土壤样品中低浓度滴滴涕分析方法的前处理研究  

Establishment of Sample Pretreatment Method for the Determination of Low Levels of DDTs in Soils

作　　者：隋红[1] 吴鹏[1] 宋静[2,3] 黄玉娟[2] 李清波[4] 余海波[2] 吕明超 

机构地区：[1]天津大学化工学院,天津300072 [2]中国科学院土壤环境与污染修复重点实验室南京土壤研究所,江苏南京210008 [3]中国科学院大学,北京100049 [4]大连海事大学环境科学与工程学院,辽宁大连116026

出　　处：《分析测试学报》2013年第11期1369-1373,共5页Journal of Instrumental Analysis

基　　金：典型工业污染场地土壤修复关键技术研究与综合示范项目(2009AA061304)

摘　　要：为准确灵敏地分析土壤中低浓度滴滴涕及其衍生物(DDTs),以正己烷-丙酮(1:1,体积比)作为提取剂超声提取土壤中的DDTs,采用自主研发的四通道色谱分离仪对提取液进行分离,利用装有电子捕获检测器的气相色谱(GC/ECD)进行分析,探讨了不同层析柱填料和洗脱剂对6种DDTs目标物回收率的影响。结果表明,采用新型混合层析柱填料,以二氯甲烷-正己烷(4:1)作为洗脱剂,各目标物的超声提取回收率为83.5%~90.3%,方法的检出限为2.0~5.4 ng·g^(-1)。并对超声提取和索氏提取法的加标回收率进行了比较。A new sample purification method was developed for the determination of low levels of DDTs in soils.The tested soil was extracted with a mixture of hexane-acetone（1∶1） by ultrasonic method.The soil extracts was purified with a patented four-channel purification chromatograph before analysis by gas chromatography with electron capture detector（GC/ECD）.Effects of different column packs and elution solvents on recoveries of DDTs were investigated.The results showed that by using ultrasonic extraction,new mixed filling material for the chromatogram column and elution with dichloromethane-n-hexane（4∶1）,the recoveries of DDTs were between 83.5% and 90.3%,and the method detection limits were between 2.0 ng？g-1 and 5.4 ng？g-1,implying that the method can be used for the determination of low levels of DDTs in soils.In addition,the spiked recoveries of DDTs based on the ultrasonic extraction and Soxhlet extraction were compared under the optimal purification conditions.The results showed that the recovery of the Soxhlet extraction method is higher than that of the ultrasonic extraction method,but the the former need consume more time.

关 键 词：四通道色谱分离仪 样品前处理 土壤 DDTS 气相色谱 电子捕获检测器 

分 类 号：O657.7[理学—分析化学] S482.3[理学—化学]