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Online anion exchange column preconcentration and high performance liquid chromatographic separation with inductively coupled plasma mass spectrometry detection for mercury speciation analysis

机译:在线阴离子交换柱预浓缩和高效液相色谱分离-电感耦合等离子体质谱检测法用于汞形态分析

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A hyphenated method for mercury speciation analysis by the coupling of high performance liquid chromatography and inductively coupled plasma mass spectrometry with the online strong anion exchange column (SAX) preconcentration was developed. The Hg analytes (Hg~+, MeHg, EtHg and Hg~(2+)) were absorbed on the SAX column preconditioned with sodium 3-mercapto-l-propanesuIfonate, and then rapidly eluted (less than 16 s) by 5 μL 3% (v/v) 2-mercaptoethanol. The enrichment factors of 1025 for Hg~+, 1084 for MeHg, 1108 for EtHg and 1046 for Hg~(2+) were obtained using 6 mL sample in a 1.5-min enrichment procedure. Rapid separation of the four mercurial compounds was achieved within 5 min on a 50-mm C_(18) column using 0.5% (v/v) 2-mercaptoethanol as the mobile phase. The detection limits for Hg~+, MeHg, EtHg and Hg~(2+) were 0.015, 0.010, 0.009 and 0.016 ng L~(-1), each, and the relative standard deviations of peak height and peak area (5 ng L~(-1) for each Hg species) were all below 5%. Mercury speciation in three freshwater, two drinking water and two seawater samples were then analyzed by the proposed method. MeHg and Hg~(2+) concentrations down to 0.14 and 0.56 ng L~(-1) were detected in the drinking waters.
机译:开发了一种通过高效液相色谱和电感耦合等离子体质谱联用在线强阴离子交换柱(SAX)预浓缩进行汞形态分析的联用方法。 Hg分析物(Hg〜+,MeHg,EtHg和Hg〜(2+))在用3-巯基-1-丙磺酸钠预处理的SAX柱上吸收,然后用5μL3迅速洗脱(少于16 s) %(v / v)2-巯基乙醇。使用6 mL样品在1.5分钟的富集程序中获得Hg〜+的富集因子1025,MeHg的1084,EtHg的1108和Hg〜(2+)的1046。在50 mm C_(18)色谱柱上,使用0.5%(v / v)2-巯基乙醇作为流动相,可以在5分钟内快速分离出四种汞化合物。 Hg〜+,MeHg,EtHg和Hg〜(2+)的检出限分别为0.015、0.010、0.009和0.016 ng L〜(-1),以及峰高和峰面积的相对标准偏差(5 ng每个Hg种类的L〜(-1)都低于5%。然后通过提出的方法分析了三种淡水,两种饮用水和两种海水样品中的汞形态。在饮用水中检测到的MeHg和Hg〜(2+)浓度低至0.14和0.56 ng L〜(-1)。

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