Determination of selenium and tellurium in polymetallic ore by coprecipitation separation-inductively coupled plasma mass spectrometry
DONG Xue-lin1,2, JIA Zheng-xun1, WANG Hui-ping1, YUAN Yan1,2, FANG Jin-dong1,2
1.Hubei Province Geological Experimental Testing Center, Wuhan 430034,China; 2.Key Laboratory of Rare Mineral Experimental Technology,Ministry of Land and Resources,Wuhan 430034,China
Abstract：If selenium and tellurium in the polymetallic ore sample was determined directly after decomposition without effective pretreatment, the determination results would be inaccurate and the instrument would be contaminated because of the complicated matrix and the low abundance of selenium and tellurium in nature. The polymetallic ore sample was decomposed by nitric acid-hydrofluoric acid-perchloric acid. Arsenic, selenium and tellurium in the sample solution was reduced to simple substance by sodium hypophosphite with copper salt as contact agent medium in hydrochloric acid. The coprecipitation of selenium and tellurium with arsenic realized the separation of selenium and tellurium from other elements, eliminating the matrix effect. Finally, the precipitate was dissolved with hot nitric acid and determined by inductively coupled plasma mass spectrometry (ICP-MS). Thus, a determination method of selenium and tellurium in polymetallic ore was established. The results showed that the matrix effect, the fluctuation and drift of instrument signal could be corrected with cesium (133Cs) as internal standard. The correlation coefficients of calibration curves were both up to 0.999. The detection limit for selenium and tellurium was 0.004 and 0.003 ng/mL, respectively. The proposed method was applied to determination of polymetallic ore actual samples. The results were basically consistent with those obtained by hydride generation-atomic fluorescence spectrometry (HG-AFS). The proposed method was applied to determination of polymetallic ore certified reference material. The results were in good agreement with the certified values. The relative standard deviation (RSD, n=7) for selenium and tellurium was 1.2%-8.5% and 1.1%-6.2%, respectively.
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