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    微波消解-电感耦合等离子体质谱法测定高纯氮化铝粉中15种杂质元素的含量

    Determination of 15 Impurity Elements in High Purity Aluminum Nitride Powder by Inductively Coupled Plasma Mass Spectrometry with Microwave Digestion

    • 摘要: 建立了微波消解-电感耦合等离子体质谱法(ICP-MS)测定高纯氮化铝粉中15种杂质元素含量的方法。在样品0.10 g中加入3 mL硝酸,按微波消解程序消解样品,冷却后,用水定容至100 mL。通过氢气模式,以铯内标法校正基体效应,采用ICP-MS测定其中硼、镁、钾、钙、钛、钒、铬、锰、铁、镍、铜、锌、锆、钼、钨等15种杂质元素的含量。结果表明,各元素标准曲线的线性范围均为1.0~100.0 μg·L-1,相关系数均不小于0.999 0,检出限(3s)为0.02~0.07 μg·g-1。用建立的方法分析氮化铝样品,测定值的相对标准偏差(n=7)均小于5.0%,按标准加入法进行回收试验,回收率为88.0%~114%。与电感耦合等离子体原子发射光谱法(ICP-AES)进行方法比对,两种方法所得结果基本一致。

       

      Abstract: A method for determination of the 15 impurity elements in high purity aluminum nitride powder by inductively coupled plasma mass spectrometry (ICP-MS) with microwave digestion was established. Nitric acid of 3 mL was added into 0.10 g of the sample and the sample was digested by microwave digestion procedure. After cooling, the volume of the sample solution was made up to 100 mL with water. The matrix effect was corrected by Cs internal standard method, and the contents of 15 impurity elements, including B, Mg, K, Ca, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Zr and Mo, were determined by ICP-MS. As shown by the results, the linear range of the standard curve of each element was 1.0-100.0 μg·L-1, and the correlation coefficient of the standard curve of each element was not less than 0.999 0, with detection limits (3s) in the range of 0.02-0.07 μg·g-1. Aluminum nitride samples were analyzed by the proposed method, with RSDs (n=7) of the determined value less than 5.0%. Test for recovery was made by standard addition method, giving values of recovery in the range of 88.0%-114%. Compared with inductively coupled plasma atomic emission spectroscopy (ICP-AES), the results obtained by the two methods were basically consistent.

       

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