diameter can be learned by using any table
giving the "area of circles" and finding the nearest area, opposite to which will be found
the diameter to correspond. [Pg 227]

Physical and Chemical Constants of Fixed Oils and Fats.

(From Lewkowitsch and other authorities.)

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Specific gravity Specific gravity Melting- Solidifying-

at 15°C. at 100°C. point. C. point. C.
Linseed oil 0.931-0.938 0.880 -16° to -26° -16°
Hemp-seed oil 0.925-0.931 -27°
Walnut oil 0.925-0.926 0.871 -27°
Poppy-seed oil 0.924-0.927 0.873 -18°
Sunflower oil 0.924-0.926 0.919 -17°
Fir-seed oil 0.925-0.928 -27° to -30°
Maize oil 0.921-0.926 -10° to -15°
Cotton-seed oil 0.922-0.930 0.867 12°
Sesame oil 0.923-0.924 0.871 -5°
Rape-seed oil 0.914-0.917 0.863 -2° to -10°
Black mustard oil 0.916-0.920 -17.5°
Croton oil 0.942-0.955 -16°
Castor oil 0.960-0.966 0.910 -12° to -18°
Apricot-kernel oil 0.915-0.919 -14°
Almond oil 0.915-0.920 -10° to -20°
Peanut (arachis) oil 0.916-0.920 0.867 -3° to -7°
Olive oil 0.914-0.917 0.862 2°
Menhaden oil 0.927-0.933 -4°
Cod-liver oil 0.922-0.927 0.874 0° to -10°
Seal oil 0.924-0.929 0.873 3°
Whale oil 0.920-0.930 0.872 -2°
Dolphin oil 0.917-0.918 5° to -3°
Porpoise oil 0.926 0.871 -16°
Neat's-foot oil 0.914-0.916 0.861 0° to 1.5°
Cotton-seed
0.919-0.923 0.867 40° 31° to 32.5°
stearine
Palm oil 0.921-0.925 0.856 27° to 42°
Cacao butter 0.950-0.952 0.858 30° to 33° 25° to 26°
Cocoa-nut oil 0.925-0.926 0.873 20° to 26° 16° to 20°
Myrtle wax 0.995 0.875 40° to 44° 39° to 43°
Japan wax 0.970-0.980 0.875 51° to 54.5° 46°
Lard 0.931-0.938 0.861 41° to 46° 29°
Bone fat 0.914-0.916 21° to 22° 15° to 17°
Tallow 0.943-0.952 0.860 42° to 46° 35° to 37°
Butter fat 0.927-0.936 0.866 29.5° to 33° 19° to 20°
Oleomargarine 0.924-0.930 0.859
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Sperm oil 0.875-0.884 0.833 -25°

Bottle-nose oil 0.879-0.880 0.827
Carnauba wax 0.990-0.999 0.842 84° to 85° 80° to 81°
Wool-fat 0.973 0.901 39° to 42° 30° to 30.2°
Beeswax 0.958-0.969 0.822 62° to 64° 60.5° to 62°
Spermaceti 0.960 0.812 43.5° to 49° 43.4° to 44.2°
Chinese wax 0.970 0.810 80.5° to 81° 80.5° to 81°
Tung (Chinese
0.936-0.942 below -17°
wood oil)
Soya-bean oil 0.924-0.927 8° to 15°

[Pg 228]
Physical and Chemical Constants of Fixed Oils and Fats.

(From Lewkowitsch and other Authorities.)

Saponification Maumené Iodine Hehner Reichert

value. test. value. value. value.
Linseed oil 190-195 104°-111° 175-190
Hemp-seed oil 190-193 95°-96° 148
Walnut oil 195 96°-101° 144-147
Poppy-seed oil 195 86°-88° 134-141 95.38
Sunflower oil 193-194 72°-75° 120-129 95
118.9-
Fir-seed oil 191.3 98°-99°
120
Maize oil 188-193 56°-60.5° 117-125 89-95.7 2.5
Cotton-seed oil 191-195 68°-77° 104-110 96-17
Sesame oil 189-193 64°-68° 105-109 95.8 0.35
Rape-seed oil 170-178 51°-60° 95-105 95
Black mustard oil 174-174.6 43°-44° 96-110 95.05
101.7-
Croton oil 210.3-215 89 13.5
104
Castor oil 178-186 46°-47° 83.4-85.9 1.4
Apricot-kernel oil 192.2-193.1 42.5°-46° 100-107
Almond oil 190.5-195.4 51°-54° 93-97 96.2
Peanut (arachis) oil 190-197 45°-49° 85-98 95.86
Olive oil 191-196 41.5°-45.5° 80.6-84.5 95.43 0.3
Menhaden oil 189.3-192 123°-128° 140-170 1.2
Cod-liver oil 182-187 102°-103° 154-180 95.3
Seal oil 190-196 92° 127-140 94.2 0.22
Whale-oil 188-193 91°-92° 110-136 93.5 2.04
Dolphin {Body oil 197.3 99.5 93.07 5.6

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oil {Jaw oil 200 32.8 66.28 65.92

Porpoise {Body oil 216-218.8 50° 119.4 23.45
oil {Jaw oil 253.7 49.6 68.41 65.8
Neat's-foot oil 194.3 47°-48.5° 69.3-70.4
Cotton-seed
194.6-195.1 48° 88.7-92.8 96.3
stearine.
Palm oil 196.3-202 53-57 95.6 0.5
Cacao butter 192.2-193.5 32-41 94.59 1.6
Cocoa-nut oil 250-253 8.5-9.3 88.6 3.7
Myrtle wax 205.7-211.7 2.9
Japan wax 220-222.4 4.2-8.5 90.6
Lard 195.3-196.6 27°-32° 57-70 96
Bone fat 190.9 46.3-49.6
Tallow 195-198 36-47 95.6 0.25
Butter fat 221.5-227 26-35 87.5 28.78
Oleomargarine 194-203.7 55.3-60 95-96 2.6
Sperm oil 132.5-147 47°-51° 84 1.3
Bottle-nose oil 126-134 41°-47° 77.4-82 1.4
Carnauba wax 80-84 13.5
Wool-fat 98.2-102.4 25-28
Beeswax 91-96 8.3-11
Spermaceti 128
Chinese wax 63
Tung (Chinese
193 150-165
wood oil)
121.3-
Soya-bean oil 190.6-192.9 59°-61° 95.5
124
[Pg 229]
*Temperature Correction Table for Hehner's Concentrated Bichromate
Solution for Glycerine Analysis

