微波消解-电感耦合等离子体原子发射光谱法测定氧化铟锡靶材中11种痕量杂质元素

使用盐酸并采用微波消解处理样品,选择Fe 238.204nm、Ca 317.933nm、Mg 285.213nm、Al 396.152 nm、Cd 214.438nm、Cr 267.716nm、Cu 324.754nm、Ni 221.647nm、Pb 220.353nm、Si 251.611nm、Tl 190.856nm为分析谱线,采用基体匹配法绘制校准曲线消除基体效应的影响,使用电感耦合等离子体原子发射光谱法(ICP-AES)同时测定铁、钙、镁、铝、镉、铬、铜、镍、铅、硅、铊,从而建立了氧化铟锡靶材中铁、钙、镁、铝、镉、铬、铜、镍、铅、硅、铊等痕量杂质元素的分析方法。各元素校准曲线线性相关系数均大于0.9995;方法中各元素的测定下限为0.30~1.78μg/g。按照实验方法测定2个氧化铟锡靶材样品中铁、钙、镁、铝、镉、铬、铜、镍、铅、硅、铊,结果的相对标准偏差(RSD,n=11)为1.1%~8.2%,加标回收率为92%~108%。

Determination of eleven trace impurity elements in indium tin oxide target material by inductively coupled plasma atomic emission spectrometry after microwave digestion

The sample was treated by microwave digestion in hydrochloric acid. Fe 238.204nm, Ca 317.933nm, Mg 285.213nm, Al 396.152nm, Cd 214.438nm, Cr 267.716nm, Cu 324.754nm, Ni 221.647nm, Pb 220.353nm, Si 251.611nm and Tl 190.856nm were selected as the analytical lines. The calibration curves were prepared by matrix matching method to eliminate the influence of matrix effect. The contents of iron, calcium, magnesium, aluminum, cadmium, chromium, copper, nickel, lead, silicon and thallium were simultaneously determined by inductively coupled plasma atomic emission spectrometry (ICP-AES). Consequently the analysis method of impurity elements (including iron, calcium, magnesium, aluminum, cadmium, chromium, copper, nickel, lead, silicon and thallium) in indium tin oxide target material was established. The linear correlation coefficients of calibration curves were higher than 0.9995. The low limit of determination of elements was in range of 0.30-1.78μg/g. The proposed method was applied for the determination of iron, calcium, magnesium, aluminum, cadmium, chromium, copper, nickel, lead, silicon and thallium in two samples of indium tin oxide target material. The relative standard deviations (RSD, n=11) of measured results were between 1.1% and 8.2%, and the recoveries were between 92% and 108%.