气相色谱-质谱法测定沉积物中3,3-二氯联苯胺

Determination of 3,3-dichlorobenzidine in Sediment by Gas Chromatography Mass Spectrometry

3,3-二氯联苯胺是一种重要的颜料中间体,在颜料生产行业中难以被取代,其常常通过工业废水的排放迁移到沉积物中对环境造成污染。本文建立了气相色谱-质谱法测定沉积物中3,3-二氯联苯胺的分析方法。使用冷冻干燥法干燥样品后,经加压流体萃取、平行浓缩,再用硅酸镁小柱净化,最后用气相色谱-质谱联用仪进行分析测试。3,3-二氯联苯胺的检出限为0.003 mg/kg,相对标准偏差为3.3%~7.7%,加标回收率为57.0%~70.8%。该方法的检出限低、精密度良好、正确度高,适合沉积物中3,3-二氯联苯胺的测定。

3,3-dichlorobenzidine is an important pigment intermediate,which is difficult to replace in the pigment production industry.It ofen migrates into the sediment through the discharge of industrial wastewater,causing environmental pollution.A gas chromatography mass spectrometry analysis method was developed for the determination of 3,3-dichlorobenzidine in sediment.Afer the samples were dried by freeze-drying method,they were extracted by pressurized fluid extraction and concentrated by parallel evaporation instruments,then the samples were purified with Florisil column.The concentration of 3,3-dichlorobenzidine in sediment were determined by gas chromatography mass spectrometer in the end.The detection limits of 3,3-dichlorobenzidine was 0.003 mg/kg.The relative standard deviation was 3.3%~7.7%,and the recovery rate was 57.0%~70.8%.The method has low detection limit,high precision and trueness,which is suitable for the determination of 3,3-dichlorobenzidine in sediment.