Determination of Au(III) and Ag(I) in Carbonaceous Shales and Pyrites by Stripping Voltammetry

Techniques of stripping voltammetry (SV) determination of silver and gold in pyrites and carbonaceous matter are developed. The problem of quantitative transfer of the analytes into the solution is solved. For this purpose, the ore matrix of carbonaceous shales was decomposed by mineral acids in autoclaves at high pressures. The element to be determined from the sample matrix was separated by extraction. Ag(I) ions from the solutions were extracted in the form of a dithizonate complex in CCl4. Au(III) ions were extracted by diethyl ether. The extracts were decomposed thermally. The dry residue was dissolved in the background electrolyte, and the element was determined by the SV method. The graphite electrode (GE) impregnated with polyethylene was used as a working electrode in the SV determination of silver. The SV determination of gold was carried out using a GE modified by bismuth. The limits of detection (LOD) of Ag(I) and Au(III) contents were equal to 0.016 mg L−1 and 0.0086 mg L−1, respectively. The results of SV determination of gold and silver in standard samples, pyrites, and carbonaceous shales were presented. The silver content in the pyrite was 13.6 g t−1, and in carbon shale it was 0.34 g t−1. The concentration of gold in the pyrite of the Kirovsko⁻Kryklinskaya ore zone was 1.15 g t−1, while in carbonaceous shales it was 2.66 g t−1. The obtained data were consistent with the data of atomic emission spectroscopy (AES) and inductively-coupled plasma mass spectrometry (ICP⁻MS). The error of determination of elements by stripping voltammetry was calculated as ranging from 10 to 6 g t−1 (less than 12%) in pyrite and carbonaceous material when determining the silver content, and from 1 to 3 g t−1 (less than 22%) when determining the gold content in pyrite and carbonaceous matter