Abstract：The accurate determination of selenium in zinc slag is of great significance for its recycle. The sample was treated with HNO3-HClO4-HF-H2SO4 system by microwave digestion. Then the sample solution was steamed on the electric heating plate until the volume remained 2-3 mL followed by extraction with aqua regia. Consequently, a method for determination of selenium in zinc slag was established by hydride generation atomic fluorescence spectrometry(HG-AFS). The results showed that the mass concentration of selenium in range of 2-16 μg/L had a good linear relationship with its corresponding fluorescence intensity. The correlation coefficient was 0.999 7. The limit of detection of the method was 0.01 μg/g, and limit of quantification was 0.03 μg/g. The statistical analysis of coexisting elements contents in a large number of zinc slag samples was conducted. It was found that the main components in zinc slag were iron, zinc, lead, and aluminum. The interference tests indicated that the coexisting elements in samples had no interference with the determination. Three zinc slag samples with different contents of selenium were used for tests of precision and recovery according to the proposed method. The relative standard deviations(RSD, n=12) of the determination results were between 1.2% and 2.0%, and the recoveries were between 93% and 101%. The content of selenium in zinc slag samples with mass fraction of 2.35-100 μg/g was determined, and the results were basically consistent with those obtained by HG-AFS with alkali fusion.
魏军, 胡艳巧, 刘爱琴, 李丹, 刘俊妙, 陈超. 微波消解-氢化物发生原子荧光光谱法测定锌渣中硒[J]. 冶金分析, 2023, 43(12): 67-72.
WEI Jun, HU Yanqiao, LIU Aiqin, LI Dan, LIU Junmiao, CHEN Chao. Determination of selenium in zinc slag by hydride generation atomic fluorescence spectrometry with microwave digestion. , 2023, 43(12): 67-72.
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