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
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
Na_{2}CO_{3} to NaCl. The corrected weight multiplied by 100 gives the
percentage of _total residue at 160deg. 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 160deg.
C. Report as organic residue at 160deg. C. (it should be noted that
alkaline salts of fatty acids are converted to carbonates on ignition
and that the CO_{3} thus derived is not included in the organic
residue).
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.
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.
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