Nitro-Explosives: A Practical TreatiseSanford, P. Gerald (Percy Gerald)
Science
Nitro-Explosives: A Practical Treatise
Sanford, P. Gerald (Percy Gerald)
Celluloid; Explosives
For the estimation of nitrogen in nitro-cellulose take .5 to .65 grm., and
place in the decomposition flask _f_ (Fig. 45), washing in with about 25
c.c. of water by alternately opening clips D and E. The air in the flask
is driven out by boiling, whilst the air is shut off by the tube _i_
dipping into the basin W, which is filled with the soda lye, and tube K is
placed in the test tube R, which contains a few c.c. of water. As soon as
all the air is completely driven out, clips D and E are closed, and the
gas jet is taken away. (This flask must be a strong one, or it will
burst.) Into test tube R, 25 c.c. of concentrated solution of
protochloride of iron and 10 to 15 c.c. concentrated hydrochloric acid are
poured, which are sucked up into the developing flask _f_ by opening clip
E, air being carefully kept from entering. The clip E is now closed, and
tube _i_ is put underneath the burette, and the development of NO gas is
commenced by heating the contents of the flask _f_. When the pressure of
the gas in the flask has become greater than the pressure of the
atmosphere, the connecting tube begins to swell at _i_, whereupon clip D
is opened, and the boiling continued with frequent shaking of the bulb,
until no more nitrous gas bubbles rise up into the soda lye, the
distilling over of the HCl causes a crackling noise, the clip D is closed,
and E opened. The burette is again put hermetically on the indiarubber
stopper in basin W, and the apparatus is left to cool until the water
discharged through P shows the same temperature as the water flowing
through (into the cooling jacket) Z. If the level of the soda solution in
the tube X is now put on exactly the same level as that in the burette by
lowering or elevating the tube X as required, the volume of NO obtained in
c.c. can be read off within 1/10 c.c., and the percentage of nitrogen
calculated by the usual formula.
[Illustration: FIG. 45.--Decomposition Flask for Schultze-Tieman Method.]
The solution of protochloride of iron is obtained by dissolving iron
nails, &c., in concentrated HCl, the iron being in excess. When the
development of hydrogen ceases, it is necessary to filter warm through a
paper filter, and acidify filtrate with a few drops of HCl. The soda
solution used has a sp. gr. of 1.210 to 1.260; equals 25 deg. to 30 deg. B. The
nitro-cellulose is dried in quantities of 2 grms. at 70 deg. C. during eight
to ten hours, and then three hours in an exiccator over H_{2}SO_{4}. The
results obtained with this apparatus are very accurate. The reaction is
founded upon that of MM. Champion and Pellet's method.
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