| 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0.2 ng/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 ~0.064 ng/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) |
| DOI： |
| 分类号: |
| 基金项目: |
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| Research of the method treatment for determination of PCBs in sediment by GC |
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SONG Xi-hong,SONG Ji-de,ZHANG Xue-chao,LI Xiao-min
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| 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. |
| Key words: Sediment PCBs Microware extraction Ultrasonic extraction Soxhlet extraction Concentrated sulfuric acid cleanup Florisil column cleanup GC(ECD) |
