=22. Caldwell’s Hydrogen Drying-Bath.=—An excellent device for drying
in hydrogen has been described by Caldwell.[9] A vessel of copper or
other suitable material serves to hold the tubes containing the samples
to be dried. It should be about twenty-four centimeters long, fifteen
high, and eight wide. This vessel is contained in another made of the
same material and of the dimensions shown in the figure. On one side
the edge of this containing vessel may not be more than one centimeter
high and the bath should rest against it. The other side is made higher
to form a support for the drying tubes as indicated.
[Illustration: FIGURE 12. CALDWELL’S HYDROGEN DRYING APPARATUS.]
The tube containing the substance _a d_ is made of glass and may be
closed by the ground stoppers _c b_ or the tube stoppers _e f_. At _a_
it carries a perforated platinum disk for holding the filtering felt.
The tube should be about thirteen centimeters long and have an internal
diameter of about twenty millimeters. With its stoppers it should weigh
only a little over thirty grams. The asbestos felt should not be thick
enough to prevent the free passage of gas. Passing diagonally through
the bath are metal tubes, preferably made of copper, and of such a
size as just to receive the glass drying tubes. If these be a little
loose they should be made tight by wrapping them with a narrow coil of
paper at either end of the tubular receptacle. The entrance of cold
air between the glass tube and its metal holder is thus prevented, and
the glass tube is held firmly in position. The glass tube should be
weighed with its two solid stoppers. Afterwards the sample, about two
grams, is placed on the asbestos felt and the stoppers replaced and
the whole reweighed. The exact weight of the sample is thus obtained.
The solid stoppers are then removed and the tube stoppers inserted.
The lower end of the tube is then connected with the supply of dry
hydrogen. The upper tube stopper is connected by a rubber tube with
a small bottle containing sulfuric acid through which the escaping
hydrogen is made to bubble. A double purpose is thus secured; moisture
is kept from entering the drying tube and the rate at which the
hydrogen is passing is easily noted. After the drying is completed the
solid stoppers are again inserted, the tube cooled in a desiccator and
weighed. The loss of weight is entered as water. The tube containing
the sample can afterwards be put into an extractor and treated with
ether or petroleum in the manner hereafter described. This apparatus
requires more hydrogen than the one previously described, but it is
rather simple in construction, is easily controlled, and has given
satisfactory results.
[Illustration: FIGURE 13. LIEBIG’S ENTE.]
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