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[References: 6 tit.]

The method of determination of rhodium by the method of Stripping voltammetry in ores and technogenic raw materials has been developed. Determination of rhodium (III) in solution by Stripping voltammetry method was carried out by peak of selective electrooxidation of bismuth from intermetallic compound Bi2Rh. 1 M KSCN was selected as a background electrolyte. The method of melting of the sample with potassium tetrafluoroborate (KBrF4) at a temperature of 500 was used for the conversion of the rhodium solution.The method of deposition of most ions present in solution of alkali metals was used to separate ions of rhodium (III) from the matrix of the samples. Ions of Pt (IV), Rh (III) and Ir (IV) remain in solution after precipitation. Ions of iridium (IV) and 10- fold excess of platinum (IV) do not interfere with the determination of rhodium (III) against the background of 1 M KSCN.