Abstract：Thallium in wolframite could cause soil and water pollution. The content of thallium in wolframite must be detected before exploitation. The sample was decomposed by fusion method with sodium peroxide. The decomposition product was leached with 30 mL of nitric acid. 205Tl was selected as the determination isotope. Thus, an analysis method of thallium in wolframite by inductively coupled plasma mass spectrometry (ICP-MS) was established with 10 ng/mL of iridium as internal standard. The dosage of sodium peroxide and fusion time were optimized. It was found that the thallium in 0.3 g of sample could be fully leached by nitric acid after fusion with 2.5 g of sodium peroxide at 700 ℃ for 20 min. Under the optimized experimental conditions, the correlation coefficient of calibration curve was 0.999 9 with linear range of 0.05-10 ng/mL. The limit of detection was 0.03 μg/g, and the limit of quantification was 0.099 μg/g. The content of thallium in wolframite samples was determined according to the proposed method. The relative standard deviations (RSDs, n=11) of determination results were less than 3%. The proposed method was applied in determination of thallium in the certified reference materials of tungsten ore for composition analysis. The relative errors between the determination results and the certified values were less than 5%. Wolframite samples were treated with acid digestion method, and the insoluble substance was further fused with sodium peroxide. The solution obtained by two decomposition was merged and determined by flame atomic absorption spectrometry. The results were consistent with the proposed method.
罗芝雅, 王贵超, 刘荣丽, 罗勉, 石雪峰. 过氧化钠熔融-电感耦合等离子体质谱法测定黑钨矿中铊[J]. 冶金分析, 2022, 42(3): 47-51.
LUO Zhiya, WANG Guichao, LIU Rongli, LUO Mian, SHI Xuefeng. Determination of thallium in wolframite by inductively coupled plasma mass spectrometry after fusion with sodium peroxide. , 2022, 42(3): 47-51.
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