A Temperature f Corrected Volume 1 c.c. Logarithm

11° C 0.9980 ccm 99913
12° " 0.9985 " 99935
13° " 0.9990 " 99956
14° " 0.9995 " 99978
15° " 1.0000 " 00000
16° " 1.0005 " 00022
17° " 1.0010 " 00043
18° " 1.0015 " 00065
19° " 1.0020 " 00087
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20° " 1.0025 " 00108

21° " 1.0030 " 00130
22° " 1.0035 " 00152
23° " 1.0040 " 00173

*Table of Important Fatty Acids

Boiling Point
Mol. Ordinary 100 mm Melting Neutralization
Name Formula
Wt. Pressure Pressure Pt. value Mg. KOH
Butyric C4H8O2 88 162.3 637.5

Caproic C6H12O2 116 199.7 483.6

Caprylic C8H16O2 144 236-237 16.5 389.6

Capric C10H20O2 172 268-270 199.5-200 31.3 326.2

Lauric C12H24O2 200 225 43.6 280.5

Myristic C14H28O2 228 250.5 53.8 246.1

Palmitic C16H32O2 256 268.5 62 219.1

Stearic C18H36O2 284 291 69.2 197.5

Arachidic C20H40O2 302 75 185.8

Behenic C22H44O2 330 77-78 170.0

Cerotic C27H54O2 400 78 140.25

Melissic C30H60O2 442 90 126.5

Oleic C18H34O2 282 185.5-286 14 198.9

Erucic C22H42O2 338 33-34 165.9

Linolic C18H32O2 280 200.4

Linolenic C18H30O2 278 201.5

Ricinoleic C18H34O3 298 181.6

[Pg 230]
*Comparison of Thermometer Scales

n Degree Celsius = 4/5n Degree Reaumur = 32 + 9/5n Degree Fahrenheit

n Degree Reaumur = 5/4n Degree Celsius = 32 + 9/4n Degree Fahrenheit
n Degree Fahrenheit = 5/9 (n - 32) Degree Celsius = 4/9 (n - 32) Deg. R

C. R. F. C. R. F. C. R. F. C. R. F.
-20 -16 -4 20 16 68 60 48 140 100 80 212
-19 -15.2 -2.2 21 16.8 69.8 61 48.8 141.8 101 80.8 213.8

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-18 -14.4 -0.4 22 17.6 71.6 62 49.6 143.6 102 81.6 215.6
-17 -13.6 1.4 23 18.4 73.4 63 50.4 145.4 103 82.4 217.4
-16 -12.8 3.2 24 19.2 75.2 64 51.2 147.2 104 83.2 219.2
-15 -12 5 25 20 77 65 52 149 105 84 221
-14 -11.2 6.8 26 20.8 78.8 66 52.8 150.8 106 84.8 222.8
-13 -10.4 8.6 27 21.6 80.6 67 53.6 152.6 107 85.6 224.6
-12 -9.6 10.4 28 22.4 82.4 68 54.4 154.4 108 86.4 226.4
-11 -8.8 12.2 29 23.2 84.2 69 55.2 156.2 109 87.2 228.2
-10 -8 14 30 24 86 70 56 158 110 88 230
-9 -7.2 15.8 31 24.8 87.8 71 56.8 159.8 111 88.8 231.8
-8 -6.4 17.6 32 25.6 89.6 72 57.6 161.6 112 89.6 233.6
-7 -5.6 19.4 33 26.4 91.4 73 58.4 163.4 113 90.4 235.4
-6 -4.8 21.2 34 27.2 93.2 74 59.2 165.2 114 91.2 237.2
-5 -4 23 35 28 95 75 60 167 115 92 239
-4 -3.2 24.8 36 28.8 96.8 76 60.8 168.8 116 92.8 240.8
-3 -2.4 26.6 37 29.6 98.6 77 61.6 170.6 117 93.6 242.6
-2 -1.6 28.4 38 30.4 100.4 78 62.4 172.4 118 94.4 244.4
-1 -0.8 30.2 39 31.2 102.2 79 63.2 174.2 119 95.2 246.2
0 0 32 40 32 104 80 64 176 120 96 248
1 0.8 33.8 41 32.8 105.8 81 64.8 177.8 121 96.8 249.8
2 1.6 35.6 42 33.6 107.6 82 65.6 179.6 122 97.6 252.6
3 2.4 37.4 43 34.4 109.4 83 66.4 181.4 123 98.4 253.4
4 3.2 39.2 44 35.2 111.2 84 67.2 183.2 124 99.2 255.2
5 4 41 45 36 113 85 68 185 125 100 257
6 4.8 42.8 46 36.8 114.8 86 68.8 186.8 126 100.8 258.8
7 5.6 44.6 47 37.6 116.6 87 69.6 188.6 127 101.6 260.6
8 6.4 46.4 48 38.4 118.4 88 70.4 190.4 128 102.4 262.4
9 7.2 48.2 49 39.2 120.2 89 71.2 192.2 129 103.2 264.2
10 8 50 50 40 122 90 72 194 130 104 266
11 8.8 51.8 51 40.8 123.8 91 72.8 195.8 131 104.8 267.8
12 9.6 53.6 52 41.6 125.6 92 73.6 197.6 132 105.6 269.6
13 10.4 55.4 53 42.4 127.4 93 74.4 199.4 133 106.4 271.4
14 11.2 57.2 54 43.2 129.2 94 75.2 201.2 134 107.2 273.2
15 12 59 55 44 131 95 76 203 135 108 275
16 12.8 60.8 56 44.8 132.8 96 76.8 204.8 136 108.8 276.8
17 13.6 62.6 57 45.6 134.6 97 77.6 206.6 137 109.6 278.6
18 14.4 64.4 58 46.4 136.4 98 78.4 208.4 138 110.4 280.4

