=189. Modification of Asboth.=—In order to adapt the moist combustion
process to nitric nitrogen Asboth proposed the use of benzoic
acid.[160] For half a gram of saltpeter 1.75 grams of benzoic acid
should be used. At the end of the combustion the residual benzoic
acid is oxidized by means of potassium permanganate with a subsequent
reheating. If the nitrogen be present as an oxid or as cyanid, one gram
of sugar is added. The metallic element added is half a gram of copper
oxid. Asboth also recommends that the soda-lye used in the distillation
be mixed with sodium potassium tartrate for the purpose of holding the
copper and manganese oxids in solution and thus preventing bumping. The
alkaline liquor contains in one liter 350 grams of the double tartrate
and 300 grams of sodium hydroxid.
The principle on which the use of benzoic acid rests is found in the
fact that it easily yields nitro-compounds and thus prevents the loss
of the nitrogen oxids, these readily combining with the benzoic acid.
The nitro-compounds can be subsequently converted into ammonia by
treatment with potassium permanganate.
The pyridin and chinolin groups of bodies do not yield all their
nitrogen as ammonia by the above treatment.
The conclusions drawn by Asboth from the analytical data obtained were:
(1) Sugar should be used in the ordinary kjeldahl process in those
cases where the nitrogen in the organic substance is present as oxids
or as cyanogen.
(2) In the case of nitrates good results may be secured with benzoic
acid but permanganate must be added at the end.
(3) The kjeldahl-wilfarth process can be applied with substances
difficultly decomposed, _e. g._, alkaloidal bodies.
=190. Variation of Jodlbaur.=—The benzoic acid method, although a step
forward, is not entirely satisfactory in the treatment of nitrates by
moist combustion. Jodlbaur has proposed to substitute for the benzoic,
phenolsulfuric acid.[161]
From two to five-tenths gram of a nitrate are treated with twenty
cubic centimeters of concentrated sulfuric and two and a half of
phenolsulfuric acid, together with three grams of zinc dust and five
drops of a solution of platinic chlorid of the strength mentioned
above. The phenolsulfuric acid is prepared by dissolving fifty grams of
phenol in 100 cubic centimeters of strong sulfuric acid. The combustion
is continued until the solution is colorless, which may take as much as
five hours. If phosphoric acid anhydrid be used as recommended above,
the time of the combustion may be diminished by one-half, but in such
a case the glass of the combustion flask is strongly attacked and is
quite likely to break.
With substances very rich in nitrates it is advisable to rub them first
with dry gypsum.
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