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
(_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 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 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 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 160deg. C.
NOTES.
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