Soap-Making Manual: A Practical Handbook on the Raw Materials, Their Manipulation, Analysis and Control in the Modern Soap Plant.Thomssen, Edgar George
Science
Soap-Making Manual: A Practical Handbook on the Raw Materials, Their Manipulation, Analysis and Control in the Modern Soap Plant.
Thomssen, Edgar George
Soap
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 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 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.
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.
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