Citation: DU Xiao-Di, CAI Hong-Wei, GUO Li-Ping, LEI Jia-Heng. Determination of Volatile Halogenated Hydrocarbon in Drinking Water Using Dispersive Liquid-Liquid Microextraction with Biphenyl-Biphenyl Ether Mixture as Extractants. Chinese Journal of Analytical Chemistry, 2018, 46(9): 1493-1500. doi: 10.11895/j.issn.0253-3820.181176 [复制]
Determination of Volatile Halogenated Hydrocarbon in Drinking Water Using Dispersive Liquid-Liquid Microextraction with Biphenyl-Biphenyl Ether Mixture as Extractants
以联苯-联苯醚混合物为萃取剂，建立了分散液液微萃取-气相色谱电子捕获检测器测定饮用水中7种挥发性卤代烃的方法。此萃取剂为无卤素萃取剂，密度大于水，可通过离心分离，萃取过程可在3 min内完成。对萃取剂用量、分散剂种类及用量、萃取时间、萃取温度等条件进行了优化。5.00 mL水样用200 μL萃取剂和0.30 mL分散剂（甲醇）的混合物进行萃取，室温下萃取30 s，7种挥发性卤代烃的萃取率≥90%，富集倍率为22.5~24.7。萃取液经DB-624毛细管柱分离，用电子捕获检测器定量检测，检出限为0.003~0.032 μg/L。检测三氯甲烷的线性范围为0.500~100.0 μg/L，三氯乙烯和三溴甲烷的线性范围为0.100~20.0 μg/L，四氯化碳、四氯乙烯、二氯一溴甲烷、一氯二溴甲烷的线性范围为0.050~10.0 μg/L。在上述线性范围内，工作曲线的相关系数≥0.998。方法的相对标准偏差在2.1%~7.6%之间，加标回收率在93.0%~102.9%之间。
A method for determination of seven volatile halogenated hydrocarbons in drinking water by dispersive liquid-liquid microextraction-gas chromatography with electron capture detection was developed. Biphenyl-biphenyl ether mixture, as a non-chlorinated organic solvent, was used as extractant. The extractant could be separated easily by centrifugation because of its high density, and the extraction process could be completed within 3 min. The amount of extractants, types and amount of dispersants, extraction time and extraction temperature were optimized. For the extraction of seven volatile halogenated hydrocarbons from 5.00 mL aqueous sample, 200 μL of extractant and 0.30 mL of methanol as disperser solvent were used, and the extraction equilibrium could be reached within 30 s with a high extraction recovery of over 90%. In addition, the enrichment factor reached a high value of 22.5-24.7. The sediment phase was injected and analyzed by gas chromatography with DB-624 column and detected by electron capture detector. The limit of detection of this method was 0.003-0.032 μg/L based on S/N=3. The linear range for chloroform was from 0.500 μg/L to 100.0 μg/L, for trichloroethylene and bromoform was from 0.100 μg/L to 20.0 μg/L, for perchlormethane, bromodichloromethan, dibromochloromethane and perchloroethylene was from 0.100 μg/L to 10.0 μg/L, while the correlation coefficients (R2) were no less than 0.998. The relative standard deviations of this method were 2.1%-7.6%. At different concentration levels, the relative recoveries ranged from 93.0% to 102.9%.
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