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Speciation and preconcentration of inorganic antimony in waters by Duolite GT-73 microcolumn and determination by segmented flow injection-hydride generation atomic absorption spectrometry (SFI-HGAAS)

机译:Duolite GT-73微柱对水中的锑进行形态分析和预富集,并通过分段流动注射氢化物发生原子吸收光谱法(SFI-HGAAS)测定

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摘要

A selective matrix removal/separation/enrichment method, utilizing a microcolumn of a chelating resin with SH functional groups (Duolite GT-73), was proposed for the determination of Sb(III) in waters by segmented flow injection-hydride generation atomic absorption spectrometry (SFI-HGAAS). The resin was selective to Sb(III) at almost all pH and acidity values employed, whereas Sb(V) was not retained at all and could be determined after a pre-reduction step with l-cysteine. Spike recoveries were tested at various concentration levels in different water types and were found to vary between 85 and 118%. Accuracy of the proposed methodology was checked by analyzing a standard reference material and a good correlation was found between the determined (13.3 ± 1.1 μg l-1) and the certified value (13.79 ± 0.42 μg l-1). The method was applied to several bottled drinking water samples for antimony determination with and without preconcentration and none of the samples were found to contain antimony above the permissible level (5 μg l-1). The characteristic concentration (the concentration of the analyte corresponding to an absorbance of 0.0044) was 0.55 μg l-1 and the 3 s limit of detection (LOD) based on five times preconcentration was 0.06 μg l-1. The applicability of the microcolumn separation/preconcentration/matrix removal method for flow injection systems was also demonstrated.
机译:提出了一种使用带SH官能团的螯合树脂(Duolite GT-73)的微柱选择性基质去除/分离/富集方法,通过分段流动注射氢化物发生原子吸收光谱法测定水中的Sb(III) (SFI-HGAAS)。在几乎所有使用的pH和酸度值下,该树脂对Sb(III)都具有选择性,而Sb(V)根本没有保留,可以在用l-半胱氨酸进行预还原步骤后确定。在不同的水类型下,以不同的浓度水平测试穗的回收率,发现其变化范围为85%至118%。通过分析标准参考物质来检验所提出方法的准确性,并且在测定的标准物质(13.3±1.1μgl-1)与认证值(13.79±0.42μgl-1)之间发现良好的相关性。该方法适用于几种瓶装饮用水样品中的锑(含或不含预浓缩),没有一个样品的锑含量超过允许水平(5μgl-1)。特征浓度(对应于0.0044的吸光度的分析物浓度)为0.55μgl-1,基于五倍预浓缩的3 s检测限(LOD)为0.06μgl-1。还展示了微柱分离/预浓缩/基质去除方法在流动注射系统中的适用性。

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