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19 15.2 66.2 59 47.2 138.2 99 79.2 210.2 139 111.2 282.2

[Pg 231]
*Quantities of Alkali Required for Saponification of Fats of Average
Molecular Weight 670

(Cocoanut Oil, Palmkernel Oil)

Liters Alkali Liters Alkali Liters Alkali

Liters Alkali
Kilos Solution Sp. Gr. Solution Sp. Gr. Solution Sp. Gr.
Solution Sp. Gr. 1.1
1.2 1.3 1.355
NaOH KOH NaOH KOH NaOH KOH NaOH KOH
1000 1875.83 1902.99 844.67 930.35 510.27 622.71 409.61 517.97
2000 3751.66 3805.97 1689.35 1860.70 1020.64 1245.41 819.21 1035.95
3000 5627.50 5708.96 2534.02 2791.04 1530.81 1868.12 1228.82 1553.92
4000 7508.33 7611.94 3378.69 3721.39 2041.01 2490.83 1638.43 2071.90
5000 9379.16 9514.93 4223.37 4651.74 2551.35 3113.54 2048.04 2589.87
6000 11254.99 11417.91 5068.04 5582.09 3061.61 3736.24 2457.65 3107.84
7000 13130.82 13320.90 5912.71 6512.44 3571.88 4358.95 2867.26 3625.82
8000 15006.66 15223.88 6757.38 7442.78 4082.15 4981.66 3276.86 4143.79
9000 16882.49 17126.87 7602.06 8373.13 4592.42 5604.36 3886.47 4661.77
10000 18758.32 19029.85 8446.73 9303.48 5102.69 6227.02 4096.08 5179.74

*Quantities of Alkali Required for Saponification of Fats of Average

Molecular Weight 860

(Tallow, Cottonseed Oil, Olive Oil, Etc.)

Liters Alkali Liters Alkali Liters Alkali

Liters Alkali
Kilos Solution Sp. Gr. Solution Sp. Gr. Solution Sp. Gr.
Solution Sp. Gr. 1.1
1.2 1.3 1.355
NaOH KOH NaOH KOH NaOH KOH NaOH KOH
1000 1461.40 1482.56 658.05 724.81 397.54 485.13 319.11 403.54
2000 2922.81 2965.12 1316.12 1449.61 795.07 970.27 638.23 807.08
3000 4384.21 4447.67 1974.18 2174.42 1192.61 1455.40 957.34 1210.61
4000 5845.62 5930.23 2632.24 2899.22 1590.14 1940.53 1276.45 1614.15
5000 7307.02 7412.79 3290.80 3624.03 1987.68 2425.67 1595.57 2017.69
6000 8768.42 8895.85 3948.35 4348.84 2385.21 2910.80 1914.68 2421.23
7000 10229.83 10377.91 4606.41 5073.64 2782.75 3395.93 2233.79 2824.77
8000 11691.23 11860.45 5264.47 5798.45 3180.28 3881.06 2552.90 3228.30
9000 13152.64 13343.02 5922.53 6523.25 3577.82 4366.20 2872.02 3631.84
10000 14614.04 14825.58 6580.59 7248.06 3975.35 4851.33 3191.13 4035.38

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DENSITY AND STRENGTH OF SULPHURIC ACID (SIDERSKY). [Pg 232]

Degrees Sp. Gr. at % of pure acid Equivalent (in cc.) of Equivalent (in cc.) of
Twaddell. 15° C. (H2SO4). a kilo of pure acid. a liter of pure acid.
1 1.007 1.9 52.620 96.930
3 1.014 2.8 35.710 66.450
4 1.022 3.8 25.650 47.230
6 1.029 4.8 20.410 37.582
8 1.037 5.8 16.670 30.690
9 1.045 6.8 14.085 25.938
10 1.052 7.8 12.198 22.460
12 1.062 8.8 10.755 19.803
13 1.067 9.8 9.524 17.540
15 1.075 10.9 8.547 15.740
17 1.083 11.9 7.752 14.278
18 1.091 13.0 7.042 12.969
20 1.100 14.1 6.452 11.882
22 1.108 15.2 5.953 10.962
23 1.116 16.2 5.526 10.177
25 1.125 17.3 5.405 9.954
27 1.134 18.5 4.76 8.770
29 1.142 19.6 4.465 8.223
30 1.152 20.8 4.184 7.723
32 1.162 22.2 3.876 7.138
34 1.171 23.3 3.663 6.745
36 1.180 24.5 3.541 6.521
38 1.190 25.8 3.258 5.999
40 1.200 27.1 3.077 5.666
42 1.210 28.4 2.907 5.353
44 1.220 29.6 2.770 5.102
46 1.231 31.0 2.618 4.865
48 1.241 32.2 2.500 4.604
50 1.252 33.4 2.392 4.406
53 1.263 34.7 2.283 4.205
55 1.274 36.0 2.179 4.012
57 1.285 37.4 2.079 3.829
60 1.297 38.8 1.988 3.661
62 1.308 40.2 1.905 3.508
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64 1.320 41.6 1.821 3.354

66 1.332 43.0 1.745 3.214
69 1.345 44.4 1.665 3.085
71 1.357 45.5 1.621 2.985
74 1.370 46.9 1.558 2.869
77 1.383 48.3 1.497 2.757
80 1.397 49.8 1.436 2.646
82 1.410 51.2 1.386 2.551
85 1.424 52.6 1.335 2.459
88 1.438 54.0 1.287 2.370
91 1.453 55.4 1.237 2.270
94 1.468 56.9 1.195 2.200
97 1.483 58.3 1.156 2.130
100 1.498 59.6 1.116 2.050
103 1.514 61.0 1.080 1.980
106 1.530 62.5 1.045 1.930
108 1.540 64.0 1.010 1.860
113 1.563 65.5 0.975 1.800
116 1.580 67.0 0.950 1.740
120 1.597 68.6 0.917 1.690
123 1.615 70.0 0.888 1.630
127 1.634 71.6 0.855 1.570
130 1.652 73.2 0.845 1.520
134 1.671 74.7 0.800 1.470
138 1.691 76.4 0.774 1.430
142 1.711 78.1 0.749 1.390
146 1.732 79.9 0.722 1.320
151 1.753 81.7 0.705 1.280
155 1.774 84.1 0.672 1.235
160 1.798 86.5 0.639 1.190
164 1.819 89.7 0.609 1.120
168 1.842 100.0 0.544 1.000

