When the jets under the mixture have all been turned on, light the gas
under the layer of oxid at the end of the tube. When the evolution
of gas has ceased, turn out all the lights except those under the
metallic copper and anterior layer of oxid, and allow to cool for a
few moments. Exhaust with the pump and remove the azotometer before
the flow of mercury is stopped. Break the connection of the tube with
the pump, stop the flow of mercury, and extinguish the lights. Allow
the azotometer to stand for at least an hour, or cool with a stream of
water until a permanent volume and temperature have been reached.
Adjust accurately the level of the potash solution in the bulb to that
in the azotometer; note the volume of gas, temperature, and height of
barometer; make calculation as usual, or read results from tables.
=156. Note on Official Volumetric Method.=—The determination of
nitrogen in its gaseous state by combustion with copper oxid, has
practically gone out of use as an analytical method. The official
chemists rarely use it even for control work on samples sent out for
comparative analysis. The method recommended differs considerably from
the process of Jenkins and Johnson, on which it is based. The only
source of oxygen in the official method is in the copper oxid. Hence it
is necessary that the oxid in immediate contact with the organic matter
be in a sufficiently fine state of subdivision, and that the substance
itself be very finely powdered and intimately mixed with the oxidizing
material. Failure to attend to these precautions will be followed by
an incomplete combustion and a consequent deficit in the volume of
nitrogen obtained.
The copper oxid before using is ignited, and is best filled into the
tube while still warm by means of a long pointed metal scoop, or other
convenient method. The copper spiral, after use, is reduced at a red
heat in a current of hydrogen, and may thus be used many times.
=157. The Pump.=—Any form of mercury pump which will secure a complete
vacuum may be used. A most excellent one can be arranged in any
laboratory at a very small expense. The pump used in this laboratory
for many years answers every purpose, and costs practically nothing,
being made out of old material not very valuable for other use.
The construction of the pump and its use in connection with the
combustion tube will be clearly understood from the following
description:
[Illustration: FIGURE 10.
MERCURY PUMP AND AZOTOMETER.]
Public-domain text, read in full here on John Shaqi.
Reviews
Reviews
No reviews yet
Be the first to share your thoughts on this work.
Elsewhere in the archive
Join the Discussion
Join the discussion
Sign in to leave a comment or review.
Sign InorCreate an account