首页> 外文期刊>Microchemical Journal: Devoted to the Application of Microtechniques in all Branches of Science >Simultaneous square wave anodic stripping voltammetric determination of Cr, Pb, Sn, Sb, Cu, Zn in presence of reciprocal interference: application to meal matrices
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Simultaneous square wave anodic stripping voltammetric determination of Cr, Pb, Sn, Sb, Cu, Zn in presence of reciprocal interference: application to meal matrices

机译:双向干扰下方波阳极溶出伏安法同时测定Cr,Pb,Sn,Sb,Cu,Zn:在粗粉中的应用

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An analytical procedure for simultaneously determining chromium(VI), lead(II), tin(II), antimony(III), copper(II) and zinc(II) by square wave anodic stripping voltammetry (SWASV) in matrices involved in foods and food chain as wholemeal, wheat and maize meal is described.The digestion of each matrix was carried out using a concentrated HCl-HNO3-H2SO4 acidic attack mixture. Dibasic ammonium citrate buffer solution pH 6.5 was employed as the supporting electrolyte. The voltammetric measurements were carried out using, as working electrode, a stationary hanging mercury drop electrode (HMDE) and a platinum electrode and an AgAgClKClsat electrode as auxiliary and reference electrodes, respectively. The analytical procedure was verified by the analysis of the standard reference materials Wholemeal BCR-CRM 189, Wheat Flour NIST-SRM 1567a and Rice Flour NIST-SRM 1568a. For all the elements in the certified matrix, the precision as repeatability, expressed as relative standard deviation (s(r)) was of the order of 3-5%. The accuracy, expressed as relative error (e) was generally of the order of 3-6%, while the detection limits were lower than 0.123 mug/g.In the presence of reciprocal interference, the standard addition method considerably improved the resolution of the voltammetric technique.Once set up on the standard reference materials, the analytical procedure was transferred and applied to commercial meals sampled on market for sale. A critical comparison with spectroscopic measurements is also discussed. (C) 2004 Elsevier B.V. All rights reserved.
机译:通过方波阳极溶出伏安法(SWASV)同时测定食品和食品中所含基质中铬(VI),铅(II),锡(II),锑(III),铜(II)和锌(II)的分析程序描述了全麦,小麦和玉米粉等食物链。使用浓盐酸-HNO3-H2SO4酸性攻击混合物对每种基质进行消化。使用pH 6.5的柠檬酸二铵缓冲溶液作为支持电解质。伏安法的测量分别使用固定的悬挂式汞滴电极(HMDE)和铂电极和Ag AgCl KClsat电极作为辅助电极和工作电极作为工作电极。通过分析标准参考材料全麦BCR-CRM 189,小麦粉NIST-SRM 1567a和米粉NIST-SRM 1568a验证了该分析方法。对于认证矩阵中的所有元素,以相对标准偏差(s(r))表示的作为重复性的精度约为3-5%。以相对误差(e)表示的准确度通常为3-6%左右,而检出限低于0.123杯/克。在存在相互干扰的情况下,标准添加方法大大提高了分离度的分辨率。伏安法:一旦建立了标准参考物质,分析方法便被转移并应用于在市场上出售的商业样品中。还讨论了与光谱测量的关键比较。 (C)2004 Elsevier B.V.保留所有权利。

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