=187. Modifications of the Kjeldahl Process.=—It would be impracticable
here to give even a summary of the many unimportant changes which
the moist combustion process has undergone since the first papers of
its author were published. These changes may be divided into three
classes; _viz._, 1. Those changes which refer solely to the quantities
of substance taken for analysis, to the composition of the acid
mixture, to the duration of the digestion, to the form and size of
the flasks, both for digestion and distillation, and to the manner of
distillation and of titration. For references to the papers on these
subjects the reader may consult the periodic journals.[155] The most
important of these minor changes are the following: Instead of the
titration by means of separated iodin most chemists have had recourse
to the simpler method of direct titration of the excess of acid by a
set solution of an alkali. Barium, sodium, and potassium hydroxids are
the alkaline solutions most employed. This process permits of a larger
quantity of the sample being taken for combustion and of the use of a
larger quantity of acid in the receiver. It also implies the use of
a larger digestion flask. In fact it is now quite common to make the
digestion in a special glass flask large enough to be used also for the
distillation. This saves one transfer of the material with the possible
danger of loss attending it.
In the distillation it is a common practice, especially in Germany, to
do away with the condensing worm and to carry a long glass tube from
the distilling flask directly into the acid on the receiver. The only
inconvenience in this method is the heating of the contents of the
receiving flask, but this is attended with no danger of loss of ammonia
and the distillate, on account of the high temperature it acquires, is
left free of carbon dioxid. Many of these minor changes have tended to
simplify the process, but without affecting the principle of the method
in the least.
2. In the second place a class of changes may be mentioned in which
there is a marked difference in the method of effecting the oxidation
secured by the introduction of a substance, usually a metal, during
the digestion for the purpose of accelerating the oxidation. In
the original process the only aid to oxidation was applied at the
end of the digestion in the use of potassium permanganate. In the
modifications now under consideration a metallic oxid or metal is
applied at the beginning of the digestion. Copper and mercury are the
metals usually employed. A separate paragraph will be given to the
description of this modification known as the process of Wilfarth.
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