=196. The Official Gunning Method.=—In a digestion flask holding
from 250 to 500 cubic centimeters place from seven-tenths to two and
eight-tenths grams of the substance to be analyzed, according to its
proportion of nitrogen. Then add ten grams of powdered potassium
sulfate and from fifteen to twenty-five cubic centimeters (ordinarily
about twenty cubic centimeters) of concentrated sulfuric acid. Conduct
the digestion as in the kjeldahl process, starting with a temperature
below boiling-point and increasing the heat gradually until frothing
ceases. Digest until colorless or nearly so. Do not add either
potassium permanganate or potassium sulfid. Dilute, neutralize, and
distil as in the kjeldahl method. In neutralizing, it is convenient
to add a few drops of phenolphthalein indicator, by which one can
tell when the acid is completely neutralized, remembering that the
pink color, which indicates an alkaline reaction, is destroyed by
a considerable excess of strong fixed alkali. The distillation and
titration are conducted as in the kjeldahl method. In distilling,
the use of zinc or of any substance to prevent bumping or foaming
is generally unnecessary, if too great an excess of fixed alkali be
avoided. The amount of sulfuric acid recommended by Gunning is two
grams for each gram of potassium sulfate; but Voorhees has found that
this mixture is so viscous as to cause troublesome foaming frequently,
and after cooling it cakes in a hard mass, which may be difficult
to redissolve.[167] To avoid foaming and caking, he has found it an
effective means to increase the amount of sulfuric acid used, taking
instead of two grams to one of potassium sulfate three or four grams
of acid to one of potassium sulfate. It is, therefore, suggested
in carrying out the work, to use from five to twenty-five cubic
centimeters (ordinarily about twenty cubic centimeters) of sulfuric
acid for ten grams of potassium sulfate. In case the potassium sulfate
is not free from nitrogen compounds, one or two recrystallizations will
make it pure.
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