Determination of gold, silver, platinum and palladium in geological samples by inductively coupled plasma mass spectrometry with sealed dissolution
LIU Jun1,2,YAN Hong-ling1,2,LIAN Wen-li1,2,CHEN Hao-feng1,2,WANG Lin*1,2,YU Ya-hui1,2
1.Henan Province Rock and Mineral Testing Center,Zhengzhou 450012,China; 2.Ministry of Land and Resources Key Laboratory of Precious Metals Analysis Technology,Zhengzhou 450012,China
Abstract：After the sample was dissolved in high pressure sealed system, a direct determination method of Au, Ag, Pt and Pd in geological samples was established by inductively coupled plasma mass spectrometry (ICP-MS). The experimental results showed that, 10.00 g of geological samples could be fully dissolved by adding 30 mL of HCl, 5.0 mL of H2O2 and 2.0 g of KClO3 in 200 mL high pressure sealed tank, which was put in constant temperature digital drying oven at 160 ℃ for 6 h. The sample digestion solution was separated and enriched with novel composite adsorbent composed of activated carbon, modified activated carbon and 717 anion exchange resin. Then the mass spectrometry interference was eliminated by selecting proper isotopes or mathematic correction. Consequently, the determination of Au, Ag, Pt and Pd in geological samples was realized by ICP-MS. The correlation coefficients of calibration curves of Au, Ag, Pt and Pd were not less than 0.999 5. The detection limit of Au, Ag, Pt and Pd was 0.097, 0.14, 0.17 and 0.082 ng/g, respectively. The proposed method was applied to the determination of Au, Ag, Pt and Pd in geochemical primary reference materials of platinum family element, and the results were consistent with the certified values. The relative standard deviation (RSD, n=12) was not more than 14.2%. The experimental method was applied to the determination of Au, Ag, Pt and Pd in geochemical primary reference materials and actual samples, and the recoveries were between 92% and 110%.
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