Nitro-Explosives: A Practical TreatiseSanford, P. Gerald (Percy Gerald)
Science
Nitro-Explosives: A Practical Treatise
Sanford, P. Gerald (Percy Gerald)
Celluloid; Explosives
~The Determination of Glycerine.~ The acetin method of Benedikt and Canton
depends upon the conversion of glycerine into triacetin, and the
saponification of the latter, and reduces the estimation of glycerine to
an acidmetric method. About 1.5 grm. of crude glycerine is heated to
boiling with 7 grms. of acetic anhydride, and 3 to 4 grms. of anhydrous
sodium acetate, under an upright condenser for one and a half hours. After
cooling, 50 c.c. of water are added, and the mixture heated until all the
triacetin has dissolved. The liquid is then filtered into a large flask,
the residue on the filter is well washed with water, the filtrate quite
cooled, phenolphthalein is added and the fluid exactly neutralised with a
dilute (2 to 3 per cent.) solution of alkali. Twenty-five c.c. of a 10 per
cent. caustic soda solution, which must be accurately standardised upon
normal acid, are then pipetted into the liquid, which is heated to boiling
for ten minutes to saponify the triacetin, and the excess of alkali is
then titrated back with normal acid. One c.c. of normal acid corresponds
to .03067 grm. of glycerine.
~Precautions.~--The heating must be done with a reflux condenser, the
triacetin being somewhat volatile. The sodium acetate used must be quite
anhydrous, or the conversion of the glycerine to triacetyl is imperfect.
Triacetin in contact with water gradually decomposes. After acetylation is
complete, therefore, the operations must be conducted as rapidly as
possible. It is necessary to neutralise the free acetic acid very
cautiously, and with rapid agitation, so that the alkali may not be
locally in excess.
~The Lead Oxide Method.~--Two grms. of sample are mixed with about 40
grms. of pure litharge, and heated in an air bath to 130 deg. C. until the
weight becomes constant, care being taken that the litharge is free from
such lead compounds and other substances as might injuriously affect the
results, and that the heating of the mixture takes place in an air bath
free from carbonic acid. The increase in weight in the litharge, minus the
weight of substance not volatilisable from 2 grms. of glycerine at 160 deg.
C., multiplied by the factor 1.243, is taken as the weight of glycerine in
the 2 grms. of sample. The glycerine must be fairly pure, and free from
resinous substances and SO_{3}, to give good results by this process.
~Analysis of the "Waste Acids" from the Manufacture of Nitro-Glycerine or
Gun-Cotton.~ Determine the specific gravity by the specific gravity bottle
or hydrometer, and the oxides of nitrogen by the permanganate method
described under nitro-glycerine. Now determine the total acidity of the
mixture by means of a tenth normal solution of sodium hydrate, and
calculate it as nitric acid (HNO_{3}), then determine the nitric acid by
means of Lunge nitrometer, and subtract percentage found from total
acidity, and calculate the difference into sulphuric acid, thus:--
Public-domain text, read in full here on John Shaqi.
Reviews
Reviews
No reviews yet
Be the first to share your thoughts on this work.
Elsewhere in the archive
Join the Discussion
Join the discussion
Sign in to leave a comment or review.
Sign InorCreate an account