GFAAS Determination of Trace Nickel in High Purity Indium with Ion-Exchange Separation
摘 要
高纯铟样品经盐酸溶解、阳离子交换树脂分离并将试液蒸发浓缩后,用石墨炉原子吸收光谱法测定其中的痕量镍。以0.7 mol·L-1盐酸溶液作为淋洗液进行离子交换,可把大部分铟基体及样品中痕量的共存离子分离除去,再用3.0 mol·L-1盐酸溶液洗脱镍并收集。镍的质量在300 pg以内与其吸光度呈线性关系,方法的检出限(3s)为15 pg。应用此法分析了3个高纯铟样品,测定值与电感耦合等离子体质谱法测定结果相符,加标回收率在95.2%~118%之间,测定值的相对标准偏差(n=8)在1.2%~18%之间。
Abstract
The sample of high purity indium was dissolved with hydrochloric acid. After separation with cation-exchange resin, trace amount of nickel in high purity indium was determined by GFAAS. After ion-exchange with 0.7 mol·L-1 hydrochloric acid solution as eluent, trace coexisting ion and most of indium in the sample were separated and removed, then nickel was eluted with 3.0 mol·L-1 hydrochloric acid solution and collected. Linear relationship between values of absorbance and mass of nickel was kept in the range within 300 pg, with detection limit (3s) of 15 pg. Three samples of high purity indium were analyzed by the proposed method, giving results in consistency with values given by ICP-MS, with values of recovery and RSD (n=8) in the ranges of 95.2%-118% and 1.2%-18%, respectively.
中图分类号 O657.31
所属栏目 工作简报
基金项目 广西出入境检验检疫局科技计划项目(2011K001)
收稿日期 2014/3/6
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联系人作者吴文启(ciqw@163.com)
备注吴文启(1956-),男,广西玉林人,高级工程师,主要从事化工、矿产、金属商品检验。
引用该论文: WU Wen-qi,LI Fen,LIAO Hong-mei,XIE Xiao-yan,SU Xin-yu. GFAAS Determination of Trace Nickel in High Purity Indium with Ion-Exchange Separation[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2015, 51(4): 450~453
吴文启,李奋,廖红梅,谢晓雁,苏信宇. 离子交换分离-石墨炉原子吸收光谱法测定高纯铟中痕量镍[J]. 理化检验-化学分册, 2015, 51(4): 450~453
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参考文献
【1】YS/T 264-2012高纯铟[S].
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【9】丁志英,张尼.石墨炉原子吸收光谱法测定氢化棉籽油中痕量镍[J].理化检验-化学分册, 2011,47(8):358-359.
【2】GRAZHALENE S, KARANDASHEV V, ZADNEPRUK L, et al. AAS-ETA, ICP-AES and ICP-MS analysis of high purity indium using matrix separation by analytical autoclaves of special design[J]. Fresenius′ Journal of Analytical Chemistry, 1996,355:297-299.
【3】刘红,李爱嫦,李继东.辉光放电质谱法测定高纯铟中痕量元素[J].分析试验室, 2012,31(5):10-12.
【4】覃祚明.电感耦合等离子体质谱法在高纯铟杂质元素分析中的应用[D].长沙:中南大学, 2009.
【5】冯先进.ICP-MS法测定铟中砷、铝、铜、镉、镍、铅、铊、锡和锌[J].有色金属, 2010,62(4):136-139.
【6】周锦帆.离子交换技术的研究方法[J].现代商检科技, 1993,3(4):46-53.
【7】孙汉文.原子吸收光谱分析技术[M].北京:中国科学技术出版社, 1992.
【8】谢华林,张萍,刘宏伟.萃取分离-石墨炉原子吸收光谱法测定金属硅中痕量镍[J].冶金分析, 2002,22(6):30-31.
【9】丁志英,张尼.石墨炉原子吸收光谱法测定氢化棉籽油中痕量镍[J].理化检验-化学分册, 2011,47(8):358-359.
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