Determination of trace gold,platinum,palladium,ruthenium, rhodium and iridium in geochemical sample by graphite furnace atomic absorption spectrometry with bismuth fire assay
YAO Mingxing1,2,3, WANG Wei*1,2,3, MAO Xiangju1,2,3, GUO Xiaorui1,2,3, WANG Tiantian1,2,3, NI Wenshan1,2,3
1. Zhengzhou Institute of Multipurpose Utilization of Mineral Resources,CAGS, Zhengzhou 450006, China; 2. China National Engineering Research Center for Utilization of Industrial Minerals, Zhengzhou 450006, China; 3. Key Laboratory for Polymetallic Ores' Evaluation and Utilization,MNR, Zhengzhou 450006, China
Abstract：The abundance of Au, Pt, Pd, Ru, Rh and Ir in geochemical samples is very low and the distribution is nonuniform. It is difficult to accurately determine their contents due to nugget effect. Based on the characteristics that Bi could form alloys or inter-compounds with Au, Pt, Pd, Ru, Rh, Os and Ir at high temperature, Bi2O3 was employed as a collector for the separation and enrichment of precious metals, and the precious metals in sample were enriched in bismuth granule in mg grade. After the bismuth granule was treated by microwave digestion with 10 mL of 40% aqua regia (V/V), the contents of precious metals in digestion solution were determined by graphite furnace atomic absorption spectrometry (GF-AAS). Consequently, a method for determination of trace Au, Pt, Pd, Ru, Rh and Ir in geochemical samples was established. The influence of remaining bismuth amount on the determination results of elements was investigated. The results showed that the influence was insignificant when the remaining bismuth amount was in range of 5-20 mg. The influence of cooling method of magnesia cupel after bismuth-remaining protection cupellation was discussed. The results showed that the complete bismuth granule could be obtained after gradual condensation under the following conditions: half of cupel was immersed in water for cooling; only cupel was contacted with cooling water while the liquid bismuth did not contact with water. Under the selected optimal experimental conditions, the calibration curves were fitted using the absorbance of Au, Pt, Pd, Ru, Rh, Ir and their corresponding mass concentrations in range of 0.01-50 ng/mL with least square method of quadratic equation. The determination coefficients of calibration curves were between 0.999 6 and 0.999 9. The characteristic concentrations were between 0.20 and 1.90 ng/mL. The proposed method was applied for determination of Au, Pt, Pd, Ru, Rh and Ir in certified reference materials of olivine, chromite, lean palladium ore, and soil. The results were consistent with the certified values. The experimental method was applied for the analysis of manganese-nickel polymetallic ore, sulfide ore and soil sample in surroundings of mining areas. The relative standard deviations (RSD, n=5) of determination results were between 3.6% and 6.1%. The recoveries were between 92% and 108%.
姚明星, 王威, 毛香菊, 郭晓瑞, 王甜甜, 倪文山. 铋试金-石墨炉原子吸收光谱法测定地球化学样品中痕量金铂钯钌铑铱[J]. 冶金分析, 2022, 42(9): 40-47.
YAO Mingxing, WANG Wei, MAO Xiangju, GUO Xiaorui, WANG Tiantian, NI Wenshan. Determination of trace gold,platinum,palladium,ruthenium, rhodium and iridium in geochemical sample by graphite furnace atomic absorption spectrometry with bismuth fire assay. , 2022, 42(9): 40-47.
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