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首页> 外文学位 >Conductivity monitoring using an amperometric detector with a copper-based compound electrode for flow injection analysis and anion chromatography.
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Conductivity monitoring using an amperometric detector with a copper-based compound electrode for flow injection analysis and anion chromatography.

机译：使用带有铜基复合电极的安培检测器进行电导率监测，用于流动注射分析和阴离子色谱分析。

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摘要

A thin-layer type of amperometric detector is used to detect anionic species in both flow-injection and anion chromatography systems. The detector is shown to respond to anionic species on the basis of conductivity changes during the passage of sample plugs in the detector cell, no matter whether the anionic species are electrochemically-active or inactive.; The working electrode of this amperometric cell is constructed from a conducting, copper-based compound which was the insoluble fraction from the chemical polymerization of 3-methyl-2,5-dibromothiophene using copper chloride as catalyst. This material exhibits a dramatic increase in conductivity on "doping" with water, and a remarkable electrochemical stability in aqueous media. This material was previously considered as a copper-containing poly(3-methyl-thiophene). After careful characterization by elemental analysis, FT-IR, ESCA, CV and solubility tests, it is found that this material is mainly an inorganic compound containing Cu(I/II) cations and cyano- and hydroxy-groups.; This amperometric detector is used for the measurement of inorganic anions; F{dollar}sp-{dollar}, Cl{dollar}sp-{dollar}, Br{dollar}sp-{dollar}, NO{dollar}sbsp{lcub}2{rcub}{lcub}-{rcub}{dollar}, and NO{dollar}sbsp{lcub}3{rcub}{lcub}-{rcub}{dollar} in both single-column and eluant-suppressed anion chromatography. The chromatograms obtained with this detector and with a commercial conductivity detector are virtually indistinguishable under the same chromatographic conditions. The results show that the limits of detection for both detectors are comparable. The working electrode used exhibits greater stability and sensitivity than other electrode materials, such as platinum, stainless steel and cuprous cyanide, when used in the same detector units.; Although the actual mechanism of the response to anions by the copper-based compound electrode is not proved, a possible mechanism is suggested that electrode oxidation current observed occurs when a positive potential (vs. Ag/AgCl) is applied to the electrode, and the magnitude of anodic current depends on the conductivity of the analyte plug passing through the detector cell.
机译：薄层型安培检测器可用于检测流动注射和阴离子色谱系统中的阴离子物质。示出，无论阴离子物质是电化学活性的还是惰性的，在样品塞通过检测器池的过程中，检测器都会根据电导率的变化对阴离子物质做出反应。该安培电池的工作电极由导电的铜基化合物构成，该化合物是使用氯化铜作为催化剂由3-甲基-2,5-二溴噻吩进行化学聚合而得的不溶级分。该材料在用水“掺杂”时显示出显着的电导率增加，并且在水性介质中表现出显着的电化学稳定性。该材料先前被认为是含铜的聚（3-甲基-噻吩）。经元素分析，FT-IR，ESCA，CV和溶解度测试仔细表征后，发现该材料主要是含有Cu（I / II）阳离子以及氰基和羟基的无机化合物。该安培检测器用于测量无机阴离子。 F {dollar} sp- {dollar}，Cl {dollar} sp- {dollar}，Br {dollar} sp- {dollar}，NO {dollar} sbsp {lcub} 2 {rcub} {lcub}-{rcub} { Dollar}和NO {dollar} sbsp {lcub} 3 {rcub} {lcub}-{rcub} {dollar}（在单柱和洗脱液抑制的阴离子色谱中）。在相同的色谱条件下，用此检测器和商用电导率检测器获得的色谱图实际上是无法区分的。结果表明，两个探测器的探测极限是可比较的。当在同一检测器单元中使用时，所使用的工作电极比其他电极材料（例如铂，不锈钢和氰化亚铜）具有更高的稳定性和灵敏度。尽管尚未证实铜基化合物电极对阴离子的实际反应机理，但提出了一种可能的机理，即在电极上施加正电势（相对于Ag / AgCl）时会观察到电极氧化电流。阳极电流的大小取决于通过检测器池的分析物塞的电导率。

著录项

  • 作者

    Xue, Zhi-Lun.;

  • 作者单位

    University of Cincinnati.;

  • 授予单位 University of Cincinnati.;
  • 学科 Chemistry General.; Chemistry Analytical.
  • 学位 Ph.D.
  • 年度 1990
  • 页码 160 p.
  • 总页数 160
  • 原文格式 PDF
  • 正文语种 eng
  • 中图分类
  • 关键词

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