[Pg 233]
*Densities of Potassium Carbonate Solutions at 15 C (Gerlach)

Per cent of
Sp. Gr. pure K2CO3

1.00914 1

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1.01829 2
1.02743 3
1.03658 4
1.04572 5
1.05513 6
1.06454 7
1.07396 8
1.08337 9
1.09278 10
1.10258 11
1.11238 12
1.12219 13
1.13199 14
1.14179 15
1.15200 16
1.16222 17
1.17243 18
1.18265 19
1.19286 20
1.20344 21
1.21402 22
1.22459 23
1.23517 24
1.24575 25
1.25681 26
1.26787 27
1.27893 28
1.28999 29
1.30105 30
1.31261 31
1.32417 32
1.33573 33
1.34729 34
1.35885 35
1.37082 36
1.38279 37
1.39476 38

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1.40673 39
1.41870 40
1.43104 41
1.44338 42
1.45573 43
1.46807 44
1.48041 45
1.49314 46
1.50588 47
1.51861 48
1.53135 49
1.54408 50
1.55728 51
1.57048 52
1.57079 53.024

*Constants of Certain Fatty Acids and Triglycerides

Per cent Yield

Triglycerides of Mol. Wt. Mol. Wt.
Fatty Acid Glycerine
of Fatty Acid of Triglycerides
Stearic Acid 284 890 95.73 10.34
Oleic Acid 282 884 95.70 10.41
Margaric Acid 270 848 95.52 10.85
Palmitic Acid 256 806 95.28 11.42
Myristic Acid 228 722 94.47 12.74
Lauric Acid 200 638 94.04 14.42
Capric Acid 172 594 93.14 15.48
Caproic Acid 116 386 90.16 23.83
Butyric Acid 88 302 87.41 30.46

[Pg 234]
PERCENTAGES OF SOLID CAUSTIC SODA AND CAUSTIC
POTASH IN CAUSTIC LYES ACCORDING TO BAUME SCALE.

Degrees Baumé. % NaOH % KOH

1 0.61 0.90
2 0.93 1.70
3 2.00 2.60
4 2.71 3.50

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5 3.35 4.50
6 4.00 5.60
7 4.556 6.286
8 5.29 7.40
9 5.87 8.20
10 6.55 9.20
11 7.31 10.10
12 8.00 10.90
13 8.68 12.00
14 9.42 12.90
15 10.06 13.80
16 10.97 14.80
17 11.84 15.70
18 12.64 16.50
19 13.55 17.60
20 14.37 18.60
21 15.13 19.50
22 15.91 20.50
23 16.77 21.40
24 17.67 22.50
25 18.58 23.30
26 19.58 24.20
27 20.59 25.10
28 21.42 26.10
29 22.64 27.00
30 23.67 28.00
31 24.81 28.90
32 25.80 29.80
33 26.83 30.70
34 27.80 31.80
35 28.83 32.70
36 29.93 33.70
37 31.22 34.90
38 32.47 35.90
39 33.69 36.90
40 34.96 37.80
41 36.25 38.90

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42 37.53 39.90
43 38.80 40.90
44 39.99 42.10
45 41.41 43.40
46 42.83 44.60
47 44.38 45.80
48 46.15 47.10
49 47.58 48.25
50 49.02 49.40

GLYCERINE CONTENT OF MORE COMMON OILS AND FATS

USED IN SOAP MAKING.

Theoretical
Yield Average % Pure
Yield Soap Lye
of Pure Free Fatty Acid Glycerine
Kind. 80% Crude
Glycerine in Commercial in Commercial
Glycerine.
of Neutral Oil or Oil. Oil.
Fat.
Beef Tallow 10.7 5 10.2 12.75
Bone Grease 10.5 20-50 5.2- 8.4 6.5 -10.5
Castor Oil 9.8 0.5-10 8.8- 9.8 11.0 -12.45
Cocoanut Oil 13.9 3-5 13.2-13.5 16.5 -16.9
Cocoanut Oil
15-40 8.3-11.8 10.37-14.75
Off
Corn Oil 10.4 1-10 9.3-10.3 11.62-12.9
Cottonseed
10.6 Trace 10.6 13.25
Oil
Hog Grease 10.6 0.5-1 10.5-10.6 13.12-13.25
Horse Grease 10.6 1-3 10.5-10.6 13.12-13.25
Olive Oil 10.3 2-25 7.7-10.2 9.62-12.75
Olive Foots 30-60 4-7 5- 8.75
Palm Oil 11.0 10-50 5.5-10 6.87-12.5
Palmkernel
13.3 4-8 12.2-12.8 15.25-16
Oil
Peanut Oil 10.4 5-20 8.3- 9.9 10.37-12.37
Soya Bean Oil 10.4 2 10.2 12.75
Train Oil 10.0 2-20 8- 9.8 10.0 -12.25
Vegetable
10.9 1-3 10.5-10.8 13.12-13.5
Tallow

[Pg 235]

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*Table of Specific Gravities of Pure Commercial Glycerine with

Corresponding Percentage of Water. Temperature 15 C.

