气相色谱法测定稀释沥青中19种多氯联苯

Determination of 19 types polychlorinated biphenyls in diluted bitumen by gas chromatography

进口稀释沥青可能因有其他不明油品或各种废油充当稀释剂而混有一定量的多氯联苯,有必要对稀释沥青中多氯联苯类物质进行检测。本研究利用气相色谱法建立了进口稀释沥青中19种多氯联苯类化合物的测定方法。采用自动固相萃取仪与自制的SPE柱对样品进行净化分离,通过混合溶剂洗脱,色谱柱分离,外标法定量。19种多氯联苯类物质在浓度0.5~20μg·kg^(-1)的浓度范围内与物质峰面积呈线性关系。2-氯联苯(PCB1)的检出限为1.0μg·kg^(-1),定量限为2.0μg·kg^(-1),其余多氯联苯(PCBs)的检出限均为0.5μg·kg^(-1),定量限均为1.0μg·kg^(-1)。加标回收率平均值在80.1%~116.9%,相对标准偏差(RSD)≤13.4%。结果表明本方法准确可靠,适用于进口稀释沥青中19种多氯联苯类化合物的检测分析。

Imported diluted asphalt may be mixed with a certain amount of polychlorinated biphenyls due to other unknown oil products or various waste oils acting as diluents.It is necessary to detect polychlorinated biphenyls in the diluted asphalt.This study established a method for the determination of 19 polychlorinated biphenyl compounds in imported diluted asphalt based on gas chromatography technology.The sample was purified and separated using an automatic solid-phase extraction instrument and a self-made SPE column,eluted with a mixed solvent,separated by a chromatographic column,and quantified using an external standard method.There is a linear relationship between the concentration range of 0.5~20μg·kg^(-1)and the peak area of the substance that 19types of polychlorinated biphenyls.The detection limit of 2-Chlorobiphenyl(PCB1)is 1.0μg·kg^(-1),with a quantification limit of2.0μg·kg^(-1),the detection limit for other Polychlorinated Biphenyls(PCBs)is 0.5μg·kg^(-1),with a quantification limit of 1.0μg·kg^(-1).The average recovery rate of spiking is 80.1%~116.9%,with a relative standard deviation(RSD)of≤13.4%.The results indicate that this method is accurate and reliable,and is suitable for the analysis and detection of 19 polychlorinated biphenyl compounds in imported diluted asphalt.