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The surface morphology of mercury plated glassy-carbon electrodes and stripping voltammetry of heavy metals

机译:镀汞玻碳电极的表面形态和重金属的溶出伏安法

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This article deals with the investigation into the correlation between the surface morphology of the glassy carbon electrodes modified with mercury and the characteristics of voltammograms of copper, lead, cadmium and mercury. The methods of voltammetry and in situ microscopy were used. It is shown that nucleation is the slow step of the mercury evolution on glassy carbon electrode. Overvoltage of the process is reduced after nuclei form. The factors, which determine the distribution of mercury on the electrode surface, are the degree of polishing of glassy carbon and exposure of the electrode to the air. Two types of insoluble compounds are formed on the electrode in solutions containing chloride-ions. One type of the compounds, a calomel, forms a reversible redox pair and is reduced to metallic mercury during cathodic polarization of the electrode. Well-defined voltammograms of the metals are observed in this case. The other type of the compounds appears during anodic polarization of the mercury-coated electrode in solutions containing chloride-ions when the mole ratio HCl/Hg2+ of the solution is less than 10(4). The formation of these compounds, which possess anomalous properties, is followed by appearance of a cathodic peak in the anodic voltammogram ('reverse' peak). A special electrochemical 'conditioning' of the electrode is needed to remove the precipitate of insoluble compounds. Otherwise, unusual 'reverse' peaks complicate the voltammograms of the elements to be determined. [References: 40]
机译:本文研究了汞修饰的玻璃碳电极的表面形态与铜,铅,镉和汞的伏安图特征之间的相关性。使用伏安法和原位显微镜法。结果表明,成核作用是玻璃碳电极上汞释放的缓慢步骤。核形成后,该过程的过电压降低。决定汞在电极表面上分布的因素是玻璃碳的抛光程度和电极暴露于空气中的程度。两种不溶性化合物在含有氯离子的溶液中形成在电极上。一类化合物,甘汞,形成可逆的氧化还原对,并在电极的阴极极化过程中还原为金属汞。在这种情况下,观察到金属的明确的伏安图。当溶液的HCl / Hg2 +摩尔比小于10(4)时,另一种类型的化合物会出现在含氯离子溶液中的带汞电极的阳极极化过程中。这些化合物具有异常性质,随后在阳极伏安图中出现一个阴极峰(“反向”峰)。需要对电极进行特殊的电化学“调节”以去除不溶性化合物的沉淀物。否则,异常的“反向”峰会使要确定的元素的伏安图复杂化。 [参考:40]

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