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Speciation of mercury in water and freshwater fish samples by a two-step solidified floating organic drop microextraction with electrothermal atomic absorption spectrometry

机译:两步凝固的漂浮有机液滴微萃取-电热原子吸收光谱法测定水和淡水鱼样品中的汞形态

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A new and simple two-step SFODME using 4-nitro-o-phenylenediamine (4-NOPD) as a chelating agent was developed for mercury speciation in water and fish samples by ETAAS. For the first step, methylmercury was extracted into 1-undecanol and for the second step, the Hg(II) remaining in the sample solution was complexed with 4-NOPD and then extracted into 1-undecanol. Under the optimized conditions, the calibration graphs of Hg (II) and methylmercury were linear in the range of 0.83-8.0 mu g L-1 and 0.78-8.0 mu g L-1, with the LOD of 0.25 mu g L-1 and 0.24 mu g L-1 and the enrichment factor were 25.7 and 32.2, respectively. The % RSDs was in the range of 2.0-4.4% at concentrations of 0.5 and 4.0 mu g L-1 (n = 5). The proposed method was successfully applied to mercury speciation in water and fish samples. The accuracy of method, tested by the analysis of SRM 1566b and DORM-4 was in good agreement with the certified values.
机译:开发了一种新的简单的两步SFODME,使用4-硝基-邻苯二胺(4-NOPD)作为螯合剂,用于通过ETAAS对水和鱼样品中的汞进行形态分析。第一步,将甲基汞萃取到1-十一烷醇中;第二步,将样品溶液中残留的Hg(II)与4-NOPD络合,然后萃取到1-十一烷醇中。在最佳条件下,汞(II)和甲基汞的校准曲线在0.83-8.0μg L-1和0.78-8.0μgL-1范围内呈线性关系,LOD为0.25μg L-1和0.24μgL-1和富集因子分别为25.7和32.2。在0.5和4.0μgL-1(n = 5)的浓度下,%RSD在2.0-4.4%的范围内。所提出的方法已成功地应用于水和鱼样品中的汞形态分析。通过对SRM 1566b和DORM-4的分析测试,方法的准确性与认证值非常吻合。

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