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
_Alcoholic Potassium Hydroxide Solution_--Dissolve 40 g. of pure
potassium hydroxide in one liter of 95 per cent redistilled alcohol (by
volume). The alcohol should be redistilled from potassium hydroxide over
which it has been standing for some time, or with which it has been
boiled for some time, using a reflux condenser. The solution must be
clear and the potassium hydroxide free from carbonates.
DETERMINATION--Weigh accurate about 5 g. of the filtered sample into a
250 to 300 cc. Erlenmeyer flask. Pipette 50 cc. of the alcoholic
potassium hydroxide solution into the flask, allowing the pipette to
drain for a definite time. Connect the flask with an air condenser and
boil until the fat is completely saponified (about 30 minutes). Cool and
titrate with the _N_/2 hydrochloric acid, using phenolphthalein as an
indicator. Calculate the Koettstorfer number (mg. of potassium hydroxide
required to saponify 1 g. of fat). Conduct 2 or 3 blank determinations,
using the same pipette and draining for the same length of time as
above.
MELTING POINT.
APPARATUS--_Capillary tubes_ made from 5 mm. inside diameter thin-walled
glass tubing drawn out to 1 mm. inside diameter. Length of capillary
part of tubes to be about 5 cm. Length of tube over all 8 cm.
_Standard thermometer_ graduated in tenths of a degree.
_600 cc. beaker._
DETERMINATION--The sample should be clear when melted and entirely free
from moisture, or incorrect results will be obtained.
Melt and thoroughly mix the sample. Dip three of the capillary tubes
above described in the oil so that the fat in the tube stands about 1
cm. in height. Now fuse the capillary end carefully by means of a small
blast flame and allow to cool. These tubes are placed in a refrigerator
over night at a temperature of from 40 to 50deg. F. They are then
fastened by means of a rubber band or other suitable means to the bulb
of a thermometer graduated in tenths of a degree. The thermometer is
suspended in a beaker of water (which is agitated by air or other
suitable means) so that the bottom of the bulb of the thermometer is
immersed to a depth of about 3 cm. The temperature of the water is
increased gradually at the rate of about 1deg. per minute.
The point at which the sample becomes opalescent is first noted and the
heating continued until the contents of the tube becomes uniformly
transparent. The latter temperature is reported as the melting point.
Before finally melting to a perfectly clear fluid, the sample becomes
opalescent and usually appears clear at the top, bottom, and sides
before becoming clear at the center. The heating is continued until the
contents of the tube become uniformly clear and transparent. This
temperature is reported as the melting point.[33] It is usually only a
fraction of a degree above the opalescent point noted. The thermometer
should be read to the nearest 1/2deg. C., and in addition this
temperature may be reported to the nearest degree Fahrenheit if desired.
CLOUD TEST.
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