_Filling the tube._—Of ordinary commercial fertilizers take from
one to two grams for analysis. In the case of highly nitrogenized
substances the amount to be taken must be regulated by the amount of
nitrogen estimated to be present. Fill the tube as follows: (1) About
five centimeters of coarse cupric oxid: (2) Place on the small paper
scoop enough of the fine cupric oxid to fill, after having been mixed
with the substance to be analyzed, about ten centimeters of the tube;
pour on this the substance, rinsing the watch-glass with a little of
the fine oxid, and mix thoroughly with a spatula; pour into the tube,
rinsing the scoop with a little fine oxid: (3) About thirty centimeters
of coarse cupric oxid: (4) About seven centimeters of metallic copper:
(5) About six centimeters of coarse cupric oxid (anterior layer):
(6) A small plug of asbestos: (7) From eight-tenths to one gram of
sodium bicarbonate: (8) A large, loose plug of asbestos; place the
tube in the furnace, leaving about two and five-tenths centimeters of
it projecting; connect with the pump by a rubber stopper smeared with
glycerol, taking care to make the connection perfectly tight.
_Operation._—Exhaust the air from the tube by means of the pump. When a
vacuum has been obtained allow the flow of mercury to continue; light
the gas under that part of the tube containing the metallic copper,
the anterior layer of cupric oxid (see (5) above), and the sodium
bicarbonate. As soon as the vacuum is destroyed and the apparatus
filled with carbon dioxid, shut off the flow of mercury and at once
introduce the delivery-tube of the pump into the receiving arm of the
azotometer just below the surface of the mercury seal, so that the
escaping bubbles will pass into the air and not into the tube, thus
avoiding the useless saturation of the caustic potash solution.
Set the pump in motion and when the flow of carbon dioxid has very
nearly or completely ceased, pass the delivery-tube down into the
receiving arm, so that the bubbles will escape into the azotometer.
Light the gas under the thirty centimeter layer of oxid, heat gently
for a few moments to drive out any moisture that may be present, and
bring to a red heat. Heat gradually the mixture of substance and oxid,
lighting one jet at a time. Avoid a too rapid evolution of bubbles,
which should be allowed to escape at the rate of about one per second
or a little faster.
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