Large volume injection GC-MS in electron capture negative ion mode utilizing isotopic dilution for the determination of polybrominated diphenyl ethers in air

A large volume injection GC-MS method for the determination of polybrominated diphenyl ethers (PBDEs) is presented. A loop-type injection system with an early solvent vapor exit has been constructed and evaluated. With this system sample volumes up to 500 muL could be injected with high reproducibility and low carry-over. The peak distortion problem associated with this kind of injection system is discussed in detail and solutions are suggested. We also introduce 13C-labeled BDE-209 as internal surrogate standard for the determination of high molecular weight PBDEs in low-resolution mass spectrometry electron capture negative ionization mode. The complete method has been applied to air samples from an electronic waste dismantling facility, collected with personal exposure measurement equipment. Nine BDE congeners have been identified and quantified.