Determination of gold, platinum and palladium in porphyry copper ore by inductively coupled plasma mass spectrometry with lead fire assay
SHAO Kun1,2,3, ZHU Zhimin1,2,3, FAN Jianxiong1,2,3, LI Gang1,2,3
1. Institute of Multipurpose Utilization of Mineral Resources, Chinese Academy of Geological Sciences, Chengdu 610041, China; 2. Innovation Center for Comprehensive Utilization Engineering Technology of Strategic Mineral, Ministry of Natural Resources, Chengdu 610041, China; 3. Technical Research Center for Comprehensive Utilization of Metal and Mineral Resources,China Geological Survey, Chengdu 610041, China
Abstract：The accurate determination of Au, Pt and Pd in porphyry copper ore is of great significance to improve its comprehensive utilization level. However, the contents of associated precious metals in porphyry copper ore are low, and the matrix is complex, leading to high difficulty in determination. A new separation and preconcentration method including porcelain disc melting and two-step cupellation was proposed with lead as the trapping agent. 197Au,195Pt and 106Pd were selected as the isotopes for determination. 115In was used as internal standard for the correction of 106Pd, and 185Re was used as internal standard for the correction of 197Au and 195Pt. Consequently, a method for determination of Au, Pt and Pd in porphyry copper ore by inductively coupled plasma mass spectrometry (ICP-MS) with lead fire assay preconcentration was established. Through the tests of assay ingredient composition, the assay ingredient was determined to be composed of lead oxide, boric acid, sodium carbonate and flour with the mass ratio of 5∶2∶2∶1. The sample mass, ingredient mass, porcelain disc volume and melting temperature were optimized as follows: the sample mass was 5 g, the ingredients mass was 50 g, the porcelain disc volume was 40 mL, and the melting temperature was 1 000 ℃. The cupellation test showed that the first cupellation (950 ℃) was directly conducted in porcelain disc by opening the furnace door to remove partial lead. After the lead button was covered with the slag, the lead button was taken out and transferred to magnesia cupel for further cupellation (920 ℃) to remove the residual partial lead. Thus, the satisfactory silver granule was obtained. The cupellation interference test showed that, although some elements, which were easily reduced or dissolved in lead, such as Cu, Ni, Bi, As, Sb, S, Se and Te, would also enter lead button, their interference with the cupellation process could be ignored. The mass spectrometry interference test showed that the interference of residual Cu, Ni, Se and Ag in test solution could be also ignored. The correlation coefficients of calibration curves for all elements were higher than 0.999. The limit of detection for Au, Pt and Pd was 0.10 ng/g, 0.05 ng/g, and 0.08 ng/g, respectively. The limits of quantification for Au, Pt and Pd was 0.33 ng/g, 0.17 ng/g, and 0.27 ng/g, respectively. The contents of Au, Pt and Pd in porphyry copper ore samples were determined according to the experimental method. The relative standard deviations (RSD, n=7) of determination results were between 2.7% and 9.5%. The spiked recoveries were between 96% and 107%. The results were basically consistent with those obtained by the national standard of GB/T 20899.1-2019 for determination of Au by flame atomic absorption spectrometry with fire assay, and the industrial standard of DZ/T 0279.31-2016 for determination of Pt and Pd by inductively coupled plasma mass spectrometry with fire assay.
邵坤, 朱志敏, 范建雄, 李刚. 铅试金-电感耦合等离子体质谱法测定斑岩铜矿中金铂钯[J]. 冶金分析, 2022, 42(12): 36-44.
SHAO Kun, ZHU Zhimin, FAN Jianxiong, LI Gang. Determination of gold, platinum and palladium in porphyry copper ore by inductively coupled plasma mass spectrometry with lead fire assay. , 2022, 42(12): 36-44.
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