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首页> 外文期刊>Talanta: The International Journal of Pure and Applied Analytical Chemistry >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)
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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)

机译:电感耦合等离子体发射光谱法(ICP-OES)测定高纯镍中的痕量As,B,Bi,Ga,Ge,P,Pb,Sb,Se,Si和Te

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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 (similar to 150 degrees 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 mu g 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. (C) 2014 Elsevier B.V. All rights reserved.
机译:开发了一种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HClO4(类似于150摄氏度)中,冷却后将镍沉淀为结晶高氯酸镍[Ni(ClO4)(2)]。将混合物超声处理,分离Ni(ClO4)(2)后,使用ICP-OES测定上清液中的目标分析物。类似地,还发现,在将镍溶解在高氯酸中之后,当溶液温度保持在100℃时,形成了长针状的高氯酸镍晶体。从混合物中分离出晶体,并使用ICP-OES测定上清液中的痕量元素。在这两种方法中,基质去除率均> 99%,分析物的回收率在92%至97%之间。发现As,B,Bi,Ga,Ge,P,Pb,Sb,Se,Si和Te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和分别为0.07μgg(-1)。该程序用于分析标准参考物质氧化镍(SRM 761,1号氧化镍,NBS,美国),并且所获得的值与认证值非常一致。 (C)2014 Elsevier B.V.保留所有权利。

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