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
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摘要
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~(24 )Mg、~(27 )Al、~(52)Cr、~(58 )Ni、~(63)Cu、~(64)Zn、~(90)Zr、~(208)Pb、~(205 )Tl、~(111 )Cd,氢气碰撞反应池模式测定~(28)Si、~(40)Ca、~(56)Fe,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。
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.~(24 )Mg,~(27 )Al,~(52)Cr,~(58 )Ni,~(63)Cu,~(64)Zn,~(90)Zr,~(208)Pb,~(205 )Tl and ~(111)Cd were determined under argon mode.The content of ~(28)Si,~(40)Ca and ~(56)Fe 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 0.999 0.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).
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.~(24 )Mg,~(27 )Al,~(52)Cr,~(58 )Ni,~(63)Cu,~(64)Zn,~(90)Zr,~(208)Pb,~(205 )Tl and ~(111)Cd were determined under argon mode.The content of ~(28)Si,~(40)Ca and ~(56)Fe 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 0.999 0.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).
引文
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[2]中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.GB/T 20510-2017氧化铟锡靶材[S].北京:中国标准出版社,2008.
[3]黄瑾,郭斌斌,郑清洪.辉光放电质谱法测定氧化铟锡靶材中的元素含量[J].分析试验室,2016,35(7):765-768.HUANG Jin,GUO Bin-bin,ZHENG Qing-hong.Impurities concentration detection in ITO target by glow discharge mass spectrometry[J].Chinese Journal of Analysis Laboratory,2016,35(7):765-768.
[4]张红梅,陈锐.ITO粉及ITO靶材中铟的测定-EDTA容量法[J].稀有金属,2003,27(1):188-190.ZHANG Hong-mei,CHEN Rui.Determination of indium in ITO powder and ITO target by EDTA titration[J].Chinese Journal of Rare Metals,2003,27(1):188-190.
[5]吴文启,黄煦,李奋,等.EDTA滴定法测定废铟锡氧化物靶材中铟[J].冶金分析,2007,27(11):37-39.WU Wen-qi,HUANG Xu,LI Fen,et al.Determination of indium in waste indium-tin oxide target by EDTA titration[J].Metallurgical Analysis,2007,27(11):37-39.
[6]曾艳,武明丽.EDTA滴定法测定铟锡氧化物废靶粉中铟的含量[J].化学分析计量,2017,26(5):91-99.ZENG Yan,WU Ming-li.Determination of indium in ITOwaste target powder by EDTA titration[J].Chemical A-nalysis and Meterage,2017,26(5):91-99.
[7]孙洪涛,王晓艳,邓培.ICP-AES法测定氧化铟-氧化锡(ITO)超细复合粉末中痕量杂质[J].宁夏工程技术,2003,2(3):232-234.SUN Hong-tao,WANG Xiao-yan,DENG Pei.Determination of trace impurities in In2O3-SnO2(ITO)ultrafine composite powder by ICP-AES[J].Ningxia Engineering Technology,2003,2(3):232-234.
[8]王志萍,孙洪涛,王巧.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[J].冶金分析,2018,38(5):60-65.WANG Zhi-ping,SUN Hong-tao,WANG Qiao.Determination of eleven trace impurity elements in indium tin oxide target material by inductively coupled plasma atomic emission spectrometry after microwave digestion[J].Metallurgical Analysis,2018,38(5):60-65.
[9]黄子敬,陈孟君,邓华阳,等.微波消解-ICP-MS混合模式测定动植物源食品中11种金属元素[J].分析试验室,2017,36(1):24-28.HUANG Zi-jing,CHEN Meng-jun,DENG Hua-yang,et al.Determination of 11trace elements in animal and plant origin food by microwave digestion with ICP-MS in mixed mode[J].Chinese Journal of Analysis Laboratory,2017,36(1):24-28.
[10]张立峰,张秀艳,张翼明,等.电感耦合等离子体质谱法测定镧镁合金中稀土杂质[J].冶金分析,2014,34(6):33-37.ZHANG Li-feng,ZHANG Xiu-yan,ZHANG Yi-ming,et al.Determination of rare earth impurities in lanthanummagnesium alloy by inductively coupled plasma mass spectrometry[J].Metallurgical Analysis,2014,34(6):33-37.
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