动态反应池-电感耦合等离子体质谱法测定高纯锑中23种痕量杂质元素

Determination of twenty-three trace impurity elements in high purity antimony by dynamic reaction cell inductively coupled plasma mass spectrometry

建立了动态反应池-电感耦合等离子体质谱法测定高纯锑中Mg、Al、Si、Ca、Fe等23种痕量元素的分析方法。优化选择了测定同位素;采用以H2作为动态反应池反应气消除了Si、Ca和Fe的质谱干扰,并确定最佳H2流量为4mL/min;采用Rh为内标元素补偿了仪器信号漂移和基体效应。方法测定下限介于0.037～0.77ng/mL,加标回收率在92%～112%之间,相对标准偏差小于10%。该方法可以满足4N5高纯锑中23种痕量杂质元素的测定。

Twenty-three trace impurities in high purity antimony such as Mg,Al,Si,Ca and Fe were determined by dynamic reaction cell inductively coupled plasma mass spectrometry.The determination isotope was optimized and selected.The spectral interference of Si,Ca and Fe was eliminated with H2 as reaction gas of dynamic reaction cell.The optimal H2 flow rate was established as 4 mL/min.The instrumental signal shift and matrix effect were compensated with Rh as internal standard element.The lower limits of quantitation were in the range of 0.037-0.77 ng/mL,the recoveries of standard addition were 92 %-112 %,and the relative standard deviations（RSD） were smaller than 10 %.This proposed method could meet the requirements for the determination of twenty-three trace impurities in 4N5 high purity antimony.