Sp. Gr. % Water Sp. Gr. % Water

1.262 0 1.160 38
1.261 1 1.157 39
1.258 2 1.155 40
1.255 3 1.152 41
1.2515 4 1.149 42
1.250 5 1.1464 43
1.2467 6 1.1437 44
1.2450 7 1.141 45
1.243 8 1.1377 46
1.241 9 1.1353 47
1.237 10 1.1326 48
1.235 11 1.1304 49
1.2324 12 1.127 50
1.229 13 1.125 51
1.2265 14 1.1224 52
1.2245 15 1.1204 53
1.2225 16 1.117 54
1.2185 17 1.114 55
1.2174 18 1.112 56
1.2142 19 1.109 57
1.211 20 1.106 58
1.207 21 1.103 59
1.203 22 1.1006 60
1.2004 23 1.088 65
1.198 24 1.075 70
1.195 25 1.0623 75
1.1923 26 1.049 80
1.189 27 1.0365 85
1.188 28 1.0243 90
1.1846 29 1.0218 91
1.182 30 1.0192 92
1.179 31 1.0168 93
1.176 32 1.0147 94
1.1734 33 1.0125 95
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1.171 34 1.01 96
1.168 35 1.0074 97
1.165 36 1.0053 98
1.163 37 1.0026 99

[Pg 236]
Table of Percentage, Specific Gravity and Beaume Degree of Pure
Glycerine Solutions

Sp. Gr. Degree Sp. Gr. Degree

Per cent Per cent
Champion and Beaumé Champion and Beaumé
Water Water
Pellet (Berthelot) Pellet (Berthelot)
0 1.2640 31.2 11.0 1.2350 28.6
0.5 1.2625 31.0 11.5 1.2335 28.4
1.0 1.2612 30.9 12.0 1.2322 28.3
1.5 1.2600 30.8 12.5 1.2307 28.2
2.0 1.2585 30.7 13.0 1.2295 28.0
2.5 1.2575 30.6 13.5 1.2280 27.8
3.0 1.2560 30.4 14.0 1.2270 27.7
3.5 1.2545 30.3 14.5 1.2255 27.6
4.0 1.2532 30.2 15.0 1.2242 27.4
4.5 1.2520 30.1 15.5 1.2230 27.3
5.0 1.2505 30.0 16.0 1.2217 27.2
5.5 1.2490 29.9 16.5 1.2202 27.0
6.0 1.2480 29.8 17.0 1.2190 26.9
6.5 1.2465 29.7 17.5 1.2177 26.8
7.0 1.2455 29.6 18.0 1.2165 26.7
7.5 1.2440 29.5 18.5 1.2150 26.5
8.0 1.2427 29.3 19.0 1.2137 26.4
8.5 1.2412 29.2 19.5 1.2125 26.3
9.0 1.2400 29.0 20.0 1.2112 26.2
9.5 1.2390 28.9 20.5 1.2100 26.0
10.0 1.2375 28.8 21.0 1.2085 25.0
10.5 1.2362 28.7

[Pg 237]
*Table of Specific Gravities of Pure Glycerine Solutions with
Corresponding Beaume Degree and Percent Water

Per cent Water Sp. Gr. Degree Beaume Per cent Water Sp. Gr. Degree Beaume
0.0 1.2640 31.2 1.0 1.2612 30.9
0.5 1.2625 31.0 1.5 1.2600 30.8
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2.0 1.2585 30.7 12.0 1.2322 28.3

2.5 1.2575 30.6 12.5 1.2307 28.2
3.0 1.2560 30.4 13.0 1.2295 28.0
3.5 1.2545 30.3 13.5 1.2280 27.8
4.0 1.2532 30.2 14.0 1.2270 27.7
4.5 1.2520 30.1 14.5 1.2255 27.6
5.0 1.2505 30.0 15.0 1.2242 27.4
5.5 1.2490 29.9 15.5 1.2230 27.3
6.0 1.2480 29.8 16.0 1.2217 27.2
6.5 1.2465 29.7 16.5 1.2202 27.0
7.0 1.2455 29.6 17.0 1.2190 26.9
7.5 1.2440 29.5 17.5 1.2177 26.8
8.0 1.2427 29.3 18.0 1.2165 26.7
8.5 1.2412 29.2 18.5 1.2150 26.5
9.0 1.2400 29.0 19.0 1.2137 26.4
9.5 1.2390 28.9 19.5 1.2125 26.3
10.0 1.2375 28.8 20.0 1.2112 26.2
10.5 1.2362 28.7 20.5 1.2100 26.0
11.0 1.2350 28.6 21.0 1.2085 25.9
11.5 1.2335 28.4

[Pg 239]

INDEX
A

Acetin process for the determination of glycerol, 155.

Acid, Clupanodonic, 20.

Acid, Hydrochloric, 111.

Acid, Lauric, 2.

Acid, Myristic, 2.

Acid, Napthenic, 24.

Acid, Oleic, 15, 19.

Acid, Palmitic, 2.

Acid, Pinic, 22.

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Acid, Resin, 144.

Acid, Stearic, 15, 19.

Acid, Sulfuric, 112.

Acid, Sylvic, 22.

Acid saponification, 120.

Air bleaching of palm oil, 12.

Albuminous matter, Removal from tallow, 6.

Alcohol, Denatured, 82.

Alcoholic method for free alkali in soap, 139.

Alkali Blue 6 B, indicator, 129.

Alkali, Total, determination of in soap, 147.

Alkalis, 25.

Alkalis used in soap making,

Testing of, 134.

Amalgamator, 33.

Analysis, Glycerine, International, 150.

Analysis, Soap, 137.

Analysis, Standard methods for fats and oils, 165-196.

Aqueous saponification, 121.

Arachis oil, 79.

Autoclave saponification, 118.

Automobile soaps, 41.

Barrels, sampling, 168.

Baumé scale, 25.

Bayberry wax, Use in shaving soap, 89.

Bichromate Process for glycerol determination, 160.

Bleaching, Fullers' earth process for tallow, 4.

Bleaching palm oil by bichromate method, 9.

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Bleaching palm oil by air, 12.

Bosshard & Huggenberg method for determination of free alkali, 140.

Bunching of soap, 52.

Candelite, 96.

Candle tar, 125.

Carbolic soap, 77.

Carbon Dioxide, Formation of in carbonate saponification, 45.

Carbonate, potassium, 29.

Carbonate, saponification, 35, 45.

Carbonate, sodium, 28.

Castile soap, 79.

Castor oil ferment, 121.

Castor oil, Use of in transparent soaps, 83.

