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    电感耦合等离子体质谱法测定高纯钨粉中13种痕量元素

    Determination of 13 Trace Elements in High Purity Tungsten Powder by Inductively Coupled Plasma Mass Spectrometry

    • 摘要: 取0.500 0 g高纯钨粉样品置于聚四氟乙烯烧杯中,加入4 mL 50%(体积分数)硝酸溶液和5 mL氢氟酸,于90 ℃电热板上加热溶解,冷却至室温,转移至100 mL塑料容量瓶中,用水定容,混匀,移取5 mL,加入1 mL氢氟酸,用水定容至50 mL,混匀,采用电感耦合等离子体质谱法(ICP-MS)测定溶液中13种痕量元素,其中镁、铝在标准模式下测定,铬、锰、铁、钴、铜、镍、砷、钼、锡、锑、铅在动能歧视碰撞模式下测定,通过标准加入法结合在线加入内标法降低基体干扰。结果显示,13种目标元素的质量浓度在一定范围内和对应的信号强度与内标信号强度的比值呈线性关系,检出限(3s)为0.01~0.30 µg·g−1。实际高纯钨粉样品测定值的相对标准偏差(n=6)均小于10%,按照标准加入法进行回收试验,回收率为92.0%~106%。方法用于分析实际高纯钨粉样品,各目标元素的测定值与辉光放电质谱法的基本一致。

       

      Abstract: The high purity tungsten powder sample (0.500 0 g) was taken and placed in a polytetrafluoroethylene beaker, and 4 mL of 50% (volume fraction) nitric acid solution and 5 mL of hydrofluoric acid were added. The mixture was heated on an electric hot plate at 90 ℃ to dissolve, and then cooled to room temperature. The solution was transferred to a 100 mL-plastic volumetric flask, made its volume up to 100 mL with water, and mixed well. 5 mL of the solution was taken, and 1 mL of hydrofluoric acid was added. The solution was made its volume up to 50 mL with water and mixed well, and 13 trace elements in the solution were determined by inductively coupled plasma mass spectrometry. Magnesium and aluminum were determined in standard mode, while chromium, manganese, iron, cobalt, copper, nickel, arsenic, molybdenum, tin, antimony, and lead were determined in kinetic energy discrimination collision mode. Matrix interference was reduced by the standard addition method combined with online internal standard addition method. As shown by the results, linear relationships between the ratios of the corresponding signal intensity to the internal standard signal intensity and mass concentrations of the 13 target elements were kept in definite ranges, with detection limits (3s) in the range of 0.01−0.30 µg·g−1. RSDs (n=6) of the determined values of actual high purity tungsten powder samples were less than 10%. Test for recovery was made according to the standard addition method, giving results in the range of 92.0%−106%. The method was applied to the analysis of an actual high purity tungsten powder sample, and the determined values of target elements were basically consistent with those obtained by glow discharge mass spectrometry.

       

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