=214. The Halle Zinc-Iron Method.=—For determining the nitrogen in
Chile saltpeter the reduction method is conducted at the Halle Station
as follows:[179] Ten grams of the nitrate are dissolved in one liter
and fifty cubic centimeters of the solution corresponding to half
a gram of the sample, taken for each determination. The apparatus
employed is shown in Fig. 15. A mixture of five grams of zinc dust
and an equal weight of iron filings is employed as the source of
hydrogen. The reduction takes place in an alkaline medium secured by
adding to the other materials mentioned, eighty cubic centimeters of
soda-lye of 1.30 specific gravity. The respective quantities of iron
and zinc may be measured instead of weighed, as exact proportions are
not required. After the addition of all the materials the flask is
allowed to stand for an hour at room temperature. The distillation
is then commenced and continued until at least 100 cubic centimeters
of distillate have been collected. The receiving flasks are ordinary
erlenmeyers, each of which contains twenty cubic centimeters of set
sulfuric acid, as in the usual kjeldahl process. The flasks are sealed
with a few drops of water by the device shown in the figure. After the
end of the operation the water in each one is washed back into its
proper flask with freshly boiled water. During the vigorous evolution
of hydrogen, at the beginning of the operation, some kind of a safety
arrangement is necessary to prevent the particles of soda-lye being
carried over by the bubbles of that gas. The siphon bulb shown in the
figure is found effective for this purpose. In this operation better
results are obtained by condensing the escaping steam, and for this
reason the block tin tubes are conducted through a tank supplied with
a current of cold water. The ends of the tubes should not dip below
the surface of the liquid in the receivers. When the condensed liquid
collects in considerable quantities in the safety tube the lamp should
be extinguished under the flask, which permits the return of the liquid
to the flask by means of the siphon. This should be done two or three
times during the progress of the distillation to prevent a too high
concentration of the soda-lye, thus endangering the flask. The excess
of the acid in the receiver is determined by titration, as in the
regular kjeldahl method. Blank determinations should be made, from time
to time, and corrections made in harmony therewith.
=215. Method of the French Sugar Chemists.=—The nitrogen in Chile
saltpeter is estimated by the French chemists according to the method
of Schlösing, described in the first volume, page 500. In order to
avoid the trouble of calculating the results from the volume of nitric
oxid obtained, a determination is first made with a pure salt, sodium
or potassium nitrate. The volume of gas obtained is read directly
without correction and taken for direct comparison. The comparison is
made as follows:
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