Caustic potash, 26.

Caustic potash, Electrolytic, 27.

Caustic soda, 26.

Changes in soap-making, 36.

Chemist, Importance of, 127.

Chipper, Soap, 32.

Chip soap, 54.

Chip soap, Cold made, 55.

Chip soap, Unfilled, 56.

Chrome bleaching of palm oil, 9.

Cloud test for oil, Standard method, 182-183.

Clupanodonic acid, 20.

Cocoanut oil, 6.

Cold cream soap, 78.

Cold made chip soaps, 55.

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Cold made toilet soaps, 72.

Cold made transparent soaps, 84.

Cold process, 35, 43.

Colophony, 22.

Coloring soap, 75.

Copra, 7.

Corn oil, 14.

Corrosive sublimate, 78.

Cotton goods. Soaps used for, 103.

Cottonseed oil, 14.

Cream, Shaving, 90.

Crude glycerine, 113.

Crutcher, 32.

Curd soap, 71.

Cutting table, 32. [Pg 240]

Determination of free fatty acid, 128.

Determination of unsaponifiable matter, 132.

Distillation of fatty acids, 125.

Drying machine, 32.

Enzymes, 17.

Eschweger soap, 81.

Examination of fats and oils, 128.

Fahrion's method for moisture, 138.

Fats and oils, Examination of, 128.

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Fats and oils used in soap manufacture, 3.

Fatty acids, 14.

Fatty acids, Distillation of, 125.

Ferments, Splitting fats with, 121.

Fillers for laundry soaps, 53.

Fillers for soap powders, 58.

Finishing change, 36.

Fish oils, 20.

Floating soap, 62.

Formaldehyde soap, 78.

Frames, 31.

Free alkali in soap, Determination of, 139.

Free fatty acid, Determination of, 128.

Free fatty acids, Extraction from tallow, 6.

Free fatty acid, Standard method of dilu., 174.

Note on method, 188-189.

Full boiled soaps, 35.

Fullers' earth bleaching of tallow, 4.

Glycerides, 2.

Glycerine, 2.

Glycerine analysis, 150.

Glycerine change, 36.

Glycerine, Crude, 113.

Glycerine in spent lyes, Recovery of, 106.

Glycerine in soap, Determination of, 149.

Glycerine, Sampling crude, 162.

Glycerine soaps, 83.

Glycerol content, Ways of calculating actual, 159.

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Glycerol determination, Acetin process, 155.

Glycerol determination, Bichromate process for, 160.

Graining soap, 30.

Grease, 21.

Grease, Bleaching, 21.

Grinding soap, 34.

Hand Paste, 93.

Hard water, 29.

Hardened oils in toilet soap, Use of, 96.

Hydrocarbon oils, 2.

Hydrogenating oils, 19.

Hydrolysis of fats and oils, 17.

Hydrolytic dissociation of soap, 1.

Hydrometers, 25.

Indicators, Action, 135-6.

Insoluble impurities in fatty oils, Determination of (standard method) 172.

Note on method 187.

Insoluble matter in soap, determination of, 143.

International committee on glycerine analysis, 150.

Iodine manufacturing oil, 191.

Iodine member Wijs method, Standard, 177-181. Note on method, 191.

Iodine soap, 78.

Joslin, ref., 113.

"Killing" change, 36.

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Koettstorfer number (Standard method), 181-182.

Kontakt reagent, 117.

Krebitz Process, 123.

Krutolin, 96.

Leiste & Stiepel method for rosin in soap, 146.

Liebermann, Storch reaction, 144. [Pg 241]

Light powders, 60.

Laundry soap, 48.

LeBlanc Process, 28.

Lewkowitsch, ref., 17, 146.

Lime saponification, 118.

Lime, Use in Krebitz Process, 123.

Lime, Use in treatment of glycerine water, 116.

Liquid medicinal soaps, 79.

Liquid soaps, 94.

Lyes, Spent, 37.

Magnesia, Use in autoclave saponification, 120.

Manganese sulfate, Use of as catalyzer in fermentative cleavage of fats, 122.

Marine soaps, 39.

Medicinal soaps, 76.

Medicinal soaps, Less important, 78.

Medicinal soaps, Therapeutic value of, 76.

Melting point of fat or oil, Standard method, 193.

Mercury soaps, 78.

Metallic soaps, 1.

Methyl orange, indicator, 136.

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Meyerheim, ref., 21.

Mill soap, 32.

Moisture in soap, Determination of, 138, 130.

Moisture and volatile matter in fats and oils, Standard method for detm. of, 170.
Note on method, 184-185.

Mottle in soap, 81.

Mug shaving soap, 90.

Naphtha, Incorporation in soap, 49.

Naphthenic acids, 24.

Nigre, 36.

Normal acids, Equivalent in alkalis, 136.

Oils and fats, 1.

Oils and fats, Chemical constants, 18.

Oils and fats, Distinction, 1.

Oils and fats, Preserving, 18.

Oils and fat, Nature of used in soap manufacture, 2.

Oils and fats, Rancidity of, 16.

Oil hardening, 19.

Oleic acid, 15, 19.

Olein, 2, 19.

Olive oil, 14.

Olive oil foots, 14.

Organoleptic methods, 127.

Palmatin, 2.

Palm kernel oil, 8.

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Palmitic acid, 2.

Palm oil, 8.

Palm oil, air bleaching, 12.

Palm oil, Chrome bleaching of, 9.

Palm oil soap, 66.

Pearl ash, 29.

Perfuming and coloring toilet soaps, 73.

Peroxide soap, 78.

Petroff reagent, 117.

Pfeilring reagent, 117.

Phenol, 77.

Phenolphthalein, indicator, 38.

Phenolphthalein, Using as indicator, 51.

Phenols, Soaps containing, 77.

Pinic acid, 22.

Plodder, 33.

Potash from wood ash, 27.

Potassium carbonate, 29.

Powders, Light, 60.

Powders, Scouring, 61.

Powders, Shaving, 90.

Powders, Soap, 56.

Precipitation test for treated spent lyes, 110.

Prevention of rancidity, 18.

