Determination of precious metal elements in lead concentrate by inductively coupled plasma mass spectrometry with tin fire assay
LI Zhi-wei1,2, HUANG Jie1,2, SUN Yong1,2, CHEN Chong-ke1,2, WANG Jun-yu1,2
1. Henan Rock Mineral Testing Centers,Zhengzhou 450012, China; 2. Key Lab of Ministry of Land and Resources Analysis and Exploration of Precious Metals, Zhengzhou 450012, China
Abstract：There are many reports on the analysis of Au and Ag in lead concentrate. But the analysis of platinum group elements is very difficult. At present, the commonly used lead fire assay and nickel matte fire assay cannot meet the requirements of simultaneous analysis of 8 precious metal elements in lead concentrate. Tin fire assay enrichment was adopted. The Sn buckle was dissolved with hydrochloric acid. The precious metal precipitates were dissolved with aqua regia, and eight precious metal elements including Pt, Pd, Os, Ir, Ru, Rh, Au and Ag in lead concentrate were simultaneously analyzed by inductively coupled plasma mass spectrometry (ICP-MS). The components for assaying in experiments included 20g of Sn powder, 10g of Fe powder, 20g of Na2CO3, 20g of K2CO3, 5g of SiO2, 30g of borax, 3g of flour, 10g of NaNO3 and 5g of CaF2. The Sn buckle obtained was good when the melting temperature was 1100℃. Moreover, NaNO3 could adjust the redox reaction of assaying flux system, and the Fe powder could reduce the proportion of lead into Sn buckle. 195Pt, 105Pd, 189Os, 193Ir, 101Ru, 103Rh (the determination of Pb was required for the elemental correction), 197Au and 109Ag were selected as the analyte isotopes. Meanwhile, Lu (20ng/mL) was employed as the internal standard element to eliminate the influence of matrix effect and signal drift. The mass concentration of platinum group elements in certain range had good linear relationship with the corresponding spectral intensity. The limit of detection was 0.028-98ng/g. The accuracy tests were conducted using actual sample of lead concentrate. The relative standard deviations (RSD, n=6) of determination results were between 1.4% and 5.4%. The spiked recoveries were between 96% and 104%. The determination results of lead concentrate sample according to experimental method were in good agreement with those obtained by other methods.
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LI Zhi-wei, HUANG Jie, SUN Yong, CHEN Chong-ke, WANG Jun-yu. Determination of precious metal elements in lead concentrate by inductively coupled plasma mass spectrometry with tin fire assay. , 2020, 40(7): 22-28.
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