气相色谱-质谱法测定电子电气产品中多溴二苯醚及多溴联苯

建立了利用气相色谱-质谱测定电子、电气产品中多溴二苯醚及多溴苯的方法。对样品的粉碎、提取方法、色谱柱的选择、测定条件进行研究,并自建标准质谱图库;采用保留时间、Br同位素规则、质谱特征离子、谱库检索等4种方式相结合进行定性,避免了假阳性及漏检的情况,结果更加准确可靠。本法检出限为5mg/kg,PBDEs的回收率为91.3%,PBBs的回收率为92.5%,相对标准偏差(RSD)为4.3%。与现有方法相比,本法分离时间最短(6min),具有简便快速、实用性强、灵敏度高、准确可靠等特点,适用于电子电气产品、塑料、橡胶、汽车内饰材料等的溴系阻燃剂分析,满足欧盟RoHS指令检测的要求。

Determination of Polybromodiphenyl Ethers and Polybromobiphenyls in Electrical and Electronic Equipments by Gas Chromatography-Mass Spectrometry

A method for the detection of polybromobiphenyls (PBBs) and polybromodiphenyl ethers (PBDEs) in electrical and electronic equipments by gas chromatography-mass spectrometry (GC-MS) has been developed. The pretreatment procedures, such as solvent selection, extraction method and column type, were discussed, and standard mass spectral library of PBBs and PBDEs was established. Four qualitative methods of retention time, isotopic rule of bromine, characteristic ion and standard library searching were used. The detection limit was 5 mg/kg, and the recovery rate of PBBs and PBDEs was 92.5% and 91.3%, respectively. The relative standard deviation was 4.3%. The separation time was 6 minutes, results meeting the directions of RoHS were obtained. This method can be used to analyze the bromine-based flame retardant in electrical and electronic equipments, plastic, rubber and decorative materials of car.