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逆固相基质分散净化和气质联机检测六氯苯生产厂厂区土壤的HCB残留

Determination of HCB in soil underneath the manufacture factory by dispersive solid-phase extraction and GC-MS

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【作者】 张卢军潘灿平郝向红赵玉珍马婧玮易爱华王琪

【Author】 Zhang Lujun, Pan Canping, Hao Xianghong, Zhao Yuzhen, Ma Jingwei, Yi Aihua, Wang Qi (College of sciences, China Agricultural University, Beijing 100094, China,Chinese Research Academy of Environmental Sciences. Beijing 100012, China, canpingp@cau.edu.cn)

【机构】 中国农业大学理学院中国环境科学研究院

【摘要】 本文研究了逆固相基质分散净化和气质联机法简单,快速,经济,准确的测定土壤中六氯苯(Hexachlorobenzen,简称HCB)残留量的方法。该方法用丙酮/正己烷(1:1,v/v)做萃取液,采用超声波萃取,用固相材料吸附净化,最后用GC-MS(选择离子方式)测定。用这种方法测定了某生产厂厂区地下1米至10米深的土壤样本,为进一步治理提供数据支持。结果表明,在0.05- 5 mg/kg浓度范围内呈现较好线性,相关系数R2=0.9995, 方法检出限为0.1 μg/kg,在 0.445-4.45mg/kg添加浓度下,添加回收率水平在106.6%-108.1%之间。该方法适合大批量样本快速检测土壤中六氯苯等有机氯农药的残留量,为六氯苯等持久性有机污染物的检测提供高效可靠的检测方法。用该方法测定的六氯苯的残留量在2.3 mg/kg至25912mg/kg之间,大部分样本残留量偏高,六氯苯在研究地块表现出显著的空间变异趋势。

【Abstract】 A simple, fast, and inexpensive method was improved to analyze HCB in soil with gas chromatography mass spectrometry (GC-MS). HCB in soil were extracted with acetone/hexane (1:1, v/v) using ultrasonic extraction and removed many polar matrix components using primary secondary amine (PSA) effectively for absorbing interferences. GC-MS was then used for quantitative and confirmatory analysis of HCB. Recoveries between 106.6% and 108.1% and R2>0.99 have been achieved from 0.05 mg/kg to 5 mg/kg . The limit of detection (LOD) was 0.1 μg/kg. Linear calibration curves were obtained for HCB with a concentration range of 0.05 - 5 mg/kg (R2=0.9995). Using this method we get the information of HCB quantity in the HCB factory soils. The sample sites were around and below the factory from 1 m to 10 m.. The results showed the concentration of HCB in the soils changed from 2.3mg/kg to 25912mg/kg.

【关键词】 HCBQuEChERSGC-MS逆固相基质分散净化土壤
【Key words】 HCBQuEChERSGC-MSPSAsoil
  • 【会议录名称】 持久性有机污染物论坛2006暨第一届持久性有机污染物全国学术研讨会论文集
  • 【会议名称】持久性有机污染物论坛2006暨第一届持久性有机污染物全国学术研讨会
  • 【会议时间】2006-05
  • 【会议地点】中国北京
  • 【分类号】X53
  • 【主办单位】清华大学持久性有机污染物研究中心、国家环境保护总局斯德歌尔摩公约履约办公室、中国化学会环境化学专业委员会、中国环境科学学会
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