_Apparatus._—(1) _Kjeldahl digestion flasks_ of hard, moderately thick,
well-annealed glass: These flasks are about twenty-two centimeters
long, with a round, pear-shaped bottom, having a maximum diameter of
six centimeters and tapering out gradually in a long neck, which is two
centimeters in diameter at the narrowest part, and flared a little at
the edge. The total capacity is from 225 to 250 cubic centimeters.
(2) _Distillation flasks_ of ordinary shape, of 550 cubic centimeters
capacity, or preferably flasks of well-annealed glass, of the same
capacity, of pear-shaped bottom, for both digestion and distillation,
fitted with a rubber stopper and a bulb-tube above to prevent the
possibility of sodium hydroxid being carried over mechanically during
distillation: The bulbs are about three centimeters in diameter, the
tubes being of the same diameter as the condenser and cut off obliquely
at the lower end. This is adjusted to the tube of the condenser by a
rubber tube.
_Manipulation._—(1) _The Digestion._—From seven-tenths to three and
five-tenths grams of the substance to be analyzed, according to its
proportion of nitrogen, are brought into a digestion flask with
approximately seven-tenths gram of mercuric oxid or its equivalent
in metallic mercury and twenty cubic centimeters of sulfuric acid.
The flask is placed in an inclined position, and heated below the
boiling-point of the acid for from five to fifteen minutes or until
frothing has ceased. If the mixture froth badly, a small piece of
paraffin may be added to prevent it. The heat is then raised until the
acid boils briskly. No further attention is required until the contents
of the flask have become a clear liquid, which is colorless or at least
has only a very pale straw color. The flask is then removed from the
frame, held upright, and while still hot, potassium permanganate is
dropped in carefully and in small quantities at a time until, after
shaking, the liquid remains of a green or purple color.
(2) _The distillation._—After cooling, the contents of the flask are
transferred to the distilling flask with about 200 cubic centimeters of
water, a few pieces of granulated zinc, pumice stone, or one-half gram
of zinc dust when found necessary to keep the contents of the flask
from bumping, and twenty-five cubic centimeters of potassium sulfid
solution are added, shaking the flask to mix its contents. Next add
fifty cubic centimeters of the soda solution, or sufficient to make the
reaction strongly alkaline, pouring it down the sides of the flask so
that it does not mix at once with the acid solution. Connect the flask
with the condenser, mix the contents by shaking, and distil until all
ammonia has passed over into the standard acid. The first 150 cubic
centimeters of the distillate will generally contain all the ammonia.
This operation usually requires from forty minutes to one hour and a
half. The distillate is then titrated with standard alkali.
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