An examination of some methods employed in determining the atomic weight of CadmiumBucher, John Emery
History
An examination of some methods employed in determining the atomic weight of Cadmium
Bucher, John Emery
Cadmium; Thesis (Ph. D.)
Whenever a current of nitrogen was required, it was prepared by passing
air over a layer of hot copper gauze in a combustion tube. A short layer
of copper oxide was first introduced, then the copper gauze and finally
another layer of copper oxide. The air was dried with caustic potash
before entering the tube and the nitrogen obtained was also passed
through a long tube filled with lumps of this substance before being
used.
Mode of Procedure.
A number of weighing tubes 140 millimetres long and 13 millimetres
internal diameter were made especially for this work. They were always
used in pairs, one being kept as a counterpoise. A porcelain boat of
such dimensions as just to slide into the tube was placed in each one.
For a determination, a tube and its boat were tared with another tube
and boat, glass against glass and porcelain against porcelain until the
difference in weight was less than two tenths of a milligramme. Both
boats were heated in a current of hydrogen sulphide to incipient redness
for about one hour. The current of hydrogen sulphide was then replaced
by one of nitrogen, in which the boats were cooled, but while still warm
they were transferred to their weighing tubes and allowed to cool in a
dessiccator containing caustic potash and weighed. Before weighing, the
stoppers of the weighing tubes were loosened for a moment in order to
equalize the internal and external pressure. This treatment was usually
repeated two or three times and the difference in weight remained
perfectly constant. A portion of cadmium oxalate sufficient for a
determination was placed in the weighed boat and dried at 150°C. The
oxalate had been prepared exactly like that used in the oxalate method
which has already been described. The gas pressure in the laboratory
varied very much while this method was under investigation and great
difficulty was experienced in maintaining a constant temperature
although a thermoregulator was used. Sometimes a specimen of oxalate
which was supposed to be dry would lose several tenths of a milligramme
when the thermometer would only have gone up to 160°C or 165°C for an
hour by accident. Under these conditions the drying was so uncertain
that only four determinations were completed although many were started.
The boat containing the oxalate which had been dried and weighed was
placed on supports of unglazed porcelain in a combustion tube and a
current of dry hydrogen sulphide passed over it. As soon as the air was
expelled, the tube, which was in a combustion furnace, was slowly heated
until all the oxalate seemed to be decomposed and then raised to dull
redness. After this temperature had been maintained for about an hour,
the sulphide was allowed to cool to a temperature of about 200°C. and
the current of hydrogen sulphide replaced by dry nitrogen, using a
three-way stopcock. When nearly cold the boat was slipped into its
weighing-tube and weighed, the same precautions being used as when
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