In the preparation of this reagent the petroleum ether of commerce,
containing bodies boiling at temperatures of from 35° to 80°, is
repeatedly fractioned by distillation until a product is obtained
which boils at from 45° to 60°. The distillation of this material
is conducted in a large flask heated with steam, furnished with a
column containing a number of separatory funnels and connected with an
appropriate condenser. The distillate is secured in a bottle packed
with broken ice, as shown in Fig. 80. A thermometer suspended in the
vapor of the petroleum serves to regulate the process. Too much care
to avoid accidents cannot be exercised in this operation. Not only
must steam be used in heating, but all flame and fire must be rigidly
excluded from the room in which the distillation takes place, and
the doors leading to other rooms where gas jets may be burning must
be kept closed. In the beginning of the process, as much as possible
of the petroleum boiling under 45° must be removed and rejected. The
distillation is then continued until the temperature rises above 60°.
The parts of the distillate saved between these temperatures are
redistilled under similar conditions. Other portions of the petroleum,
boiling at other temperatures, may be secured in the same way. The
products may be in a measure freed of unpleasant odors by redistilling
them from a mixture with lard. When used for quantitive purposes the
petroleum ether must leave no residue when evaporated at 100°.
[Illustration: FIG. 80.—APPARATUS FOR FRACTIONAL DISTILLATION OF
PETROLEUM ETHER.]
=281. Freeing Extracted Oils from Petroleum.=—The petroleum ether which
is used for extracting oils tends to give them an unpleasant odor and
flavor and its entire separation is a matter of some difficulty. The
greater part of the solvent may be recovered as described in paragraph
=43=. Heating the extracted oil for several hours in thin layers, will
remove the last traces of the solvent, but affords opportunity for
oxidation, especially in the case of drying oils. An effective means
of driving off the last traces of petroleum is to cause a current of
dry carbon dioxid to pass through the sample contained in a cylinder
and heated to a temperature of from 85° to 90°. The atmosphere of the
inert gas will preserve the oil from oxidation and the sample will,
as a rule, be found free of the petroleum odor after about ten hours
treatment. Ethyl ether or chloroform may be used instead of petroleum,
but these solvents act on other matters than the glycerids, and the
extract is therefore liable to be contaminated with more impurities
than when the petroleum ether is employed. Other solvents for fats
are carbon tetrachlorid, carbon disulfid, and benzene. In general,
petroleum ether should be employed in preference to other solvents,
except in the case of castor oil, which is difficultly soluble in both
petroleum and petroleum ethers.
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