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Simultaneous analysis of 23 priority volatile compounds in water by solid-phase microextraction-gas chromatography-mass spectrometry and estimation of the method's uncertainty

机译:固相微萃取-气相色谱-质谱法同时分析水中的23种优先挥发性化合物及其不确定度的估计

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摘要

Most water contaminations with volatile organic compounds (VOCs) are traceable to leaking underground fuel reservoirs, solvent storage vessels, agricultural practices, industrial residues, and deficient wastewater treatment and disposal. In order to perform effective monitoring of such organic micropollutants in a straightforward manner, a multiresidue method for the determination of 23 VOCs (trihalomethanes (THMs), BTEX and chlorinated solvents) in water has been developed using solid-phase microextraction (SPME) and capillary gas chromatography-mass spectrometry (GC-MS). This group includes also methyl-tert-butyl ether, epichlorhydrine, and vinyl chloride which present additional analytical difficulties. Three different fibres were assayed: 7-μm polydimethylsiloxane (PDMS), 100-μm PDMS, and 75-μm Carboxen-PDMS, and the extraction conditions were optimized. The best results for the majority of the analytes and mainly for those with the lowest signals were obtained using the Carboxen-PDMS fibre after 15 min of extraction in the headspace mode at a room temperature of 20 ± 2℃. The analytical sensitivity, linearity, precision, accuracy, and uncertainties have been studied for method validation in agreement with the international standard ISO/1EC 17025:2005. The limits of detection achieved with the proposed method (0.06-0.17 μg L~(-1)) are adequate to determine the VOCs at the restrictive levels established by the European legislation. This was a decisive achievement to enable the analysis of all VOCs listed under the drinking-water directive in a single assay. The method exhibits performance capabilities suitable for routine analysis of VOCs in drinking-water by quality-control laboratories as enforced by EU Directives. The method is currently being used for this purpose, and participation in proficiency tests was assessed, with encouraging results.
机译:挥发性有机化合物(VOC)造成的大多数水污染可追溯到地下燃料库,溶剂储存容器,农业实践,工业残留物以及废水处理和处置不足的泄漏。为了以一种直接的方式对此类有机微量污染物进行有效监控,已经开发了一种使用固相微萃取(SPME)和毛细管法测定水中23种VOC(三卤甲烷(THMs),BTEX和氯化溶剂)的多残留方法。气相色谱-质谱(GC-MS)。这一组还包括甲基叔丁基醚,环氧氯丙烷和氯乙烯,它们带来了额外的分析困难。测定了三种不同的纤维:7-μm聚二甲基硅氧烷(PDMS),100-μmPDMS和75-μmCarboxen-PDMS,并优化了提取条件。使用Carboxen-PDMS纤维在20±2℃的室温顶空模式下萃取15分钟后,对于大多数分析物(主要是信号最低的那些)而言,结果最佳。已按照国际标准ISO / 1EC 17025:2005对分析灵敏度,线性,精度,准确性和不确定性进行了方法验证的研究。所提出的方法达到的检出限(0.06-0.17μgL〜(-1))足以确定欧洲法规规定的限制水平下的VOC。这是一项决定性的成就,可以在一次测定中分析饮用水指令中列出的所有VOC。该方法表现出的性能适用于欧盟指令执行的质量控制实验室对饮用水中VOC进行常规分析的功能。该方法目前正用于此目的,并评估了参加能力测试的结果,令人鼓舞。

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