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    标准加入法-电感耦合等离子体质谱法测定海绵钯中17种痕量杂质元素

    Determination of 17 Trace Impurity Elements in Sponge Palladium by Inductively Coupled Plasma Mass Spectrometry with Standard Addition Method

    • 摘要: 取海绵钯样品0.900 0 g,加入10 mL水润湿后,用10 mL体积比3∶1的盐酸-硝酸混合液于100 ℃溶解,用水定重至90 g。通过质谱干扰分析并结合同位素丰度确定了待测同位素,52Cr、56Fe、55Mn在动态反应池(DRC)模式下检测,其他元素的同位素均在标准模式下检测。在射频功率1 100 W、雾化气流量0.85 L·min-1等条件下,采用电感耦合等离子体质谱法(ICP-MS)测定海绵钯中17种痕量杂质元素,绘制各元素标准加入法的校准曲线,并用仪器软件设置为“外标法”模式的工作曲线,后续对其他海绵钯样品进行检测时可直接在此工作曲线下进行,不需要每个样品都进行标准加入。结果表明,17种元素的检出限(3s)为0.012~0.452 μg·g-1,按照标准加入法进行回收试验,回收率为93.0%~107%,测定值的相对标准偏差(n=11)小于8.0%。采用本方法和GB/T 1420-2015中的电感耦合等离子体原子发射光谱法对海绵钯样品进行对比分析,两种方法的测定结果基本一致。

       

      Abstract: The sponge palladium sample (0.900 0 g) was wet in 10 mL of water, and dissolved in 10 mL of a mixture of hydrochloric acid and nitric acid at a volume ratio of 3∶1 at 100 ℃. Water was added to the above solution to make the mass of solution attained to 90 g. The isotope to be tested was determined through mass spectrometry interference analysis combined with isotope abundance, and 52Cr, 56Fe, and 55Mn were detected in dynamic reaction cell (DRC) mode, while isotopes of other elements were detected in standard mode. 17 trace impurity elements in sponge palladium were determined by inductively coupled plasma mass spectrometry (ICP-MS) under the conditions of radio frequency power at 1 100 W and atomization gas flow at 0.85 L·min-1. The calibration curves for elements were drew by standard addition method, and the working curves were set through “external standard method” mode with instrument software. Subsequent testing for other sponge palladium samples could be directly carried out under those working curves, without standard addition method for each sample. As shown by the results, values of detection limit (3s) for 17 elements were in the range of 0.012-0.452 μg·g-1. Test for recovery was made by standard addition method, giving results in the range of 93.0%-107%, with RSDs (n=11) of the determined values less than 8.0%. The comparison analysis of sponge palladium samples by this method and inductively coupled plasma atomic emission spectrometry in GB/T 1420-2015 was carried out, and it was shown that the determined results obtained by the two methods were basically consistent.

       

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