The other details of the arrangement and connections have been
sufficiently shown in the previous paragraph.
=159. Volumetric Method in this Laboratory.=—It has been found
convenient here to vary slightly the method of the official chemists
in the following respects: The tube used for the combustion is made of
hard refractory glass, which will keep its shape at a high red heat. It
is drawn out and sealed at one end after being well cleaned and dried.
It should be about eighty centimeters in length and from twelve to
fourteen millimeters in internal diameter. The relative lengths of the
spaces occupied by the several contents of the tube are approximately
as follows: Sodium bicarbonate, two; asbestos, three; coarse copper
oxid, eight; fine copper oxid, containing sample, sixteen; coarse
copper oxid, twenty-five; spiral copper gauze, ten to fifteen; copper
oxid, eight; and asbestos plug, five centimeters, respectively.
The copper oxid should be heated for a considerable time to redness in
a muffle with free access of air before using and the copper gauze be
reduced to pure metallic copper in a current of hydrogen at a low red
heat. The anterior layer of copper oxid serves to oxidize any hydrogen
that may have been occluded by the copper. When a sample is burned
containing all or a considerable part of the nitrogen as nitrates, the
longer piece of copper gauze is used.
=160. The Combustion.=—The tube having been charged and connected
with the pump it is first freed from air by running the pump until
the mercury no longer rises in the manometer. The end of the tube
containing the sodium bicarbonate is then gently heated so that the
evolution of carbon dioxid will be at such a rate as to slowly depress
the mercury in the manometer, but never fast enough to exceed the
capacity of the pump to remove it. The lamp is extinguished under the
sodium carbonate and the carbon dioxid completely removed by means of
the pump. The delivery-tube is then connected with the azotometer, and
the combustion tube carefully heated from the front end backwards, the
copper gauze and coarse copper oxid being raised to a red heat before
the part containing the sample is reached. When the nitrogen begins to
come off, its flow should be so regulated by means of the lamps under
the tube, as to be regular and not too rapid. From half an hour to
an hour should be employed in completing the combustion. Since most
samples of fertilizer contain organic matter, the nitrogen will be
mixed with aqueous vapor and carbon dioxid. The former is condensed
before reaching the azotometer, and the latter is absorbed by the
potassium hydroxid. When the sample is wholly of a mineral nature it
should be mixed with some pure sugar, about half a gram, before being
placed in the tube. When bubbles of gas no longer come over, the heat
should be carried back until there is a gradual evolution of carbon
dioxid under the conditions above noted. Finally the gas is turned
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