Mercury speciation by high-performance liquid chromatography atomic fluorescence spectrometry using an integrated microwave/UV interface. Optimization of a single step procedure for the simultaneous photo-oxidation of mercury species and photo-generation of Hg 0 ☆
Mercury speciation by high-performance liquid chromatography atomic fluorescence spectrometry using an integrated microwave/UV interface. Optimization of a single step procedure for the simultaneous photo-oxidation of mercury species and photo-generation of Hg 0 ☆
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DOI：
10.1016/j.sab.2014.09.019
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发表时间：
2014-11
期刊：
影响因子：
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通讯作者：
Daiane P. C. de Quadros;B. Campanella;M. Onor;E. Bramanti;Daniel L. G. Borges;A. D’Ulivo
中科院分区：
文献类型：
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作者：
Daiane P. C. de Quadros;B. Campanella;M. Onor;E. Bramanti;Daniel L. G. Borges;A. D’Ulivo
我们描述了光诱导化学气相发生与高效液相色谱-原子荧光光谱法（HPLC-AFS）联用定量无机汞，甲基汞（MeHg）和乙基汞（EtHg）。在所开发的程序中，甲酸在移动的相用于光解有机汞化合物和还原Hg 2+汞蒸气在微波/紫外（MW/UV）照射。考察了有机酸的种类、浓度、微波功率、高效液相色谱移动的相组成以及纳米TiO 2的催化作用等因素对该方法的影响。在优化条件下，无机汞、甲基汞和乙基汞的检出限分别为0.15、0.15和0.35 μg L− 1。所开发的方法进行了验证，通过确定的主要分析品质因数，并适用于三个认证的参考物质的分析。液相色谱-光化学-蒸气发生-原子荧光法在线联用测定汞是一种简单、环境友好的方法，是传统四氢硼酸盐（THB）系统的一种有吸引力的替代方法。
We described the hyphenation of photo-induced chemical vapor generation with high performance liquid chromatography–atomic fluorescence spectrometry (HPLC–AFS) for the quantification of inorganic mercury, methylmercury (MeHg) and ethylmercury (EtHg). In the developed procedure, formic acid in mobile phase was used for the photodecomposition of organomercury compounds and reduction of Hg2 +to mercury vapor under microwave/ultraviolet (MW/UV) irradiation. We optimized the proposed method studying the influence of several operating parameters, including the type of organic acid and its concentration, MW power, composition of HPLC mobile phase and catalytic action of TiO2nanoparticles. Under the optimized conditions, the limits of detection were 0.15, 0.15 and 0.35 μg L− 1for inorganic mercury, MeHg and EtHg, respectively. The developed method was validated by determination of the main analytical figures of merit and applied to the analysis of three certified reference materials. The online interfacing of liquid chromatography with photochemical-vapor generation–atomic fluorescence for mercury determination is simple, environmentally friendly, and represents an attractive alternative to the conventional tetrahydroborate (THB) system.