首页> 外文学位 >Application of microelectrodes for the detection of metallic analytes using thin layer chromatography-square wave anodic stripping voltammetry (TLC-SWASV).
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Application of microelectrodes for the detection of metallic analytes using thin layer chromatography-square wave anodic stripping voltammetry (TLC-SWASV).

机译:微电极在使用薄层色谱-方波阳极溶出伏安法(TLC-SWASV)的金属分析物检测中的应用。

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摘要

Further studies of Thin Layer Chromatography-Square Wave Anodic Stripping Voltammetry (TLC-SWASV) for the determination of metal ions (Cd{dollar}sp{lcub}2+{rcub}{dollar}, Cu{dollar}sp{lcub}2+{rcub}{dollar}, Pb{dollar}sp{lcub}2+{rcub}){dollar} are accomplished by two modifications of the original TLC-SWASV method developed in our laboratory: (1) Implementation of a glassy carbon mercury film microelectrode (10 {dollar}mu{dollar}m diameter) to replace the original 3 mm diameter glassy carbon mercury film electrode; (2) The development of direct on-plate TLC-SWASV, which incorporates the separation and detection steps in quantitative TLC. In addition, the stability of the mercury film microelectrode is described. Its importance arises from its implementation as a TLC-SWASV detector.; Indirect on-plate TLC-SWASV. Heavy metal ion standards were separated on a carboxymethyl cellulose TLC plate. A canopy containing a thin layer of electrolyte solution was placed over the analyte spot and determined at a mercury film microelectrode using SWASV. Cadmium and lead had detection limits of 1 and 4 ng, linear calibration curves to at least 500 ng, and lead had a relative standard deviation of 22.5% (n = 4).; Off-plate SWASV determination after TLC separation. TLC was used to separate lead and cadmium from humic acid, a ubiquitous voltammetric interferent. Analyte spots were scraped from the TLC plate and quantitated using SWASV. The method sensitivity for lead and cadmium standards containing 100 ppm humic acid was statistically equivalent to standards free of humic acid. This method was also successfully applied to spiked lake water samples.; Stability of {dollar}Znsp{lcub}2+{rcub}{dollar} at a 10 {dollar}mu{dollar}m GCMFE. A spontaneous transition from a reversible to an irreversible SWASV response was noted for Zn{dollar}sp{lcub}2+{rcub}{dollar} at the 10 {dollar}mu{dollar}m GCMFE in quiescent solution. The nature of this transition is consistent with a decrease in the surface area of the mercury film and coalescence of the film into thicker mercury droplets.; Direct on-plate TLC-SWASV. Incorporation of the separation and the detection steps in TLC-SWASV was accomplished by securing a screen-printed microelectrode array to the TLC stationary phase in a homemade TLC development chamber. The analytical performance for Cd{dollar}sp{lcub}2+{rcub}{dollar}, Cu{dollar}sp{lcub}2+{rcub}{dollar}, and Pb{dollar}sp{lcub}2+{rcub}{dollar} are described. Direct on-plate TLC-SWASV was also shown to be effective for standards that contain humic acid.
机译:薄层色谱-方波阳极溶出伏安法(TLC-SWASV)用于测定金属离子(Cd {dollar} sp {lcub} 2+ {rcub} {dollar,Cu {dollar} sp {lcub} 2)的进一步研究+ {rcub} {dollar},Pb {dollar} sp {lcub} 2+ {rcub}){dollar}是通过对我们实验室开发的原始TLC-SWASV方法进行的两次修改而实现的:(1)实施玻璃碳汞膜微电极(直径10 {μm}μm)可替代原来直径3 mm的玻璃碳汞膜电极; (2)直接板载TLC-SWASV的开发,它在定量TLC中结合了分离和检测步骤。另外,描述了汞膜微电极的稳定性。它的重要性来自其作为TLC-SWASV检测器的实现。间接板载TLC-SWASV。重金属离子标准品在羧甲基纤维素TLC板上分离。将包含电解质溶液薄层的顶盖放置在分析物斑点上方,并使用SWASV在汞膜微电极处进行测定。镉和铅的检出限为1和4 ng,线性校准曲线至少为500 ng,铅的相对标准偏差为22.5%(n = 4)。 TLC分离后的板外SWASV测定。 TLC用于从腐殖酸(一种普遍存在的伏安干扰物)中分离铅和镉。从TLC板上刮下分析物斑点,并使用SWASV进行定量。对于含100 ppm腐殖酸的铅和镉标准溶液,方法灵敏度在统计学上等同于不含腐殖酸的标准溶液。该方法也成功地应用于加标的湖水样品中。 Znsp {lcub} 2+ {rcub} {dollar}在10 {μm}美元的GCMFE上的稳定性。在静态溶液中10μmGCMFE下,Zn {sp}} {lcub} 2+ {rcub} {dol}出现了自可逆的SWASV反应的自发转变。这种转变的性质与汞膜表面积的减少以及该膜聚结成较厚的汞滴相一致。直接板载TLC-SWASV。通过将丝网印刷的微电极阵列固定在自制的TLC显影室中的TLC固定相上,将分离和检测步骤结合到TLC-SWASV中。 Cd {dollar} sp {lcub} 2+ {rcub} {dollar},Cu {dollar} sp {lcub} 2+ {rcub} {dollar}和Pb {dollar} sp {lcub} 2+ {的分析性能描述了rcub} {dollar}。直接板载TLC-SWASV还被证明对含有腐殖酸的标准品有效。

著录项

  • 作者

    Petrovic, Steven Charles.;

  • 作者单位

    Ohio University.;

  • 授予单位 Ohio University.;
  • 学科 Chemistry Analytical.; Chemistry Inorganic.
  • 学位 Ph.D.
  • 年度 1998
  • 页码 147 p.
  • 总页数 147
  • 原文格式 PDF
  • 正文语种 eng
  • 中图分类 化学;无机化学;
  • 关键词

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