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化学发光检测气相扩散流动注射法测定汞(II)

Gas-diffusion flow injection determination of Hg(II) with chemiluminescence detection.

作者信息

Amini Nazanin, Kolev Spas D

机构信息

School of Chemistry, The University of Melbourne, Victoria 3010, Australia.

出版信息

Anal Chim Acta. 2007 Jan 16;582(1):103-8. doi: 10.1016/j.aca.2006.09.002. Epub 2006 Sep 8.

Abstract

A gas-diffusion flow injection method for the chemiluminescence detection of Hg(II) based on the luminol-H(2)O(2) reaction was developed. The analytical procedure involved the injection of Hg(II) samples and standards into a 1.50 M H(2)SO(4) carrier stream, which was subsequently merged with a reagent stream of 0.60% (w/v) SnCl(2) in 1.50 M H(2)SO(4) to reduce Hg(II) to metallic Hg. The gas-diffusion cell was thermostated at 85 degrees C to enhance the vaporisation of metallic Hg. Mercury vapour, transported across the Teflon membrane of the gas-diffusion cell into the acceptor stream containing 1.00 x 10(-4) M KMnO(4) in 0.30 M H(2)SO(4), was oxidised back to Hg(II). The acceptor stream was merged with a reagent stream containing 2.50 M H(2)O(2) in deionised water and then the combined stream was merged with another reagent stream containing 7.50 x 10(-3) M luminol in 3.00 M NaOH at a confluence point opposite to the photomultiplier tube of the detection system. The chemiluminescence intensity of the luminol-H(2)O(2) reaction was enhanced by the presence of Hg(II) in the acceptor stream. The corresponding increase was related to the original concentration of Hg(II) in the samples and standards. Under optimal conditions, the chemiluminescence gas-diffusion flow injection method was characterised by a linear calibration range between 1 microg L(-1) and 100 microg L(-1), a detection limit of 0.8 microg L(-1) and a sampling rate of 12 samples per hour. It was successfully applied to the determination of mercury in seawater and river samples.

摘要

建立了一种基于鲁米诺 - H₂O₂反应的化学发光检测汞(II)的气体扩散流动注射方法。分析过程包括将汞(II)样品和标准品注入1.50 M H₂SO₄载流中,随后与含0.60%(w/v)SnCl₂的1.50 M H₂SO₄试剂流合并,将汞(II)还原为金属汞。气体扩散池在85℃恒温以促进金属汞的汽化。汞蒸气透过气体扩散池的聚四氟乙烯膜进入含有0.30 M H₂SO₄中1.00×10⁻⁴ M KMnO₄的接受流中,被氧化回汞(II)。接受流与含去离子水中2.50 M H₂O₂的试剂流合并,然后合并后的流在检测系统光电倍增管相对的汇合点与另一个含3.00 M NaOH中7.50×10⁻³ M鲁米诺的试剂流合并。接受流中汞(II)的存在增强了鲁米诺 - H₂O₂反应的化学发光强度。相应的增加与样品和标准品中汞(II)的原始浓度相关。在最佳条件下,化学发光气体扩散流动注射方法的线性校准范围为1 μg L⁻¹至100 μg L⁻¹,检测限为0.8 μg L⁻¹,采样率为每小时12个样品。该方法成功应用于海水和河水样品中汞的测定。

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