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采用顶空单滴微萃取和光纤无池微量分光光度法测定高锰酸盐氧化法中的氯离子。

Headspace single-drop microextraction and fibre optics-based cuvetteless micro-spectrophotometry for the determination of chloride involving oxidation with permanganate.

机构信息

Department of Chemistry, Rani Durgavati University, Pachpedi, Jabalpur 482001, Madhya Pradesh, India.

出版信息

Talanta. 2010 Mar 15;80(5):1816-22. doi: 10.1016/j.talanta.2009.10.027. Epub 2009 Oct 23.

DOI:10.1016/j.talanta.2009.10.027
PMID:20152416
Abstract

Headspace single-drop microextraction has been investigated for the determination of chloride in conjunction with fibre optic-based cuvetteless micro-spectrophotometry which accommodates sample volume of 1 microL placed between the two ends of optical fibres. Method has been evolved for the determination of 0.025-4 mg L(-1) of chloride involving its oxidation with permanganate in sulphuric acid medium, and reaction of chlorine with 2 microL drop of starch-iodide reagent suspended at the tip of microsyringe needle in the headspace of the reaction mixture. The limit of detection was found to be 2.8 microg L(-1) of chloride which was better than obtained by existing methods. The method was highly selective and a number of ions which interfered severely in other methods did not affect the results. The method has been used to analyze water samples, inorganic compounds and cement when the overall recovery of chloride was 94.9% with a relative standard deviation of 3.9%.

摘要

顶空单滴微萃取结合光纤无池微分光光度法已被用于测定氯,该方法可容纳 1 微升的样品体积,放置在光纤的两端之间。该方法已发展用于测定 0.025-4mg/L 的氯,涉及在硫酸介质中用高锰酸盐氧化,以及在反应混合物的顶空中,用微注射器针尖上悬挂的 2 微升淀粉-碘试剂与氯反应。检测限为 2.8μg/L 的氯,优于现有方法。该方法具有高度选择性,许多在其他方法中严重干扰的离子不会影响结果。该方法已用于分析水样、无机化合物和水泥,当氯的总回收率为 94.9%,相对标准偏差为 3.9%时。

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