Assaying Cadmium Determination Methods

Assaying Cadmium Determination Methods

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 bo 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.