• 中文核心期刊
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土壤和沉积物中22种有机氯农药和8种多氯联苯的气相色谱分析

Method for the Analysis of 22 Organochlorine Pesticides and 8 Polychlorinated Biphenyls in Soils and Sediments Using Gas Chromatography

  • 摘要: 近年来地下水、土壤和沉积物等介质中有机氯农药和多氯联苯分析方法的改善主要集中在样品前处理和分析测试条件等方面,而探讨布点、采样等方面的整套方法较少。本文建立了一套适用性较广的气相色谱法同时测定土壤和沉积物中22种有机氯农药和8种多氯联苯,方法检出限为0.09~0.48 ng/g,平均空白回收率为58.7%~133.7%。针对布点、采样、运输、保存、提取、净化、浓缩、仪器测试、数据处理和提交报告整个过程阐述了方法的有效性和实用性;并对提取、净化、测试等多个环节提供了两种或更多的选择,使方法具有更大的灵活性。本文提出,布点前应根据踏勘样品和前人资料考虑采集不同深度的样品;样品的布点、采集和制备均需选择样品,它们共同决定了样品的代表性;分析方法要灵活运用,对于很少检出的目标化合物可采用允许共峰但分析快速的方法,如果有检出再采用针对性的方法分别测定;样品的测定序列不应为了节约分析成本而过于简单。

     

    Abstract: In recent years, the main focus for improving detection methods for organochlorine pesticides (OCPs) and polychlorinated biphenyls (PCBs) in groundwater, soils and sediments has focused mainly on pretreatment and analysis conditions. Comprehensive methods including sampling point design and sample collection were seldom studied. A new method was has been developed for the simultaneous determination of 22 OCPs and 8 PCBs in soils and sediments by Gas Chromatography coupled with electron capture detection. Method detection limits range from 0.09 ng/g to 0.48 ng/g, and the average recoveries are 58.7%-133.7%. This developed method seems to be a relatively integrated and widely applicable method, including sampling point design, sample collection, transportation, preservation, extraction, clean-up, concentration, determination, data analysis and reporting. Alternative technologies were recommended for extraction, clean-up and Gas Chromatographic condition, etc, which improves the flexibility of the method. The results show that the sampling point design for the samples collected from different depths should be considered on the basis of scouting samples and pre-existing data since the representativeness of samples comprehensively depends on selecting procedure, sampling point design, sample collection and preparation. A flexible Gas Chromatographic condition can be used for those samples with rare target compounds, and a corresponding Gas Chromatographic condition can be used further if special target compounds need to be separated. Sequence of the samples should not be oversimplified in order to save cost.

     

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