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    电感耦合等离子体质谱法测定高纯五氧化二钽中20种痕量杂质元素

    ICP-MS Determination of 20 Trace Impurity Elements in High Purity Tantalum Pentoxide

    • 摘要: 将五氧化二钽样品在105 ℃下烘干2 h,冷却至室温后,取样品0.500 0 g,加入氢氟酸5 mL,硝酸2.5 mL,按程序升温微波消解,用水定重至50.0 g。应用动态反应池技术消除多原子离子对铁元素的干扰,甲烷反应气流量为0.2 mL·min-1,Rpq为0.80。以标准加入法补偿基体效应制作标准曲线,采用电感耦合等离子体质谱法测定20种杂质元素的含量。各元素的检出限(3s)在0.009~0.53 μg·g-1之间,用标准加入法做回收试验,测得回收率在90.0%~116%之间,测定值的相对标准偏差(n=11)在1.8%~17%之间。

       

      Abstract: Tantalum pentoxide sample was dried for 2 h at 105 ℃. After cooling to room temperature, the sample (0.500 0 g) was treated with 5 mL of HF and 2.5 mL of HNO3 in a microwave digestor under programmed temperature elevation. Water was added to the digested solution to make the mass of solution attained to 50.0 g. The solution was used for ICP-MS determination of the 20 impurity-elements. Dynamic reaction cell technology was adopted to eliminate the interferences of polyatomic ions to Fe, with a flow-rate of 0.2 mL·min-1 for CH4 reaction gas and Rpq of 0.80, and the standard addition method was used to correct the matrix effect in preparation of standard curves. Values of detection limits (3s) found for the 20 elements were in the range of 0.009-0.53 μg·g-1. Test for recovery was made by standard addition method, giving results in the range of 90.0%-116%, with RSDs (n=11) ranged from 1.8% to 17%.

       

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