DIRECT TEMPERATURE RESOLVED HRMS OF FIRE-RETARDED POLYMERS BY IN-SOURCE PYMS ON AN EXTERNAL ION-SOURCE FOURIER-TRANSFORM ION-CYCLOTRON RESONANCE MASS-SPECTROMETER

Rapid microscale analysis with high mass accuracy is demonstrated by direct temperature resolved desorption and pyrolysis from a Pt/Rh filament probe inside the external ion source of a 7-T FTICR-MS. High pressure generated during desorption and pyrolysis in the ion source does not interfere with analysis in the hydrocarbon-free UHV of the ICR cell, thus allowing short observation cycles at high resolution. The typical conditions achieved, a mass resolution (m/Delta m)(50%) equals 50 000 at m/z 600 with cycle times of 100 ms, were used to analyze isobaric compound mixtures generated by pyrolysis of brominated fire-retarded polymers spiked with antimony-containing synergists. Unknown fire-retarded polymer blends sampled from household appliances were found to contain brominated biphenyls, brominated diphenyl ethers, tetrabromoBisphenol-A and its butylated isomers, polystyrene, and antimony oxides. High-resolution temperature-resolved analysis by ''in-source'' pyrolysis FTICR-MS confirms the elemental composition. The resolution is sufficient to separate the nominally isobaric ions from the antimony(III) oxide (Sb4O6) synergist and the n-butyl ether derivative of tetrabromoBisphenol-A.