Abstract
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/Δm) 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, tetra-bromoBisphenol-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 (Sb 4 O 6 ) synergist and the n-butyl ether derivative of tetrabromoBisphenol-A.
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