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Aqueous two-phase extraction of nickel dimethylglyoximato complex and its application to spectrophotometric determination of nickel in stainless steel

机译:二甲基乙二酰肟基镍络合物的水两相萃取法及其在光度法测定不锈钢中的应用

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摘要

A polyethylene glycol (PEG)-based aqueous two-phase system has been established for the extraction of Ni-dimethylglyoximato complex. Appropriate amounts of PEG solution and solid (NH4)(2)SO4 were added to the Ni-dimethylglyoximato complex which had been formed in the presence of sodium tartrate and K2S2O8 at pH 12 in a separatory funnel and shaken vigorously for about 1 min. The mixture was allowed to stand for 10 min and then the absorbance of the extracted complex in the upper PEG-rich phase was measured at 470 nm. Beer's law was obeyed over the range of 0.26-2.1 ppm Ni. The proposed extraction method has been applied to the determination of Ni in steel. A steel sample was decomposed with an appropriate acid mixture. An aliquot of the sample solution was taken, treated with H3PO4 and most of the iron and copper were removed by hydroxide precipitation using solid BaCO3 to control the pH of the sample solution in advance of the extraction of Ni. The analytical results obtained for Ni in steel certified reference material JSS 650-10 (The Japan Iron and Steel Federation), BCS 323 (Bureau of Analysed Samples Ltd.) and NIST SRM 361 and 362 (National Institute of Standards and Technology) were in good agreement with certified values. (c) 2004 Elsevier B.V. All rights reserved.
机译:已经建立了基于聚乙二醇(PEG)的含水两相系统,用于提取Ni-二甲基乙二酰肟酸酯络合物。将适量的PEG溶液和固体(NH4)(2)SO4添加到在分液漏斗中在酒石酸钠和K2S2O8的存在下于分液漏斗中形成的Ni-二甲基乙二肟复合物中,并剧烈振摇约1分钟。将混合物静置10分钟,然后在470nm处测量提取的复合物在上层富含PEG的相中的吸光度。在0.26-2.1 ppm Ni的范围内遵守比尔定律。所提出的萃取方法已应用于钢中镍的测定。用适当的酸混合物将钢样品分解。取试样溶液的等分试样,用H 3 PO 4处理,并使用固体BaCO 3通过氢氧化物沉淀除去大部分铁和铜,以在萃取镍之前控制试样溶液的pH。在钢认证参考材料JSS 650-10(日本钢铁联合会),BCS 323(分析样品局)和NIST SRM 361和362(美国国家标准技术研究所)中对Ni的分析结果在与认证值的良好协议。 (c)2004 Elsevier B.V.保留所有权利。

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