Pumice or sand soaps, 93.

Purple shade in soap, 75.

Rancidity of oils and fats, 16.

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Rancidity, Prevention, 18.

Recovery of glycerine from spent lye, 106.

Red oil, 15.

Red oil, Saponified, 15.

Resin acids, Total fatty and, Determination of in soap, 144.

Ribot, ref., 20.

Rosin, 22. [Pg 242]

Rosin, Determination of in soap, 144.

Rosin saponification, 23.

Run and glued up soaps, 69.

Run soaps, 39.

Sal soda, 29.

Salt, 30.

Salting out, 30.

Salt "pickle," 37.

Sampling crude glycerine, 162.

Sampling for standard method, 166. Note on, 184.

Sampling oils and fats, 128.

Sampling soap, 137.

Saponification by ferments, 121.

Saponification, Acid, 120.

Saponification, Aqueous, 121.

Saponification, Autoclave, 118.

Saponification, Carbonate, 45.

Saponification defined, 2, 105.

Saponification, Lime, 118.

Saponification number, 181-182.

Saponification, Rosin, 23.

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Saponification, Various methods, 105.

Scouring and fulling soaps for wool, 98.

Scouring powders, 61.

Scouring soap, 61.

Semi-boiled laundry soaps, 49.

Semi-boiled process, 44.

Shaving cream, 90.

Shaving powder, 90.

Shaving soaps, 87.

Silica and silicates, Determination of in soap, 148.

Silk dyeing, 102.

Silk industry, Soaps used in, 101.

Slabber, 32.

Smith method for moisture in soap, 138.

Soap analysis, 137.

Soap, Automobile, 41.

Soap, Carbolic, 71.

Soap, Castile, 79.

Soap, Chip, 54.

Soap Chip, cold made, 55.

Soap, Chip, unfilled, 56.

Soap, Cold cream, 78.

Soap, Coloring, 75.

Soap containing phenols, 77.

Soap, Curd, 71.

Soap, Defined, 1.

Soap, Determination insoluble matter, 143.

Soap, Determining glycerine in, 149.

Soap, Eschweger, 81.

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Soap, Floating, 62.

Soap, Formaldehyde, 78.

Soap for wool, Scouring and fulling, 98.

Soap, Full boiled, 35.

Soap, Iodine, 78.

Soap kettle, 31.

Soap, Laundry, 48.

Soap, Liquid, 94.

Soap lye crude glycerine, 113.

Soap, Marine, 39.

Soap, Medicinal, 76.

Soap, Medicinal, less important, 78.

Soap, Mercury, 78.

Soap, Metallic, 1.

Soap, Peroxide, 78.

Soap powders, 56.

Soap, Pumice or sand, 93.

Soap, Rosin settled, 50.

Soap, Run and glued up, 69.

Soap, Scouring, 61.

Soap, Semi-boiled laundry, 49.

Soap, Shaving, 87.

Soap, Sulphur, 77.

Soap, Tannin, 78.

Soap, Tar, 77.

Soap, Test for color of, 133.

Soap, Textile, 98.

Soap, Toilet, 65.

Soap, Toilet cheaper, 68.

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Soap, Toilet, cold made, 72.

Soap, Toilet perfuming and coloring, 73.

Soap, Transparent, 82.

Soap, Transparent, cold made, 84.

Soap used for cotton goods, 103.

Soap used in the silk industry, 101.

Soap, Witch hazel, 78.

Soap, Wool thrower's, 100.

Soap, Worsted finishing, 101.

Soda ash, 28.

Sodium carbonate, 28.

Sodium perborate, Use of in soap powders, 57.

Soft soaps, 40.

Soluble mineral matter detm. of in fats and oils, 173.

Note on method, 187-188. [Pg 243]

Solvay process, 28.

Soya bean oil, 14.

Spent lye, Recovery of glycerine from, 106.

Spent lyes, 37.

Spent lyes, Treatment of for glycerine recovery, 107.

Splitting fats with ferments, 121.

Standard methods of analysis for fats and oils, 165-196.

Starch and gelatine, Determination in soap, 143.

Stearic acid, 15, 19.

Stearin, 2, 19.

Strengthening change, 36.

Strengthening lyes, 38.

Strunz crutcher, 63.

Sugar in soap, Determination of, 150.

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Sugar, Use in transparent soap, 83.

Sulfate of alumina, Use of in spent lyes, 108.

Sulphonated oils, 104.

Sulphur soaps, 77.

Sweating of soap, 62.

Sweet water, 119.

Sylvic acid, 22.

Talgol, 96.

Tallow, 4.

Tallow, Fullers' earth bleaching of, 4.

Tallow, Improving color by extraction of free fatty acid, 6.

Tannin soap, 78.

Tar soap, 77.

Test for color of soap, 133.

Testing of alkalis used in soap making, 134.

Textile soaps, 98.

Titer, 130.

Tank cars, Sampling, 166.

Tierces, Sampling, 168.

Titer, Standard method, 175.

Titer, Note on, 189.

Tung oil, Note one iodine, number of, 180.

Toilet soap, 65.

Toilet soaps, Cheaper, 68.

Toilet soap, Use of hardened oils in, 96.

Total alkali, Determination of in soap, 147.

Total fatty and resin acids, Determination of in soap, 144.

Train oils, 20.

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Transparent soap, 82.

Transparent soap, Cold made, 84.

Troweling soap, 52.

Tsujimoto, ref., 20.

Tubes for transparent soap, 85.

Turkey red oil, 104.

Twaddle scale, 25.

Twitchell method for rosin, 145.

Twitchell process, 113.

Twitchell process, Advantages, 113.

Unsaponifiable matter, Determination of in oils and fats, 132.

Unsaponifiable matter, Determination of in soap, 148.

Unsaponifiable matter, determination of by standard method, 176.

Vacuum Oven, Standard, 176.

Vegetable oils, 6.

Water, 29.

Water, Hard, 29.

Witch hazel soap, 78.

Wool thrower's soap, 100.

Worsted finishing soaps, 101.

Zinc oxide, Use of in autoclave saponification, 120.

