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超临界CO2流体萃取——气相色谱法测定土壤中的类二癋英类多氯联苯

崔兆杰,赵士燕   

  1. 山东大学环境科学与工程学院, 山东济南250100
  • 收稿日期:2006-06-22 修回日期:1900-01-01 出版日期:2006-10-24 发布日期:2006-10-24
  • 通讯作者: 崔兆杰

Determination of dioxinlike polychlorinated biphenyls in soil by supercritical CO2 fluid extraction and gas chromatography

CUI Zhao-lin,ZHAO Shi-yan   

  1. School of Environmental Science and Engineering, Shandong Univ., Jinan 250100, Shandong, China
  • Received:2006-06-22 Revised:1900-01-01 Online:2006-10-24 Published:2006-10-24
  • Contact: CUI Zhao-lin

摘要: 利用超临界CO2流体萃取(SFECO2)及气相色谱技术,建立了土壤中12种类二癋英类多氯联苯(PCBs)的分析测定方法. 对SFECO2的萃取条件进行了优化,其最佳萃取条件为:压力25?MPa,温度100?℃,静态萃取时间20?min,动态萃取时间45?min,收集溶剂丙酮,CO2流量2.5?mL/min,改性剂10%(质量分数)二氯甲烷. 12种PCBs的加标回收率为73.0%~129.0%,相对标准偏差(RSD)为1.0%~10.5%. 测定麦田土壤样品中12种类二癋英类多氯联苯,共检出8种PCBs,质量比为77~667?pg/g,其他4种未检出.

关键词: 超临界CO2流体萃取, 气相色谱, 土壤 , 类二癋英类多氯联苯

Abstract: By using supercritical CO2 fluid extraction (SFECO2) and gas chromatography, a method was established for the determination of twelve dioxinlike polychlorinated biphenyls (PCBs) in soil. The extraction conditions were optimized. The optimized operational variables of SFECO2 are obtained as following:the pressure is 25?MPa, the temperature is 100?℃, the static extraction time is 20 min, the dynamic extraction time is 45 min, the trapping solvent is acetone, the CO2 flow rate is 2.5?mL/min and the modifier is 10% dichloromethane. The recoveries of twelve PCBs ranges from 73.0% to 129.0% and the method precision is 1.0%~10.5%. The contents are 77~667?pg/g for eight PCBs in the soil sample from cornfield. The other four PCBs are undetectable.

Key words: soil , dioxinlike polychlorinated biphenyls, gas chromatography, supercritical carbon dioxide fluid extraction

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