_Manipulation._—The substance to be analyzed should be powdered
finely enough to pass through a sieve of one millimeter mesh; from
seven-tenths to one and four-tenths grams, according to the amount of
nitrogen present, are taken for the determination. Into the closed
end of the combustion tube, put a small loose plug of asbestos, and
upon it about four centimeters of fine soda-lime. In a porcelain dish
or mortar, mix the substance to be analyzed, thoroughly but quickly,
with enough fine soda-lime to fill about sixteen centimeters of the
tube, or about forty times as much soda-lime as substance, and put the
mixture into the combustion tube as quickly as possible by means of
a wide-necked funnel, rinsing out the dish and funnel with a little
more fine soda-lime, which is to be put in on top of the mixture. Fill
the rest of the tube to within about five centimeters of the end with
granulated soda-lime, making it as compact as possible by tapping
the tube gently while held in a nearly upright position during the
filling. The layer of granulated soda-lime should not be less than
twelve centimeters long. Lastly, put in a plug of asbestos about two
centimeters long, pressed rather tightly, and wipe out the end of the
tube to free it from adhering soda-lime.
Connect the tube by means of a well-fitting rubber stopper or cork
with the =U= tube or Will’s bulbs, containing ten cubic centimeters
of standard acid, and adjust it in the combustion furnace so that the
end of the tube projects about four centimeters from the furnace,
supporting the =U= tube or Will’s bulb suitably. Heat the portion of
the tube containing the granulated soda-lime to a moderate redness, and
when this is attained extend the heat gradually through the portion
containing the substance, so as to keep up a moderate and regular flow
of gases through the bulbs, maintaining the heat of the first part
until the whole tube is heated uniformly to the same degree. Continue
the combustion until gases have ceased bubbling through the acid in the
bulbs, and the mixture of substance and soda-lime has become white, or
nearly so, which shows that the combustion is finished. The process
should occupy about three-quarters of an hour, or not more than one
hour. Remove the heat, and when the tube has cooled below redness break
off the closed tip and aspirate air slowly through the apparatus for
two or three minutes to bring all the ammonia into the acid. Disconnect
the tube, wash the acid into a beaker or flask, and titrate with the
standard alkali.
During the combustion the end of the tube projecting from the furnace
must be kept heated sufficiently to prevent the condensation of
moisture, yet not enough to char the stopper. The heat may be regulated
by a shield of tin slipped over the projecting end of the combustion
tube.
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