水中五氯酚的顶空固相微萃取气相色谱测定法

Determination of Pentachlorophenol in Water by Headspace Solid Phase Microextraction Gas Chromatography

目的探讨顶空固相微萃取(SPME)技术与气相色谱法联用测定水中五氯酚。方法优化水中五氯酚的SPME顶空浓缩和微萃取技术,然后使用毛细气相色谱法分离,电子捕获检测器定量测定。结果水样调pH=2,60℃搅拌平衡40min,聚丙烯酸酯萃取头(85μm)顶空吸附10min,280℃解吸3min。最低检出浓度为0.13μg/L;五氯酚线性范围0～12μg/L,r=0.999;对水加标五氯酚1、6、10μg/L回收率分别为88.9%～105.0%、88.9%～102.8%和98.0%～99.5%,相对标准偏差分别为4.9%～8.4%、3.1%～8.5%和4.0%～5.4%(n=6)。结论该方法简便、灵敏、稳定,且无溶剂污染,是测定水中五氯酚理想的方法。

Objective To study the method for determination of pentachlorophenol(PCP) in water by headspace solid phase microextraction(SPME) gas chromatography. Methods Pentachlorophenol in water samples was extracted using optimized SPME technology, separated by SE30 chromatographic column and the content of pentachlorophenol in water was determined by electron capture detector (ECD) under the conditions: adjusting water samples to pH 2.0, to maintain an agitating equilibrium concentrations at 60 ℃ for 40 min, headspace absorption for 10 min using extraction head holding polyacrylic ester-coated microfiber (0.83 μm in thickness), desorption at 280 ℃ for 3 min. Results The detection limit of the method was 0.13 μg/L. The correlation coefficient r=0.999 was noticed in range of pentachlorophenol concentrations 0-12 μg/L. When adding standard material of pentachlorophenol at concentrations of 1 μg/L, 6 μg/L, 10 μg/L, the recovery rates were 88.9%-105.0%, 88.9%-102.8% and 98.0%-99.5% respectively and the RSD were 4.9%-8.4%, 3.1%-8.5% and 4.0%-5.4%(n=6)respectively. Conclusion The method was simple, sensitive, stable and without solvent pollution, which was an ideal method for determination of pentachlorophenol in water.