=197. Gunning Method Adapted to Nitrates.=—The essential features
of this modification are due to Winton and Voorhees.[168] The
modifications of the kjeldahl method, for similar purposes, furnished
the material details for the gunning modified process. Winton reports
good results from digesting for two hours, from half a gram to a gram
of the sample with thirty cubic centimeters of sulfuric containing
two grams of salicylic acid, in a flask of half a liter capacity. Two
grams of zinc dust are then slowly added, with constant shaking, and
the flask heated, at first gently, until, after a few minutes boiling,
dense fumes are no longer emitted. Three grams of potassium sulfate are
next added and the boiling continued until the solution is colorless,
or if iron be present, until a light straw color is produced. On
cooling, when the mixture begins to solidify, water is added with
caution, and afterwards sodium hydroxid, and the ammonia is obtained by
distillation.
In the process, as conducted by Voorhees, about one gram of the sample
is digested with ten grams of potassium sulfate and thirty cubic
centimeters of sulfuric containing one gram of salicylic acid, and
three grains of zinc sulfid. The heat is kept down until frothing
ceases, and then the mass kept in gentle ebullition until clear. The
distillation is accomplished with the usual precautions. The voorhees
process is superior to that recommended by Winton in adding the
potassium sulfate at the beginning of the combustion.
=198. Official Gunning Method Modified to Include the Nitrogen
of Nitrates.=—In a digestion flask holding from 250 to 500 cubic
centimeters, place from seven-tenths to three and five-tenths grams
of the substance to be analyzed, according to the amount of nitrogen
present. Add from thirty to thirty-five cubic centimeters of salicylic
acid mixture, namely, thirty cubic centimeters of sulfuric to one gram
of salicylic acid, shake until thoroughly mixed, and allow to stand
from five to ten minutes, with frequent shaking; then add five grams of
sodium thiosulfate and ten grams of potassium sulfate. Heat very gently
until frothing ceases, then strongly until nearly colorless. Dilute,
neutralize, and distil the same as in the gunning method.
DETERMINATION OF NITROGEN IN DEFINITE FORMS OF COMBINATION.
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