DETERMINATION OF ANTIMONY.
Antimony may be precipitated in its metallic state from a hydrochloric acid solution, but it does not adhere very firmly to the electrode. If potassium oxalate is added to a solution of the trichloride, the antimony may be readily reduced, but the metal adheres still less firmly to the electrode than it did in the first instance. An adherent coating may be obtained by adding an alkaline tartrate, but in that case the separation takes place too slowly. The precipitation of antimony may be very readily effected from solutions of its sulpho salts.
To a liquid, which may contain free hydrochloric acid, hydrogen sulphide is added, then neutralized with ammonium hydrate, and saturated with ammonium sulphide in excess. The reduction may be accelerated by the addition of some ammonium sulphate. The antimony separates out as a fine, light gray precipitate on the electrode, and which adheres very firmly, provided the precipitation has not been carried on too rapidly, i. e., if the current employed for the reduction was not too strong.
When the reduction has been completed, the supernatant liquid is poured off, and the residue washed in the ordinary manner.