微波消解-电感耦合等离子体质谱法测定氧化铟锡靶材中13种痕量杂质元素

氧化铟锡中杂质元素的含量是衡量其产品性能的重要参数。采用盐酸以微波消解法处理样品,以Cs为内标,氩气模式下测定²⁴Mg、²⁷Al、⁵²Cr、⁵⁸Ni、⁶³Cu、⁶⁴Zn、⁹⁰Zr、²⁰⁸Pb、²⁰⁵Tl、¹¹¹Cd,氢气碰撞反应池模式测定²⁸Si、⁴⁰Ca、⁵⁶Fe,实现了电感耦合等离子体质谱法(ICP-MS)对氧化铟锡靶材(ITO)中镁、铝、硅、钙、铬、铁、铜、镍、锌、锆、镉、铅、铊等13种痕量杂质元素的测定。实验表明,当氧化铟锡基体质量浓度为1.00mg/mL时,基体效应可忽略;13种杂质元素在1.0~100ng/mL范围内线性良好,线性相关系数均大于0.9990。方法检出限为0.002~0.15μg/g,测定下限为0.007~0.50μg/g。将方法应用于氧化铟锡靶材样品中13种痕量杂质元素的分析,相对标准偏差(RSD,n=7)均小于5%,加标回收率为88%~114%。采用实验方法对氧化铟锡靶材样品进行分析,并与电感耦合等离子体原子发射光谱法(ICP-AES)进行比对,二者测定值基本一致。

Determination of thirteen trace impurity elements in indium tin oxide target material by microwave digestion-inductively coupled plasma mass spectrometry

The content of impurity elements in indium tin oxide (ITO) is an important parameter to measure the product performance. The sample was treated in hydrochloric acid by microwave digestion. Cs was selected as the internal standard. ²⁴Mg, ²⁷Al, ⁵²Cr, ⁵⁸Ni, ⁶³Cu, ⁶⁴Zn, ⁹⁰Zr, ²⁰⁸Pb, ²⁰⁵Tl and ¹¹¹Cd were determined under argon mode. The content of ²⁸Si, ⁴⁰Ca and ⁵⁶Fe was determined under hydrogen collision reaction cell mode. The determination of 13 trace impurity elements (including magnesium, aluminum, silicon, calcium, chromium, iron, copper, nickel, zinc, zirconium, cadmium, lead and thallium) in ITO target material by inductively coupled plasma mass spectrometry (ICP-MS) was realized. The experiments showed that the matrix effect could be ignored when the mass concentration of ITO matrix was 1.00mg/mL. The linearity was good for 13 impurity elements in range of 1.0-100ng/mL and the linear correlation coefficients were all higher than 0.9990. The detection limit was 0.002-0.15μg/g. The low limit of determination was 0.007-0.50μg/g. The proposed method was applied for the analysis of 13 trace impurity elements in indium tin oxide target material sample. The relative standard deviation (RSD, n=7) were all less than 5%. The recoveries were between 88% and 114%. The indium tin oxide target material sample was analyzed according to the experimental method. The found results were basically consistent with those obtained by inductively coupled plasma atomic emission spectrometry (ICP-AES).