off and the pump kept in operation until the manometer again shows a
perfect vacuum when the operation may be considered finished. In the
manipulation our chief variation from the official method consists in
connecting the combustion apparatus with the measuring tube before
the heat is applied to the front end of the combustion tube. Any
particles of the sample which may have stuck to the sides of the tube
on filling will thus be subject to combustion and the gases produced
measured. Where it is certain that no such adhesion has taken place it
is somewhat safer on account of the possible presence of occluded gases
to heat the front end of the tube before connecting the combustion
apparatus with the azotometer.
=161. Method of Johnson and Jenkins.=—In the method of Johnson and
Jenkins the principal variation from the process described consists
in introducing into the combustion tube a source of oxygen whereby
any difficultly combustible carbon may be easily oxidized and all the
nitrogen be more certainly set free.[135] The potassium chlorate used
for this purpose is placed in the posterior part of the tube, which is
bent at slight angle to receive it. The sodium bicarbonate is placed
in the anterior end of the tube. The combustion goes on as already
described, and at its close the potassium chlorate is heated to evolve
the oxygen. The free oxygen is absorbed by the reduced copper oxid, or
consumed by the unburned carbon. Any excess of oxygen is recognized at
once by its action on the copper spiral. As soon as this shows signs
of oxidation the evolution of the gas is stopped. Care must be taken
not to allow the oxygen to come off so rapidly as to escape entire
absorption by the contents of the combustion tube. In such a case the
nitrogen in the measuring tube would be contaminated.
It is rarely necessary in fertilizer analysis to have need of more
oxygen than is contained in the copper oxid powder in contact with the
sample during the progress of combustion.
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