痕量PBBs/PBDEsGC/MS分析法中PCB及其衍生物干扰消除方法

电子电气产品中痕量阻燃剂聚溴联苯/聚溴联苯醚(PBBs/PBDEs)的检测通常采用气相色谱/质谱(GC-MS)联用法,但该法是建立在持久性污染物多氯化苯/多氯化萘(PCBs/PCNs)基础上,因此此类物质干扰不可避免。为了解决此类问题,提出了2种解决方法:1)阴离子化学电离-气相色谱/质谱联用法(GC/MS-NICI)和电子轰击-气相色谱/质谱联用法(GC/MS-EI)联合使用;2)以YMC ODS-C18为载体,基质固相分散法(MSPD)吸附分离。结果显示,前者可以同时洞察聚溴联苯和联苯醚的分子链断裂后阴离子碎片[Br]-,[HBr2]-和分子链段碎片[M+2]+,[M+4]+,[M+6]+,[M+8]+的滞留峰,增加了对溴系阻燃剂的选择性。后者可以有效分离多种多氯化苯与聚溴联苯醚的色谱峰,这为溴系阻燃剂气相色谱/质谱联用分析法中多氯化苯及其衍生物干扰提供了新的解决方法。采用此方法对8类电子电气产品中10种聚溴联苯醚和多氯化苯进行加标回收实验及精密度分析,回收率在60%～98%,相对误差在9.5%以内,符合国际电工委员会(IEC)对溴系阻燃剂检测精度要求,说明方法具有较高的可靠性,也为我国电子电气业更好遵守...

Interference elimination of PCB and its ramification in determining trace PBBs/PBDEs by GC/MS

The normal method to determine the trace brominated flame retardants such as polybrominated biphenyls(PBBs) and polybrominated diphenylethers(PBDEs) contained in the electronic and electrical products is gas chromatography/mass spectrometry(GC/MS).However,the method is based on the determinations of the persistent organic pollutants(POPs) such as polychlorinated biphenyls(PCBs),and polychlorinated naphthalene(PCNs) etc.The interferences of those compounds are inevitable.Therefore,in order to overcome this p...