加速溶剂萃取-气相色谱法测定土壤中12种氯苯类化合物  

Determination of 12 chlorobenzene compounds in soil by gas chromatography with accelerated solvent extraction

作　　者：杨开放 李双双 周旭平 魏静 YANG Kaifang;LI Shuangshuang;ZHOU Xuping;WEI Jing(Zhenjiang Environmental Monitoring Center of Jiangsu Province,Zhenjiang Soil Characteristics Laboratory of Jiangsu Province Zhenjiang 212000,China)

机构地区：[1]江苏省镇江环境监测中心,江苏省镇江土壤特色实验室,江苏镇江212000

出　　处：《化学分析计量》2024年第11期40-45,共6页Chemical Analysis And Meterage

基　　金：江苏省镇江环境监测中心监测基金项目(ZJ2401)。

摘　　要：建立加速溶剂萃取-气相色谱法同时测定土壤中12种氯苯类化合物。以正己烷-丙酮为萃取溶剂,采用加速溶剂萃取处理土壤样品,萃取温度为100℃,压力为10.3 MPa,静态萃取5 min,淋洗10%萃取池体积,氮气吹扫60 s,萃取循环3次。采用弗罗里硅土柱净化,浓缩后经过DB-WAX色谱柱分离。12种氯苯类化合物在各自质量浓度范围内与色谱峰面积线性关系良好,相关系数均大于0.999,检出限为0.0001~0.1129 mg/kg,定量限为0.0004~0.4516 mg/kg。样品平均回收率为58.3%~111%,测定结果的相对标准偏差为5.0%~11.2%(n=6)。该方法准确、灵敏度高,能够实现对土壤中12种氯苯类化合物的检测。A method for simultaneous determination of 12 chlorobenzene compounds in soil by accelerated solvent extraction and gas chromatography was established.With n-hexane/acetone as extraction solvent,soil samples were treated with accelerated solvent extraction.The extraction temperature was 100℃,the pressure was 10.3 MPa,the static extraction was 5 min,the extraction pool volume was washed by 10%,the nitrogen purge was 60 s,and the extraction cycle was 3 times.Frori silica column was used for purification,concentrated and separated by DB-WAX column.The correlation coefficients were all greater than 0.999.The limits of detection were 0.0001-0.1129 mg/kg,and the limits of quantitation were 0.0004-0.4516 mg/kg.The average recoveries were 58.3%-111%,and the relative standard deviation was 5.0%-11.2%(n=6).The method is accurate and sensitive,which can realize the detection of 12 chlorobenzene compounds in soil.

关 键 词：加速溶剂萃取 气相色谱法 土壤 氯苯类化合物 

分 类 号：O657.7[理学—分析化学]