The use of mercuric oxid in this operation greatly shortens the time
necessary for digestion, which is rarely over an hour and a half in
case of substances most difficult to oxidize, and is more commonly
less than an hour. In most cases the use of potassium permanganate is
quite unnecessary, but it is believed that in exceptional cases it is
required for complete oxidation, and in view of the uncertainty it is
always used. The potassium sulfid removes all the mercury from the
solution, and so prevents the formation of mercurammonium compounds
which are not completely decomposed by soda solution. The addition
of zinc gives rise to an evolution of hydrogen and prevents violent
bumping. Previous to use, the reagents should be tested by a blank
experiment with sugar, which will partially reduce any nitrates that
are present, which might otherwise escape notice.
[Illustration: FIGURE 13. DISTILLING APPARATUS.]
=185. The Distillation Apparatus in Use in the Laboratory of the
Department of Agriculture.=—In this laboratory the distilling apparatus
is arranged as shown in Figure 13. The flasks are the same as are
used in the digestion. They are connected to the block tin condensers
by the bulb and rubber tubes, shown hanging on the projecting ends
of the block tin condensers on the right and left of the figure. The
condensers are contained in a trough through which cold water flows
during the distillation. The bulb above the flask carries an emergent
tube which extends to near the center of the bulb and is bent laterally
to avoid any danger of carrying over any alkali that may be projected
into the bulb during boiling. The boiling is continued usually for
nearly an hour or until bumping begins. The table on which the
apparatus is placed is so arranged as to permit of easy access on all
sides. The standard acid is held in erlenmeyers placed on wooden blocks
so that the end of the condenser which is a drawn-out glass tube, dips
beneath the surface of the acid.
=186. Patrick’s Distilling Flask.=—To avoid the expense and annoyance
attending the breaking of the distilling flasks Patrick has proposed to
make them of copper.[154] The size, about half a liter, made for the
evolution of oxygen for experimental purposes, may be used. A little
excess of potassium sulfid is used to make up for any of it which
might be consumed by the copper. About twenty-five cubic centimeters
of this solution are recommended. No zinc or pumice stone is required
to prevent bumping and the distillation may be finished within thirty
minutes, thus securing a saving of time. There will doubtless be a
slight corrosion of the flasks by the sulfid employed but where the
gunning oxidation process is practiced this danger would be avoided.
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