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
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 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 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.
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