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    电感耦合等离子体质谱法测定重晶石中的微量元素

    ICP-MS Determination of Trace Elements in Barite

    • 摘要: 重晶石样品(0.200 0~0.250 0 g)经氢氟酸(6 mL)、盐酸(3 mL)和硝酸(1 mL)溶样,蒸干,最后用盐酸(1+3)溶液4 mL溶解残渣,加水定容至100 mL。采用电感耦合等离子体质谱法测定其中锶、铝、钙、镁、钾、钠、铜、铅、锌等9种微量元素的含量。用一级标准物质(GBW 07811、GBW 07814、GWB 07812)绘制标准曲线,以铼为内标物。方法的检出限在2.2×10-7~1.51×10-6之间。方法用于实样分析,测定值的相对标准偏差(n=10)在2.2%~3.8%之间。应用此方法分析了4种重晶石标准物质(GBW 07813、GBW 07815、GBW 07816、GBW 07817),所得测定值与认定值相符。用标准加入法做方法的回收试验,测得回收率在90.0%~120%之间。

       

      Abstract: The barite sample (0.200 0-0.250 0 g) was dissolved with HF (6 mL), HCl (3 mL) and HNO3 (1 mL), and evaporated to dryness. The residue was taken up with 4 mL of HCl(1+3) and finally the solution was diluted to 100 mL with water, and the 9 trace elements, i.e. Sr, Al, Ca, Mg, K, Na, Cu, Pb and Zn in the solution were determined by ICP-MS. Standard curves were prepared with GB CRM′s (GBW 07811, GBW 07814, GWB 07812). Re was used as internal standard. Detection limits of the method found were in the range of 2.2×10-7-1.51×10-6. The proposed method was applied to the analysis of barite samples, giving values of RSD′s (n=10) in the range of 2.2%-3.8%. The proposed method was applied to the analysis of 4 barite CRM′s (GBW 07813, GBW 07815, GBW 07816, GBW 07817), giving results in consistency with the certified values. Test for recovery was performed by standard addition method, giving values of recovery in the range of 90.0%-120%.

       

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