=179. The Method of Kjeldahl.=—The process originally proposed by
Kjeldahl is applicable only to nitrogenous bodies free of nitric
nitrogen. The principle of the process is based on the action of
concentrated sulfuric acid at the boiling-point in decomposing
nitrogenous compounds without producing volatile combinations and
the subsequent completion of the oxidation by means of potassium
permanganate. The original process has been modified by many analysts
but the basic principle of it has remained unchanged. It will therefore
prove useful here to describe the process as originally given.[149]
The weighed substance is placed in a small flask. With solid bodies
this is a very simple operation, but with liquids more difficult.
Liquids which are not decomposed, on heating, should be evaporated in
a thin glass dish which can be ground up and placed in the digestion
flask with the desiccated sample. The strongest sulfuric acid is added
in sufficient quantity to secure complete decomposition, not less than
ten cubic centimeters in any case. The acid must be free of ammonia and
be kept in such a way as not to absorb ammonia from the atmosphere of
the laboratory. To guard against danger of error from such an impurity
frequent control determinations should be made. In control experiments
one or two grams of pure sugar should be used as the organic matter. If
the acid employed contain traces of ammonia the necessary corrections
should be made in each analysis. The flask having been charged is
placed on a wire gauze over a small flame. The organic matter becomes
black and tar-like and soon there is a rapid decomposition attended
with the evolution of gaseous products among which sulfur dioxid is
found. To avoid danger from spurting, the digestion flask should be
placed in an oblique position. The flask should have, at least, a
capacity of 100 cubic centimeters and a long neck and be made of a
kind of glass capable of withstanding the action of the boiling acid.
Particles of the carbonized organic matter left on the sides of the
flask by the foaming of the mass at first are gradually dissolved by
the vapors of the boiling acid as the digestion proceeds. The action
of the sulfuric acid is not entirely finished when gases cease to be
given off but the digestion should be continued until the liquid in the
flask is clear and colorless or nearly so. Usually about two hours are
required to secure this result. When aided by the means mentioned below
the time of digestion can be very materially shortened. By adding some
fuming sulfuric acid, or glacial phosphoric acid, the dilution caused
by the formation of water in the combustion of the organic matter, can
be avoided. For albuminoid bodies it is hardly necessary to continue
the combustion until all carbonaceous matter is destroyed. The full
complement of ammonia is usually obtained after an hour’s combustion
even if the liquid be still black or brown, but with other nitrogenous
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