利用国产GC建立土壤中多氯联苯快速检测方法

A Rapid Detection Method for Polychlorinated Biphenyls (PCBs) in Soil by Domestic Gas Chromatograph

[目的]寻找简便、快捷、低成本的多氯联苯检测方法,为土壤中多氯联苯含量的监控提供切实可行的手段。[方法]采用超声-振荡萃取,国产气相色谱仪检测PCB9、PCB30、PCB773种多氯联苯在土壤中的含量。[结果]在气谱条件为:进样口温度270℃;柱温220℃;检测器温度280℃;电源1nA;流速10ml/min;30.00m×0.53mm×1.00μmOV-1701毛细管柱;进样量2μl,检测得PCB9、PCB30、PCB773种多氯联苯的线性方程分别为y=2193.8x+20.617,r=0.9993;y=3682.5x-58.52,r=0.9993;y=7291.1x-64.148,r=0.9996;并在0.1～1.6μg/ml范围内线性关系良好。PCB9、PCB30、PCB773种多氯联苯的加样回收率分别为:85%～105%、87%～110%、84%～108%;RSD值分别为1.104%、3.213%、4.316%。[结论]该方法中样品前处理过程简单、回收率较高、重现性好,检测效果达到了进口气相色谱的检测水平,是一种简便、快捷、低成本的多氯联苯检测方法。

[Objective] The aim was to find a simple,fast,low cost detection method for polychlorinated biphenyls（PCBs）and provide a feasible way for monitoring PCBs content in soil.[Method] Ultrasound-oscillating technique was used to extract,and domestic gas chromatograph was adopted to detect contents of PCB9,PCB30,PCB77 in soil.[Result] The results showed that the linear equation of PCB9,PCB30,PCB77 are y=2 193.8x＋20.617,r=0.999 3;y=3 682.5x-58.52,r=0.999 3;y=7 291.1x-64.148,r=0.999 6 when conditions are：inlet temperature 270 ℃,column temperature 220 ℃,detector temperature 280 ℃,power supply 1nA,flow velocity 10 ml/min,capillary column 30.00 m×0.53 mm×1.00 μm OV-1701,sampling volume 2 μl.And showed good linear relationship in the range of 0.1-1.6 μg/ml.The recovery rate of PCB9,PCB30,PCB77 are 85%-105%,87%-110%,84%-108%,RSD value are 1.104%,3.213%,4.316% respectively.[Conclusion] The detection result reached the level of import gas chromatography,which indicated that the method is simple,fast and low cost.