Department of Chemistry, Biochemistry and Environmental Protection, Faculty of Sciences, Trg D. Obradovića 3, 21000 Novi Sad, Serbia.
Anal Chim Acta. 2010 Jan 18;658(1):12-7. doi: 10.1016/j.aca.2009.10.049. Epub 2009 Oct 31.
The possibility of applying antimony-film modified glassy carbon electrode in sequential-injection analysis (SIA) was investigated with the objective of determining Pb(II) and Cd(II) by anodic stripping voltammetry (ASV). The conditions of antimony-film deposition concerning composition of the plating/carrier solutions, concentrations of Sb(III) and hydrochloric acid, effects of different supporting electrolyte salts, and plating potential were optimized. It was found that the antimony-film deposition on glassy carbon substrate in a sample solution consisting of 750 microg L(-1) Sb(III), 0.5 mol L(-1) HCl at -1.5 V (vs. Ag/AgCl/3 mol L(-1) KCl) yielded a modified electrode suitable for the determination of Pb(II) and Cd(II) at the microg L(-1) level. The reproducibility of the analytical signals was characterized by a relative standard deviation lower than 2.8%, and the calculated values of detection limits were 1.2 microg L(-1) for Pb(II) and 1.4 microg L(-1) for Cd(II). The presence of KSCN in the sample solution offers the possibility of detecting ions with more negative oxidation potentials like Zn(II), Mn(II) or Cr(III). The developed SIA-ASV procedure was compared with the commonly used batch method, and its applicability was tested on a spiked tap water sample.
研究了载 Sb 膜修饰玻碳电极在顺序注射分析（SIA）中的应用，目的是通过阳极溶出伏安法（ASV）测定 Pb(II)和 Cd(II)。优化了载 Sb 液组成、Sb(III)和盐酸浓度、不同支持电解质盐和电镀电位等 Sb 膜沉积条件。结果表明，在由 750μg L(-1) Sb(III)、0.5 mol L(-1) HCl 和-1.5 V（相对于 Ag/AgCl/3 mol L(-1) KCl）组成的样品溶液中，在玻碳基体上沉积 Sb 膜可得到适用于测定 Pb(II)和 Cd(II)的修饰电极，其浓度低至μg L(-1)。分析信号的重现性以低于 2.8%的相对标准偏差为特征，计算得到的检测限分别为 1.2μg L(-1)的 Pb(II)和 1.4μg L(-1)的 Cd(II)。样品溶液中 KSCN 的存在为检测具有更负氧化电位的离子（如 Zn(II)、Mn(II)或 Cr(III)）提供了可能。所建立的 SIA-ASV 程序与常用的批量法进行了比较，并对加标自来水样品进行了适用性测试。
