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采用电感耦合等离子体-光学发射光谱法(ICP-OES)测定高纯镍中痕量砷、硼、铋、镓、锗、磷、铅、锑、硒、硅和碲。

Determination of traces of As, B, Bi, Ga, Ge, P, Pb, Sb, Se, Si and Te in high-purity nickel using inductively coupled plasma-optical emission spectrometry (ICP-OES).

机构信息

National Centre for Compositional Characterization of Materials, Bhabha Atomic Research Centre, ECIL-Post, Hyderabad-500062, India.

National Centre for Compositional Characterization of Materials, Bhabha Atomic Research Centre, ECIL-Post, Hyderabad-500062, India.

出版信息

Talanta. 2015 Jan;131:505-9. doi: 10.1016/j.talanta.2014.08.026. Epub 2014 Aug 19.

Abstract

A method has been developed for the determination of traces of arsenic, boron, bismuth, gallium, germanium, phosphorus, lead, antimony, selenium, silicon and tellurium in nickel matrix. The sample was dissolved in HClO4 (~ 150°C) and nickel was settled as crystalline nickelperchlorate [Ni(ClO4)2] on cooling. The mixture was ultrasonicated and after the separation of Ni(ClO4)2, analytes of interest were determined in the supernatant using ICP-OES. Similarly, it was also found that, after the dissolution of nickel in perchloric acid, when the solution temperature was maintained at ~ 100°C, long needle like crystals of nickel perchlorate were formed. The crystals were separated from the mixture and trace elements in the supernatant were determined using ICP-OES. In both methods the matrix removal was >99% and the recoveries of analytes were in the range 92-97%. The limits of detection for As, B, Bi, Ga, Ge, P, Pb, Sb, Se, Si and Te were found to be 0.18, 0.21, 0.07, 0.06, 0.25, 0.11, 0.09, 0.10, 0.17, 0.20 and 0.07 μg g(-1) respectively. The procedure was applied for the analysis of a standard reference material nickel oxide (SRM 761, Nickel Oxide No.1, NBS, USA) and the values obtained are in close agreement with the certified values.

摘要

已开发出一种用于测定镍基体中痕量砷、硼、铋、镓、锗、磷、铅、锑、硒、硅和碲的方法。将样品溶解在高氯酸中(150°C),冷却时镍以结晶高氯酸镍[Ni(ClO4)2]的形式沉淀。将混合物进行超声处理,在分离出 Ni(ClO4)2 后,使用 ICP-OES 在上清液中测定感兴趣的分析物。同样,还发现,在高氯酸中溶解镍后,当溶液温度保持在100°C 时,会形成长针状的高氯酸镍晶体。将晶体从混合物中分离出来,使用 ICP-OES 测定上清液中的微量元素。在这两种方法中,基体去除率均>99%,分析物的回收率在 92-97%范围内。检测到的砷、硼、铋、镓、锗、磷、铅、锑、硒、硅和碲的检出限分别为 0.18、0.21、0.07、0.06、0.25、0.11、0.09、0.10、0.17、0.20 和 0.07μg g(-1)。该程序已应用于标准参考物质氧化镍(SRM 761,美国 NBS 的氧化镍 No.1)的分析,所得值与认证值非常吻合。

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