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Solid-Phase Extraction and LC with Fluorescence Detection for Analysis of PAHs in Rainwater

机译:固相萃取-LC-荧光检测法分析雨水中的多环芳烃

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The efficiency of extraction of polycyclic aromatic hydrocarbons (PAHs) from rainwater by solid-phase extraction (SPE) with three different types of cartridge, and analysis by high-performance liquid chromatography with fluorescence detection, are discussed in this paper. Three cartridges were investigated but only one was suitable. After equilibration in a desiccator for 65–80 h or in ambient air for 90–100 h the SPE cartridges were activated with 5 mL dichloromethane then 5 mL 2-propanol. The volume of sample passed through the cartridges was 50 mL; after loading of the sample the cartridges were dried under vacuum for approximately 20 min by application of a pressure of 15 mbar to the SPE manifold. The PAHs were eluted with 5 mL dichloromethane–hexane, 50:50 (v/v). The flow rate used for conditioning, sample loading, and elution was 2.5 mL min?1, achieved by application of a pressure of 6 mbar. For analysis of PAHs in rainwater, recovery was between 67 and 99%, the relative standard deviation varied between 2 and 5%, and the detection limits of the method were less than 16.9 ng L?1 for several PAHs. These optimum conditions were used for analysis of rainwater collected between June 2002 and May 2003 at two sites in Alsace (eastern France) and 17 PAHs were quantitatively determined. Concentrations varied between 1.6 and 968.1 ng L?1.
机译:本文讨论了使用三种不同类型的小柱通过固相萃取(SPE)从雨水中萃取多环芳烃(PAHs)的效率,以及通过高效液相色谱和荧光检测进行分析的效率。研究了三种墨盒,但只有一种适合。在干燥器中平衡65–80小时或在环境空气中平衡90–100小时后,先用5 mL二氯甲烷,再用5 mL 2-丙醇激活SPE柱。通过小柱的样品量为50 mL;加载样品后,通过在SPE歧管上施加15 mbar的压力,将小柱在真空下干燥约20分钟。 PAHs用5 mL二氯甲烷-己烷50:50(v / v)洗脱。通过施加6 mbar的压力,用于调节,上样和洗脱的流速为2.5 mL min?1 。对于雨水中的多环芳烃,回收率在67%至99%之间,相对标准偏差在2%至5%之间变化,对于几种多环芳烃,该方法的检出限小于16.9 ng L?1 。这些最佳条件用于分析2002年6月至2003年5月在阿尔萨斯(法国东部)的两个站点收集的雨水,并定量测定了17种多环芳烃。浓度范围为1.6至968.1 ng L?1

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