An examination of some methods employed in determining the atomic weight of Cadmium — John Shaqi
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.)
weighing the empty boat.
At this stage the sulphide was always from one to two milligrammes
lighter than at the end of the determination. It was reheated for
periods of one hour until the weight remained constant. This generally
required from three to five hours. All weighings were reduced to the
vacuum standard on the basis of 4.5 for the Sp. Gr. of cadmium sulphide,
3.31 for the Sp. Gr. of cadmium oxalate, 8.4 for the Sp. Gr. of brass
weights and 21 for the Sp. Gr. of platinum weights.
The results are as follows:
Cd C_{2}O_{4} CdS At. Wt. Cd.
I. 2.56319 1.84716 112.25
II. 2.18364 1.57341 112.17
III. 2.11643 1.52462 112.05
IV. 3.13105 2.25582 112.12
The first three determinations were made exactly as above described, the
heating in hydrogen sulphide being done in a Bohemian glass combustion
tube. The hydrogen sulphide was dried with calcium chloride.
The fourth determination was made under somewhat different conditions.
The boat containing the weighed oxalate was placed in a combustion tube
which passed through an asbestus covered air-bath. The air was displaced
by a current of dry hydrogen sulphide and the bath slowly heated. When
the temperature had risen to 210°C. it was maintained there for three
hours, and then raised to 250°C. for three hours. The sulphide then
weighed 2.27 grammes, being 14 milligrammes heavier than when the
determination was finished. It was replaced in the tube and reheated in
a current of hydrogen sulphide at a temperature of 300°C. for four
hours. It was then transferred to a porcelain tube and heated to redness
for one hour. It then weighed 2.25437 grammes, being 1.45 milligrammes
lighter than at the end of the determination. The weight did not become
constant until it had been heated six hours more to redness in a current
of hydrogen sulphide. When this oxalate was slowly heated in H_{2}S, a
small amount of oxalic acid sublimed to the colder part of the tube,
but, in the other cases where the heating was more rapid, only carbon
monoxide, carbon dioxide, and water were observed.
Discussion of the Method.
When hydrogen sulphide is passed through a red-hot tube, sulphur is
deposited on the colder parts because at this temperature hydrogen
sulphide dissociates and the elements do not recombine on cooling. In
this work, a faint sublimate was noticed before coming to the zone of
sulphur deposit. On exposure to air, it deliquesced in a few minutes
forming small yellow drops which had a saline taste, and gave tests for
potassium and sulphur. The sublimate had a yellow color and was
evidently formed by the action of sulphur on glass. It seemed to do no
harm, but in the fourth determination an effort was made to avoid it by
using a porcelain tube instead of a glass combustion tube for heating to
redness in a current of hydrogen sulphide.
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