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On-line redox speciation analysis of antimony using L-proline immobilized on controlled pore glass and hydride generation inductively coupled plasma optical emission spectrometry for detection

机译:使用固定在受控孔玻璃上的L-脯氨酸和氢化物发生电感耦合等离子体发射光谱法在线检测锑的氧化还原形态

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摘要

L-proline was immobilized on controlled pore glass to study the ability of this material for the separation and preconcentration of Sb(III) and Sb(V). The substrate was packed in a minicolumn and incorporated in a flow injection system. The effluents of the on-line solid phase extraction (before and after elution) were directly coupled to the hydride generation inductively coupled plasma optical emission spectrometry system. The effect of pH, sample (and eluent) volume, flow rates of sample loading and elution on separation of Sb(III) e Sb(V) were evaluated. Our experiments demonstrated that Sb(V) was not retained and it was selectively determined during the loading step, while retained Sb(III) was determined after elution. The proposed system was also used for the selective preconcentration of Sb(III). In this case, a preconcentration factor of 11 and a limit of detection of 90 ng L~(-1) for Sb(III) were achieved when 8 mL of sample were loaded into the column. The speciation analysis of inorganic Sb in river water and effluent samples was performed using the proposed method. The values obtained for total Sb (obtained by sum of Sb(III) and Sb(V)) were in good agreement with expected values. Recoveries of Sb(III) and Sb(V) in the river water Standard Reference Material 1640 (from National Institute of Standard and Technology) and spiked river waters were between 83 and 111%.
机译:将L-脯氨酸固定在可控孔玻璃上,以研究该物质分离和预富集Sb(III)和Sb(V)的能力。将基材包装在小柱中,并加入流动注射系统中。在线固相萃取(洗脱前后)的流出物直接与氢化物发生电感耦合等离子体发射光谱系统耦合。评估了pH,样品(和洗脱液)的体积,样品加载和洗脱的流速对分离Sb(III)和Sb(V)的影响。我们的实验表明,未保留Sb(V),在上样步骤中对其进行了选择性测定,而洗脱后确定了Sb(III)。拟议的系统还用于Sb(III)的选择性预浓缩。在这种情况下,当将8 mL样品上样时,Sb(III)的预富集因子为11,检出限为90 ng L〜(-1)。利用所提出的方法对河流水和污水样品中的无机锑进行了形态分析。获得的总Sb值(由Sb(III)和Sb(V)的总和获得)与预期值非常吻合。河流水标准参考材料1640(来自美国国家标准与技术研究院)和加标河水中的Sb(III)和Sb(V)回收率在83%至111%之间。

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