气相色谱法测定土壤中有机氯农药的分析

Determination of Organochlorine Pesticides in Soil by Gas Chromatography

为提高测定土壤中有机氯农药准确度,建立加压流体萃取-气相色谱联用技术对土壤中的六六六、滴滴涕进行测定,并探讨了实验条件对分析准确度的影响。实验中探究了土壤类型、样品装填、净化措施和程序升温等条件对萃取效率和分析准确性的影响,摸索出适合实际样品的分析条件。实验结果表明,在最佳分析条件下,8种有机氯农药方法线性范围0.01~1.00mg/L,相关系数r大于0.9990,样品加标回收率为70%~91%,相对标准偏差为4.21%~6.88%(n=6),对有证标准样品的测定均在有效值范围。该方法具有较高的准确度和良好的精密度,用于标准土壤的分析结果令人满意,可用于环境监测中对土壤中多种有机氯农药的准确测定。

In order to improve the analytical accuracy in the determination of organochlorine pesticides(OCPs)in soil,a combined technique of pressurized fluid extraction-gas chromatography was established to determine BHC and DDT in soil,and the influence of experimental conditions on the accuracy was discussed.The effects of soil types,sample loading,purification measures and temperature-programmed conditions on extraction efficiency and analysis accuracy were investigated,and the suitable analysis conditions for actual samples were found.Results showed that under the optimal analysis conditions,the linear range of 8 OCPs were in the range of 0.01~1.00 mg/L,the correlation coefficient r was greater than 0.9990.The recoveries of standard addition for 8 OCPs were ranging from 70% to 91%,and the relative standard deviations(RSD)were 4.21%~6.88%(n=6).The determination of certified standard sample were all in the range of effective values.The proposed method has high accuracy and good precision,and the analysis results of standard soil are satisfactory,which can be used for the accurate determination of Ocps in soil in environmental monitoring.