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Application of Headspace Solid-Phase Microextraction for Determination of Chloro-Organic Compounds in Sewage Samples

机译:顶空固相微萃取在污水样品中氯有机化合物测定中的应用

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摘要

Solid phase microextraction (SPME) has been optimized and applied to the determination of the volatile halogenated compounds (VHCs) and semi-volatile halogenated compounds (SVHCs). Three types of SPME fiber coated with different stationary phases (PDMS–100 μm, CAR/PDMS-75 μm, PDMS/DVB–65 μm) were used to examine their extraction efficiencies for the compounds tested. Experimental parameters such as the selection of SPME coatings, extraction time, and addition of salts were studied. The carboxen-polydimethylsiloxane (CAR/PDMS) fiber appears to be the most suitable for the determination of VHCs. Analytical parameters such as linearity, limit of detection, and precision were also evaluated. Application of ECD detector for the determination of VHCs and SVHCs allows their determination on the low concentration level, ranging from 0.005 to 0.8 μg/L−1. The HS-SPME-GC/ECD procedure gave good analytical precision expressed as relative standard deviation (RSD) (ranged from 5.08% to 8.07%) for a concentration level of 5 μg/L−1 and good linearity (r2 > 0.98) in a wide calibration range. The applied HS-SPME-GC/ECD method was found to be a quick and effective technique for the determination of microtrace amounts of volatile and semi-volatile halogenated compounds in samples containing high amounts of various organic compounds.
机译:固相微萃取(SPME)已得到优化,并已用于测定挥发性卤代化合物(VHC)和半挥发性卤代化合物(SVHC)。使用三种涂覆有不同固定相的SPME纤维(PDMS–100μm,CAR / PDMS-75μm,PDMS / DVB–65μm)来检查其对测试化合物的提取效率。实验参数如SPME涂层的选择,萃取时间和盐的添加进行了研究。羧基-聚二甲基硅氧烷(CAR / PDMS)纤维似乎最适合测定VHC。还评估了分析参数,例如线性,检测限和精密度。通过使用ECD检测器测定VHC和SVHC,可以在0.005至0.8μg/ L -1 的低浓度水平下进行检测。 HS-SPME-GC / ECD方法在浓度水平为5μg/ L -1 时,以相对标准偏差(RSD)(范围为5.08%至8.07%)表示,具有良好的分析精度,并且宽校正范围内的线性(r 2

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