Nitro-Explosives: A Practical TreatiseSanford, P. Gerald (Percy Gerald)
Science
Nitro-Explosives: A Practical Treatise
Sanford, P. Gerald (Percy Gerald)
Celluloid; Explosives
The organic acids, formic and butyric acids may be detected by heating a
sample of the glycerine in a test tube with alcohol and sulphuric acid,
when, if present, compound ethers, such as ethylic formate and butyrate,
the former smelling like peaches and the latter of pine-apple, will be
formed.
~Oleic Acid~, if present in large quantity, will come down upon diluting
the sample with water, but smaller quantities may be detected by passing a
current of nitrogen peroxide, N_{2}O_{4} (obtained by heating lead
nitrate), through the diluted sample, when a white flocculent precipitate
of elaidic acid, which is less soluble than oleic acid, will be thrown
down. By agitating glycerol with chloroform, fatty acids, rosin oil, and
some other impurities are dissolved, while certain others form a turbid
layer between the chloroform and the supernatant liquid. On separating the
chloroform and evaporating it to dryness, a residue is obtained which may
be further examined.
~Sodium Chloride~ can be determined in 100 c.c. of the glycerine by adding
a little water, neutralised with sodium carbonate, and then titrated with
a deci-normal solution of silver nitrate, using potassium chromate as
indicator.
~Organic Impurities~ of various kinds occur in crude glycerine, and are
mostly objectionable. Their sum may be determined with fair accuracy by
Sulman and Berry's method: 50 grms. of the sample are diluted with twice
its measure of water, carefully neutralised with acetic acid, and warmed
to expel carbonic acid; when cold, a solution of basic lead acetate is
added in slight but distinct excess, and the mixture well agitated. The
formation of an abundant precipitate, which rapidly subsides, is an
indication of considerable impurity in the sample. To ascertain its
amount, the precipitate is first washed by decantation, and then collected
on a tared, or preferably a double counter-poised filter, where it is
further washed, dried at 100 deg. to 105 deg. C., and weighed. The precipitate and
filter paper are then ignited separately in porcelain, at a low red heat,
the residues moistened with a few drops of nitric acid and reignited; the
weight of the lead oxide deducted from that of the original precipitate
gives the weight of the organic matter precipitated by the lead. Raw
glycerines contain from 0.5 to 1.0 per cent.
~Albuminous Matters.~ An approximate determination of the albuminous
matters may be made by precipitating with basic lead acetate as already
described, and determining the nitrogen by the Kjeldahl method; the
nitrogen multiplied by 6.25 gives the amount of albuminous matter in the
precipitate.
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