氢化物发生-原子荧光光谱法测定金属锰粉中硒

用硝酸溶解样品, 控制盐酸酸度为0.72 mol/L, 硼氢化钾浓度为10.0 g/L, 建立了氢化物发生-原子荧光光谱法(HG-AFS)测定金属锰粉中硒的方法。研究了样品溶液中共存离子的干扰, 结果表明, Mn²⁺、Al³⁺、Fe³⁺、Si、Cu²⁺、Mg²⁺、Pb²⁺、Ca²⁺对硒的测定均不产生干扰。方法的线性范围为0.20~100.0 μg/L, 相关系数为0.999 6, 仪器检出限为0.059 6 μg/L。方法用于金属锰粉样品中硒的测定, 结果与电感耦合等离子体原子发射光谱法相符, 相对标准偏差(RSD, n=4)为1.9%～3.4%, 加标回收率为95%~102%。

Determination of selenium in manganese powders by hydride generation-atomic fluorescene spectrometry

After the sample was dissolved in nitric acid, a method for determination of selenium in manganese powder was established by hydride generation-atomic fluorescence spectrometry (HG-AFS) with the acidity of hydrochloric acid at 0.72 mol/L and the concentration of potassium borohydride of 10.0 g/L. The interference from the coexisting ions in the sample solution was investigated and it was found that Mn²⁺, Al³⁺, Fe³⁺, Si , Cu²⁺, Mg²⁺, Pb²⁺ and Ca²⁺ did not interfere with the determination of selenium. The linear range of this method was 0.20-100.0 μg/L with correlation coefficient of 0.999 6 and the instrument detection limit was 0.059 6 μg/L. When the method was applied to determination of selenium in manganese powder samples, the results were consistent with those obtained by inductively coupled plasma atomic emission spectrometry, the relative standard deviations (n=4)were in the range of 1.9%-3.4% and the recoveries were in the range of 95%-102%.