A text-book of assaying : $b for the use of those connected with mines.Beringer, C. (Cornelius)
Science
A text-book of assaying : $b for the use of those connected with mines.
Beringer, C. (Cornelius)
Assaying
Cadmium occurs in nature as cadmium sulphide in greenockite, CdS, which
is very rare. It is widely diffused in calamine, blende, and other zinc
ores, forming, in some cases, as much as 2 or 3 per cent. of the ore.
Oxide of cadmium forms the "brown blaze" of the zinc smelters.
Sulphide of cadmium is used as a pigment (cadmium yellow); and the metal
and some of its salts are useful reagents.
The salts of cadmium closely resemble those of zinc. The hydrate,
however, is insoluble in excess of potash, and the sulphide is insoluble
in dilute acids. It forms only one series of salts.
Cadmium is detected by giving with sulphuretted hydrogen in solutions,
not too strongly acid, a yellow precipitate, which is insoluble in
solutions of the alkalies, alkaline sulphides, or cyanide of potassium.
~Solution and Separation.~--Substances containing cadmium are soluble in
acids. The solution is evaporated to dryness (to render any silica that
may be present insoluble) and taken up with 10 c.c. of dilute
hydrochloric acid. Dilute to 100 c.c., and pass sulphuretted hydrogen.
Filter, digest the precipitate with soda, wash, and boil with dilute
sulphuric acid. Filter; the filtrate contains the cadmium and, possibly,
a small quantity of zinc, from which it is best separated by
reprecipitating with sulphuretted hydrogen.
GRAVIMETRIC DETERMINATION.
The solution containing the cadmium freed from the other metals is
precipitated with sulphuretted hydrogen in a moderately-acid solution.
The precipitate is collected on a weighed filter, and washed, first with
an acid solution of sulphuretted hydrogen, and afterwards with water. It
is dried at 100° C. and weighed. If free sulphur is suspected to be
present, extract with bisulphide of carbon, and again weigh. The residue
is cadmium sulphide, which contains 77.78 per cent. of cadmium. It is a
yellow powder insoluble in solutions of the alkalies, alkaline
sulphides, or cyanide of potassium. It dissolves readily in acid. It
cannot be ignited in a current of hydrogen without loss.
VOLUMETRIC METHOD.
The solution containing the cadmium is concentrated by evaporation, and
mixed with an excess of oxalic acid and alcohol. The precipitate is
filtered, washed with alcohol, dissolved in hot hydrochloric acid, and
titrated with permanganate of potassium.
FOOTNOTES:
[64] When chromium is present some of the iron may escape precipitation
but it can be recovered from the solution by means of ammonic sulphide.
[65]
(1) 10FeSO_{4} + 2KMnO_{4} + 8H_{2}SO_{4} = 5Fe_{2}(SO_{4})_{3} +
2MnSO_{4} + K_{2}SO_{4} + 8H_{2}O.
(2) 6FeCl_{2} + K_{2}Cr_{2}O_{7} + 14HCl = 3Fe_{2}Cl_{6} + Cr_{2}Cl_{6}
+ 2KCl + 7H_{2}O.
[66] (1) Fe_{2}Cl_{6} + SnCl_{2} = 2FeCl_{2} + SnCl_{4}.
(2) Fe_{2}Cl_{6} + SH_{2} = 2FeCl_{2} + 2HCl + S.
(3) Fe_{2}Cl_{6} + Na_{2}SO_{3} + H_{2}O = 2FeCl_{2}
+ Na_{2}SO_{4} + 2HCl.
(4) Fe_{2}Cl_{6} + Zn = 2FeCl_{2} + ZnCl_{2}.
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