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基于新试剂 4-羟基-3-(2-氧代吲哚啉-3-亚基氨基)-2-硫代-2H-1,3-噻嗪-6(3H)-酮中氰化物的亲核加成反应,双波长β校正分光光度法测定痕量氰离子。

Dual-wavelength beta-correction spectrophotometric determination of trace concentrations of cyanide ions based on the nucleophilic addition of cyanide to imine group of the new reagent 4-hydroxy-3-(2-oxoindolin-3-ylideneamino)-2-thioxo-2H-1,3-thiazin-6(3H)-one.

机构信息

Department of Chemistry, Faculty of Science, King Abdulaziz University, P.O. Box 80203, Jeddah 21589, Saudi Arabia.

出版信息

Anal Chim Acta. 2010 Jan 4;657(1):69-74. doi: 10.1016/j.aca.2009.10.025. Epub 2009 Oct 20.

Abstract

A simple, fast, low cost and sensitive direct beta-correction spectrophotometric assay of cyanide ions based on its reaction with the reagent 4-hydroxy-3-(2-oxoindolin-3-ylideneamino)-2-thioxo-2H-1,3-thiazin-6(3H)-one, abbreviated as HOTT in aqueous media of pH 7-10 is described. The electronic spectrum of the produced brown-red colored species showed well defined and sharp peak at lambda(max)=466 nm. The effective molar absorptivity for the produced cyano compound was 2.5 x 10(4) L mol(-1) cm(-1). Beer's law and Ringbom's plots were obeyed in the concentration range 0.05-2.0 and 0.30-1.5 microg mL(-1) cyanide ions, respectively. The proposed method offers 16.0 and 50.3 microg L(-1) lower limits of detection (LOD) and quantification (LOQ) of the cyanide ion, respectively. The analytical utility of the method for the analysis of cyanide ions in tap and drinking water samples was demonstrated and the results were compared successfully with the conventional cyanide ion selective electrode. The short time response and the detection by the naked eye make the method available for the detection and quantitative determination of cyanide in a variety of samples e.g. fresh and drinking water. Moreover, the structure of the produced colored species was determined with the aid of spectroscopic measurements (UV-Vis, IR, 1H and 13C NMR) and elemental analysis.

摘要

基于氰离子与试剂 4-羟基-3-(2-氧代吲哚啉-3-亚基氨基)-2-硫代-2H-1,3-噻嗪-6(3H)-酮(缩写为 HOTT)在 pH 7-10 的水介质中的反应,描述了一种简单、快速、低成本且灵敏的直接β-校正分光光度法测定氰离子。所产生的棕红色显色物质的电子光谱在 λ(max)= 466nm 处显示出清晰锐利的峰。所产生的氰基化合物的有效摩尔吸光率为 2.5 x 10(4) L mol(-1) cm(-1)。Beer 定律和 Ringbom 图在 0.05-2.0 和 0.30-1.5μg mL(-1)氰离子浓度范围内分别得到遵守。该方法对氰离子的检测限(LOD)和定量限(LOQ)分别为 16.0 和 50.3μg L(-1)。该方法用于自来水中氰离子的分析,结果与传统的氰离子选择电极法成功进行了比较。该方法具有响应时间短、肉眼检测等优点,可用于各种样品(如新鲜水和饮用水)中氰化物的检测和定量测定。此外,通过光谱测量(UV-Vis、IR、1H 和 13C NMR)和元素分析确定了所产生的有色物质的结构。

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