Nitro-Explosives: A Practical TreatiseSanford, P. Gerald (Percy Gerald)
Science
Nitro-Explosives: A Practical Treatise
Sanford, P. Gerald (Percy Gerald)
Celluloid; Explosives
A method for the determination of soluble nitro-cellulose in gun-cotton
and smokeless powder has been published by K.B. Quinan (_Jour. Amer. Chem.
Soc._, 23 [4], 258). In this method about 1 grm. of the finely divided dry
sample to be analysed is placed in an aluminium cup 1.9 inch in diameter
and 4-1/8 inch deep. It is then covered and well stirred with 50 c.c. of
alcohol, 100 c.c. of ether are then added, and the mixture is stirred for
several minutes. After removing the stirrer, the cup is lightly covered
with an aluminium lid, and is then placed in the steel cup of a
centrifugal machine, which is gradually got up to a speed of 2,000
revolutions per minute, the total centrifugal force at the position
occupied by the cups (which become horizontal when in rapid rotation) is
about 450 lbs. They are rotated at the full speed for ten to twelve
minutes, and the machine is then gradually stopped. By this time the whole
of the insoluble matter will be at the bottom of the cup, and the
supernatant solution will be clear. It is drawn off to within a quarter of
an inch of the bottom (without disturbing the sediment), with the aid of a
pipette.
Care must be taken that the solution thus withdrawn is perfectly clear.
About 10 to 15 c.c. of colloid solution and a film of insoluble matter
remain at the bottom of the cup; these are stirred up well, the stirrer is
rinsed with ether-alcohol, about 50 c.c. of fresh ether-alcohol are added;
the mixture is again treated in the centrifugal apparatus for about eight
minutes; the whole washing process is then repeated until all soluble
matter has been removed. This may require about seven or eight (or for
samples with much insoluble matter ten or twelve or more) washings, but as
the extraction proceeds, the period of rotation may be somewhat reduced.
After extraction is completed, the insoluble matter is transferred to a
Gooch crucible with the usual asbestos pad, dried at 100 deg. C., and weighed.
The residue may, if wished, be dried and weighed in the aluminium cup, but
then it cannot be ignited. The whole time for an analysis exclusive of
that required for drying, is from one to two hours--average time, 1-1/4
hour. The results are satisfactory both as to accuracy and rapidity.
Acetone-soluble nitro-cellulose may be determined by the same method.
~The Unconverted or Non-nitrated Cotton.~--However well the cotton has
been nitrated, it is almost certain to contain a small quantity of non-
nitrated or unconverted cotton. This can be determined thus:--Five grms.
of the sample are boiled with a saturated solution of sodium sulphide, and
then allowed to stand for forty-eight hours, and afterwards filtered or
decanted, and again boiled with fresh solutions of sulphide, and again
filtered, washed first with dilute HCl and then with water, dried, and
weighed. The residue is the cellulose that was not nitrated, plus ash, &c.
It should be ignited, and the weight of the ash deducted from the previous
weight.
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