Abstract：During the enrichment of gold, platinum, and palladium in high nickel matte by lead fire assay, the smelting enrichment and cupellation effect of lead fire assay are seriously affected due to the high content of nickel and copper in high nickel matte. The matrix components of nickel and copper in high nickel matte were dissolved and separated using hydrochloric acid in experiments. The residue containing precious metals was further enriched and separated by wrap lead cupelling method. The accurate determination of gold, platinum, and palladium in high nickel matte by lead fire assay-inductively coupled plasma atomic emission spectrometry (ICP-AES) was finally realized. The effect of hydrochloric acid dosage, the lead foil dosage, the cupel type, cupellation loss, the addition amount of silver, and the analytical lines on the determination results were discussed. The results showed that the matrix components including nickel and copper in 5 g of high nickel matte sample could be fully dissolved with 80 mL hydrochloric acid. The residue was collected with 0.45 μm membrane and then wrapped in 6.0 g of lead foil after adding 5 mg of silver. The cupellation was conducted in magnesia cupel at 950 ℃. Lead and few sulfides of base metals were oxidized and separated without loss of gold, platinum, and palladium. The formed silver granule was decomposed with mixed acid. Silver was separated in the form of silver chloride precipitate and had no interference with the determination. In the medium of aqua regia (1+9), the contents of gold, platinum, and palladium were determined by ICP-AES using Au 267.595 nm, Pt 265.945 nm and Pd 340.458 nm as the analytical lines. The correlation coefficients of calibration curves of elements were all greater than 0.999. The limits of detection for gold, platinum, and palladium were 0.067 μg/g(Au),0.085 μg/g(Pt) and 0.107 μg/g(Pd), respectively. The proposed method was applied for the determination of gold, platinum, and palladium in high nickel matte. The relative standard deviations (RSD, n=7) of determination results were between 2.8% and 5.9%. The found results were basically consistent with those obtained by the industrial standard method (YS/T 252.8-2020).
邵坤, 范建雄, 李刚, 赵改红. 铅试金-电感耦合等离子体原子发射光谱法测定高镍锍中金铂钯[J]. 冶金分析, 2021, 41(10): 49-56.
SHAO Kun, FAN Jianxiong, LI Gang, ZHAO Gaihong. Determination of gold, platinum and palladium in high nickel matte by inductively coupled plasma atomic emission spectrometry with lead fire assay. , 2021, 41(10): 49-56.
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