Electron Capture Negative Ion Mass Spectra of Selected Polybrominated Diphenyl Ethers (PBDEs) and Related Compounds The following 61 mass spectra were measured using the JMS-GCmateII (JEOL Peabody, MA, USA) in the electron-capture negative ionization (ECNI) mode; methane (99.99%) was used as a reagent gas. Standards were introduced by gas chromatography (GC) (6890N, Agilent Tech., Palo Alto, CA) equipped with an on-column injector and a 30 m column (J&W Scientific, Agilent Tech.,) (DB-5HT, 30 m x 0.25 mm, 0.1 µm stationary phase). Injections (1 µL), were made on a low temperature on-column injector, carry gas helium. Initial injector temperature 55 o C, increased to 150 o C at 30- o C/minute o C, then rate is reduced to 10- o C/minute until 300 o C was reached, held for 15 minutes, increased to 350 o C at 30- o C/minute and held at 350 o C for 5 minutes, as a bake-out procedure prior to subsequent analysis. The instrument was tuned and calibrated using 1000:1 mixture of Perfluorokerosene (PFK) and 1,2,4 Trichlorobenzene, tune target ion 331 m/z. Typical values for the ion source were: electron energy 50 eV, filament 300 uA, source temperature 300 o C. ECNI mass spectra were measured in full scan (10 to 550 m/z), at 1.0 scans/sec. All reported mass spectra were identified at > ½ peek height. Mark J. La Guardia Virginia Institute of Marine Science Gloucester Point, Virginia [email protected]
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Electron Capture Negative Ion Mass Spectra of Selected Polybrominated Diphenyl Ethers (PBDEs) and Related Compounds
The following 61 mass spectra were measured using the JMS-GCmateII (JEOL Peabody,
MA, USA) in the electron-capture negative ionization (ECNI) mode; methane (99.99%) was used as a reagent gas. Standards were introduced by gas chromatography (GC) (6890N, Agilent Tech., Palo Alto, CA) equipped with an on-column injector and a 30 m column (J&W Scientific, Agilent Tech.,) (DB-5HT, 30 m x 0.25 mm, 0.1 µm stationary phase). Injections (1 µL), were made on a low temperature on-column injector, carry gas helium. Initial injector temperature 55 oC, increased to 150 oC at 30-oC/minute oC, then rate is reduced to 10-oC/minute until 300 oC was reached, held for 15 minutes, increased to 350 oC at 30-oC/minute and held at 350 oC for 5 minutes, as a bake-out procedure prior to subsequent analysis.
The instrument was tuned and calibrated using 1000:1 mixture of Perfluorokerosene
(PFK) and 1,2,4 Trichlorobenzene, tune target ion 331 m/z. Typical values for the ion source were: electron energy 50 eV, filament 300 uA, source temperature 300 oC. ECNI mass spectra were measured in full scan (10 to 550 m/z), at 1.0 scans/sec. All reported mass spectra were identified at > ½ peek height.
Mark J. La Guardia Virginia Institute of Marine Science