Development of rapid techniques based on selective dissolution for the determination of the precious metals in geological samples

Gowing, Charles John Buttress (1993). Development of rapid techniques based on selective dissolution for the determination of the precious metals in geological samples. PhD thesis The Open University.



The development of a rapid analytical technique for the determination of the platinumgroup elements (PGE) and gold in geological samples is described. The technique is based on selective aqua regia acid leach followed by a selective extraction (using diphenylthiourea and 1,2-dichloroethane) to separate the PGE and Au as a group from concomitant matrix elements. Organic extracts and aqueous raffinates were analysed by graphite furnace atomic absorption spectrometry, for which a comprehensive assessment of matrix interference effects was undertaken. Direct analysis of the aqua regia acid leachates by inductively coupled plasma-mass spectrometry (ICP-MS) was also evaluated. A number of other techniques were used to evaluate recoveries following acid attack, including x-ray fluorescence spectrometry and instrumental neutron activation analysis of solid residues and beta-autoradiography of thin sections to characterise PGE mineral solubility.

The results of these investigations identified optimum conditions for aqua regia extraction (20 ml of normal (3: 1) aqua regia for a 10 g sample, stirring for two hours at room temperature) and that quantitative recoveries can be expected for Au and semiquantitative for Pd with lower, but variable recoveries for Pt, Rh, Ru and Os and very low recovery of Ir. The solvent extraction procedure was effective in selectively extracting Au and Rh but was not quantitative in the extraction of Pt, Pd and Ru, the extraction of which appeared to be influenced by the sample matrix.

Further studies on the solubility in aqua regia of individual PGE minerals indicated that the main control of aqua regia extraction efficiency was sample mineralogy. The aqua regia leach procedure was applied to a range of samples that had been independently analysed by NiS fire assay as well as appropriate reference materials. This extraction procedure, with direct analysis of leachates by ICP-MS, was also used as the primary technique for characterising the homogeneity of two new chromitite reference materials, CHR-Pt+ and CHR-Bkg.

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