Zinc oxide, Use of in soap, 33.

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LITERATURE OF THE CHEMICAL INDUSTRIES

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A list of standard books relating to soapmaking and allied industries.
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Askinson, George W. Perfumes and Cosmetics. Their preparation and manufacture.
Fourth Edition, translated from the German, and revised with additions by W. L. Dudley.
32 illustrations. 6-1/4 × 9-1/2. Cloth. 354 pp. New York, 1915. $5.00
Chalmers, T. W. The Production and Treatment of Vegetable Oils. Including chapters on
the refining of oils, the hydrogenation of oils, the generation of hydrogen, soap making,
the recovery and refining of glycerine, and the splitting of oils. 95 illustrations, 9 folding
plates. 8 × 11-1/2. Cloth. 163 pp. London, 1919. $7.50
Deite, C. Manual of Toilet Soap-Making. Comprising toilet soaps, medicated soaps, and
other specialties. Second Revised Edition. 85 illustrations. 6-1/2 × 10. Cloth. 356 pp.
London, 1920. $7.50
Ellis, Carleton G. The Hydrogenation of Oils, Catalyzers and Catalysis and the
Generation of Hydrogen and Oxygen. Second Edition, thoroughly revised and enlarged.
240 illustrations. 6-1/4 × 9-1/2. Cloth. 767 pp. N. Y., 1919. $7.50
Fischer, M. H. Soaps and Proteins, Their Colloid Chemistry in Theory and Practice.
With the collaboration of G. D. McLaughlin and M. O. Hooker. 114 illustrations. 6 × 9-
1/4. Cloth. 281 pp. New York, 1921. $4.00
Holde, D. The Examination of Hydrocarbon Oils, and of the Saponifiable Fats and
Waxes. Translated from the Fourth German Edition by Edward Mueller. 115 illustrations.
6-1/4 × 9-1/4. Cloth. 499 pp. N. Y., 1915. Net, $5.00
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Hurst, G. H. Soaps. A practical manual of the manufacture of domestic, toilet and other
soaps. Second Edition. 66 illustrations. 6 × 8-3/4. Cloth. 385 pp. London, 1907. $6.00
Hurst, George H., and Simmons, W. H. Textile Soaps and Oils. A handbook on the
preparation, properties, and analysis of the soaps and oils and in textile manufacturing,
dyeing and printing. Third Edition, revised. 12 illustrations. 5-1/2 × 8-3/4. Cloth. 212 pp.
London, 1921. $4.00
Koller, T. Cosmetics. A handbook of the manufacture, employment, and testing of all
cosmetic materials and cosmetic specialties, with numerous recipes. Translated from the
German. Third Edition. 5 × 7-1/2. Cloth. 264 pp. London, 1920. $3.50
Koppe, S. W. Glycerine. Its introduction, Uses and Examination. For chemists,
perfumers, soapmakers, pharmacists, and explosives technologists. 7 illustrations. 5-1/4 ×
7-1/2. Cloth. 260 pp. New York, 1915. $3.50
Lamborn, L. L. Modern Soaps, Candles, and Glycerin. A practical manual of modern
methods of utilization of fats and oils in the manufacture of soaps and candles, and the
recovery of glycerin. 228 illustrations. 6-1/2 × 9-1/4. Cloth. 708 pp. N. Y., 1906. $10.00
Murray, B. L. Standards and Tests for Reagent Chemicals. 6 × 9. Cloth. 400 pp. New
York, 1920. $3.00
Parry, Ernest J. The Chemistry of Essential Oils and Artificial Perfumes. Vol. I,
Monographs on Essential Oils. Fourth Edition, revised and enlarged. 51 illustrations. 6-
1/4 × 10. Cloth. 557 pp. London, 1921. $9.00
Vol. II. Constituents of Essential Oils, Synthetic Perfumes and Isolated Aromatics, and
the Analysis of Essential Oils. Third Edition, revised and enlarged. Illustrated. 351 pp.
London, 1919. $7.00
Partington, J. R. The Alkali Industry. 63 illustrations. 5-1/2 × 8-1/2. Cloth. 318 pp.
London, 1918. $3.00
Rogers, Allen. Industrial Chemistry. A manual for the student and manufacturer. Third
Edition, thoroughly revised and enlarged. 377 illustrations. 6-1/2 × 9-3/4. Flexible
fabrikoid. 1255 pp. New York, 1920. $7.50
Scott, Wilfred W. (Editor). Standard Methods of Chemical Analysis. A manual of
analytical methods and general reference for the analytical chemist and for the advanced
student. Second Edition, revised, with additional tables. 142 illustrations, 3 color plates. 7
× 9-1/4. Cloth. 900 pp. N. Y., 1917. $7.50
Simmons, W. H. Fats, Waxes and Essential Oils. In Press.
Simmons, William H. Soap. Its composition, manufacture and properties. 11
illustrations. 4-3/4 × 7-1/4. Cloth. 133 pp. London, 1916. $1.00
Simmons, W. H., and Appleton, H. A. The Handbook of Soap Manufacture. 27
illustrations. 6 × 9. Cloth. 166 pp. London, 1908. $4.00
Van Nostrand's Chemical Annual. Edited by John C. Olsen. A handbook of useful data
for analytical manufacturing and investigating chemists and chemical students. Fourth
Issue, enlarged. 5 × 7-1/2. Flexible fabrikoid. 785 pp. New York, 1918. $3.00
Watt, A. Art of Soapmaking. A practical handbook of the manufacture of hard and soft
soaps, toilet soaps, etc. Seventh Edition, revised and enlarged. 43 illustrations. 5-1/4 × 7-
1/2. Cloth. 323 pp. London, 1918. $4.00
Wright, C. R. A. Animal and Vegetable Fixed Oils, Fats, Butters, and Waxes: Their
Preparation and Properties, and the Manufacture Therefrom of Candles, Soaps, and Other
Products. Third Edition, revised and greatly enlarged by C. Ainsworth Mitchell. 185
illustrations, 3 plates. 6 × 9. Cloth. 953 pp. London, 1921. $16.50
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