At first the tripodal support of the flasks is so turned as to bring
them between the lamps and in this way a too rapid reaction is at
first avoided. After half an hour the tripods are so turned as to
bring each flask directly over the lamp, the flame of which is allowed
to impinge directly against the glass. The flame is so regulated
that after the evolution of the sulfur dioxid has nearly ceased the
contents of the flask are brought into gentle ebullition. The boiling
is continued until the contents of the flask are colorless, usually
about two hours. As a rule such substances as cottonseed-meal and
dried blood will take a longer time for complete combustion than other
fertilizing materials. During the combustion the flasks are closed with
an oblong loose-fitting unground glass stopper. When the oxidation is
finished the contents of the flasks are allowed to cool, the stoppers
are removed, and enough water is added to fill the flasks about
three-quarters full. The flasks are gently shaken, and the possibility
of breaking, from the heat developed, must not be overlooked. To avoid
confusion the flasks are all numbered before beginning the work, and
the numbers noted by the analyst in connection with the samples. The
contents of each one are next poured into the distillation flask and
the digestion vessels are washed with 100 cubic centimeters of water in
three portions, and the wash-water added to the liquid. Sometimes in
washing out the digestion flask yellow basic mercury compounds separate
on its walls, but this does not, in any way, influence the accuracy
of the results. The distillation flasks should have about 600 cubic
centimeters capacity. To avoid the transfer the digestion may take
place in the distillation flask in which case the latter must be made
of special glass as indicated.
To the liquid thus transferred are added seventy-five cubic centimeters
of soda-lye containing one and one-half times as much potassium sulfid
as is necessary to combine with the mercuric sulfate present. The lye
is of such a strength that sixty cubic centimeters are sufficient to
neutralize the acid present. It has a specific gravity of 1.375 and
contains thirty-three grams of potassium sulfid in a liter.
In order to avoid the bumping which may take place during the
distillation, some granulated zinc should be added.
Public-domain text, read in full here on John Shaqi.
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