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气相色谱测定沉积物中多氯联苯的样品处理方法研究
引用本文:宋喜红,宋吉德,张学超,李晓敏.气相色谱测定沉积物中多氯联苯的样品处理方法研究[J].海洋科学,2010,34(2):40-44.
作者姓名:宋喜红  宋吉德  张学超  李晓敏
作者单位:威海市海洋环境监测中心,山东,威海,264209
摘    要:通过比较密闭微波萃取、超声波萃取、索氏提取3种方法对沉积物中多氯联苯(PCBs)提取效率,对比浓硫酸和Florisil小柱两种净化方式的净化效果,在实验基础上建立了密闭微波萃取-Florisil小柱净化-气相色谱(ECD)测定沉积物中多氯联苯的分析方法,加标质量比为0.2ng/g时,其相对标准偏差(RSD)为2.19%~8.71%,回收率为77.3%~94.6%,检出限为0.027~0.064ng/g。采用该方法对威海湾养殖区沉积物中PCBs进行了监测,结果表明本方法适用于海洋沉积物样品中PCBs的测定。

关 键 词:沉积物    多氯联苯    密闭微波萃取    超声波萃取    索氏提取    浓硫酸净化    Florisil  小柱净化    气相色谱(ECD)
收稿时间:2009/6/10 0:00:00
修稿时间:2009/12/1 0:00:00

Research of the method treatment for determination of PCBs in sediment by GC
SONG Xi-hong,SONG Ji-de,ZHANG Xue-chao and LI Xiao-min.Research of the method treatment for determination of PCBs in sediment by GC[J].Marine Sciences,2010,34(2):40-44.
Authors:SONG Xi-hong  SONG Ji-de  ZHANG Xue-chao and LI Xiao-min
Institution:Ocean Environment Monitoring Center of Weihai;Weihai 264209;China
Abstract:The sediment of ocean was extracted respectively by microware extraction, ultrasonic extraction and Soxhlet extraction, and the extracted were purified through Florisil column or concentrated sulfuric acid cleanup. The recovery and precision experiment were both conducted to compare the three extractions and the two cleanup methods. A method for the determination of PCBs in sediment of ocean has been developed, which was extracted with microwave extraction and Florisil column cleanup, and the detection could be achieved by gas chromatography with electron-capture detection(ECD). The results showed that with this method satisfactory recoveries 77.3%~94.6%, relative standard deviation(RSD)2.19%~8.71% and detection limits 0.027~0.064 ng/g could be obtained. It was confirmed that the method could be used in sediment by the determination of PCBs in Weihai Bay.
Keywords:Sediment  PCBs  Microware extraction  Ultrasonic extraction  Soxhlet extraction  Concentrated sulfuric acid cleanup  Florisil column cleanup  GC(ECD)
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