引用本文:姚远,宋维涛,张洋,王清.顶空固相微萃取-气相色谱法测定水中氯酚类化合物[J].环境监控与预警,2015,7(6):25-29
YAO Yuan, SONG Wei tao, ZHANG Yang, WANG Qing.Determination of Chlorophenols in Water Samples Using Headspace Solid Phase Microextraction Coupled with Gas Chromatography[J].Environmental Monitoring and Forewarning,2015,7(6):25-29
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顶空固相微萃取-气相色谱法测定水中氯酚类化合物
姚远,宋维涛,张洋,王清
连云港市环境监测中心站,江苏 连云港 222001
摘要:
建立了水中2,4-二氯酚、2,4,6-三氯酚和五氯酚的顶空固相微萃取-气相色谱分析方法。研究确定以聚丙烯酸酯(PA,85 μm)为萃取头,加入0.3 mL质量浓度为0.1 mol/L 的H2SO4溶液和1.5 g 的Na2SO4调节待测液的pH值和离子强度,萃取温度为80℃,萃取时间为50min,搅拌速率为250 r/min时萃取效果最好;最佳解吸时间为5 min。在该优化条件下,3种物质在0.1~10 000 μg/L范围内线性良好,相关系数R2均>0.999,检出限为0.023~0.13 μg/L,实际样品的加标回收率为82.5%~101.7%。该方法萃取过程不需有机溶剂,绿色、简便,且具有较高的灵敏度,适用于地表水、地下水等环境水样中氯酚类化合物的痕量检测与批量分析。
关键词:  顶空固相微萃取  气相色谱法    氯酚类化合物
DOI:
分类号:O657.7+1; X832
基金项目:
Determination of Chlorophenols in Water Samples Using Headspace Solid Phase Microextraction Coupled with Gas Chromatography
YAO Yuan, SONG Wei tao, ZHANG Yang, WANG Qing
(Lianyungang Environmental Monitoring Center Station, Lianyungang, Jiangsu 222001, China
Abstract:
This study established a method for the determination of 2,4 dichlorophenol, 2,4,6 trichlorophenol and pentachlorophenol by headspace solid phase microextraction coupled with gas chromatography. The results showed that the best extraction efficiency was obtained when using polyacrylate (PA,85 μm) as the extraction fiber, and the test solution stirred at 250r/min for 50 min at 80 ℃ with the addition of 0.3 mL of 0.1 mol/L H2SO4and 1.5 g Na2SO4 for adjusting the pH and ionic strength of the test solution, respectively. The optimal desorption time was 5 min. Under the optimum conditions, the three compounds showed good linearity in the range of 0.1~10 000 μg/L and the correlation coefficients(R2) were all over 0.999. The detection limits were in the range of 0.023-0.11 g/L. The recoveries of spiked samples were between 82.5% and 101.7%.The extraction process in this method is free of organic reagents, and is green, simple and highly sensitive, which is applicable for trace and batch determination of chlorophenol compounds in surface water, groundwater and other environmental water samples.
Key words:  Headspace solid phase microextraction  Gas chromatography  Water  Chlorophenols