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
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. 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 Huebl 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:
Weigh out 0.15 +- 0.05 g., use an excess of 55 +- 3 per cent Wijs
solution. Conduct the absorption at a temperature of 20-25deg. 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.
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