Spectra Library Electron Capture Negative Ion (ECNI) Mass Spectra of Selected Polybrominated Diphenyl Ethers (PBDEs)

Transcription

1 Spectra Library Electron Capture Negative Ion (ECNI) Mass Spectra of Selected Polybrominated Diphenyl Ethers (PBDEs) The following 63 mass spectra were measured by gas chromatography (GC) (6890N, Agilent Tech., Palo Alto, CA) with mass spectrometer (MS) detection (JMS-GC Mate II, JEL, Peabody, MA.) using ECNI; methane (99.99%) as the reagent gas. (The JMS-GC Mate II is a benchtop magnetic sector MS with similar ion optics as larger highresolution double-focusing MS systems). Individual PBDE standards were obtained from third-party analytical standard manufacturers. Each PBDE standard was diluted with hexane to a final injection concentration of approximately 500 pg/μl, on-column. Standards were introduced (1-μL) into the split/splitless injector, equipped with a glass liner (1 mm, ID), using a 15 m retention column (J&W Scientific, Agilent Tech., DB- 5T, 15 m x 0.25 mm, 0.1 μm stationary phase) to separate analytes from their carrier solvent (hexane). The injector temperature was 300 o C and initial carrier gas (helium) head pressure was 50-psi. The split vent was opened and pressure reduced to 15.2 psi after 4 minutes, following sample injection. Thereafter, column flow rate (1.5 ml/min.) was kept constant throughout the remaining portion of the run, by increasing carrier gas pressure at the head of the column compensating for increasing oven temperatures. Initial column oven temperature was 90 o C, held for 4 minutes, then increased to 150 o C at 30 o C/minute, then 10 o C/minute to 300 o C, and held for 7 minutes. Then increased to 350 o C at 30 o C/minute and held at 350 o C for 5 minutes, as a column bake-out procedure. The MS was tuned and calibrated with a 1000:1 mixture of perfluorokerosene (PFK) and 1,2,4 trichlorobenzene, using ion 331 m/z, resolution Mass calibration included 84 points, ranging from 35.0 to 998 m/z. Typical values for the ion source were: electron energy 200 ev, filament 300 µa. A source temperature of 200 o C was observed optimal to produce fragmentation characteristic of PBDE ether cleavage and molecular ions for the higher brominated compounds. ECNI mass spectra were collected in full scan (10 to 1000 m/z), at 1.0 scan/sec. All reported spectra were identified at greater than one-half peak height.

2 CNTENTS Compound IUPAC ID Page Compound IUPAC ID Page 2, 4-di BDE 3 BDE-7 1 2, 2, 3,3, 4,4, 6-hepta BDE 3 BDE ,4 -di BDE 3 BDE ,2, 3,3, 4, 5, 6-hepta BDE 1 BDE ,2, 3,3, 4,5, 6-hepta BDE 1 BDE ,2, 4-tri BDE 3 BDE ,2, 3,3, 5, 6,6 -hepta BDE 1 BDE , 4,4 -tri BDE 3 BDE ,2, 3, 4,4, 5, 5 -hepta BDE 3 BDE ,4, 6-tri BDE 4 BDE ,2, 3, 4,4, 5, 6-hepta BDE 3 BDE , 3,4-tri BDE 4 BDE ,2, 3, 4,4, 5,6 -hepta BDE 1 BDE ,3, 4-tri BDE 4 BDE ,2, 3, 4,4, 5, 6-hepta BDE 3 BDE , 4,4 -tri BDE 4 BDE ,2, 3, 4,4, 6,6 -hepta BDE 3 BDE ,2, 3, 4, 5,5, 6-hepta BDE 1 BDE ,2, 3,4 -tetra BDE 1 BDE , 2, 3,4, 5, 6,6 -hepta BDE 1 BDE ,2, 4,4 -tetra BDE 3 BDE , 3,3, 4,4, 5, 6-hepta BDE 1 BDE ,2, 4,5-tetra BDE 1 BDE , 3,3, 4,4, 5, 6-hepta BDE 3 BDE ,2, 4,5 -tetra BDE 3 BDE , 3,3, 4, 5,5, 6-hepta BDE 1 BDE ,2, 4,6 -tetra BDE 1 BDE ,3, 4,4 -tetra BDE 3 BDE ,2, 3,3, 4,4, 5,5 -octa BDE 3 BDE , 4,4, 5-tetra BDE 1 BDE ,2, 3,3, 4,4, 5,6 -octa BDE 3 BDE , 4,4, 6-tetra BDE 4 BDE ,2, 3,3, 4,4, 6,6 -octa BDE 3 BDE ,3, 4,4 -tetra BDE 3 BDE ,2, 3,3, 4, 5,5, 6-octa BDE 1 BDE ,2, 3,3, 4,5, 6,6 -octa BDE 3 BDE ,2, 3, 4,4 -penta BDE 3 BDE ,2, 3,3, 5,5, 6,6 -octa BDE 1 BDE ,2, 3, 4, 5-penta BDE 1 BDE ,2, 3, 4,4, 5,5, 6-octa BDE 1 BDE ,2, 4,4, 5-penta BDE 3 BDE ,2, 3, 4,4, 5, 6,6 -octa BDE 1 BDE ,2, 4,4, 6-penta BDE 3 BDE , 3,3, 4,4, 5,5, 6-octa BDE 1 BDE ,2, 4, 5,5 -penta BDE 1 BDE ,2, 4,5,6 -penta BDE 1 BDE ,2, 3,3, 4,4, 5,5, 6-nona BDE 3 BDE ,3,4,5, 6-penta BDE 4 BDE ,2, 3,3, 4,4, 5, 6,6 -nona BDE 3 BDE ,3, 4,4, 5-penta BDE 1 BDE ,2, 3,3, 4, 5,5, 6,6 -nona BDE 3 BDE , 3, 4,4, 5-penta BDE 3 BDE ,3, 4,5,5 -penta BDE 3 BDE ,2, 3,3, 4,4, 5,5, 6,6 -deca BDE 3 BDE ,3, 4,4, 5-penta BDE 3 BDE ,2, 3,3, 4,4 -hexa BDE 1 BDE ,2, 3,4,4, 5 -hexa BDE 3 BDE ,2, 3, 4,5, 6-hexa BDE 1 BDE ,2, 4,4, 5,5 -hexa BDE 3 BDE ,2, 4,4, 5,6 -hexa BDE 3 BDE ,2, 4,4, 6,6 -hexa BDE 4 BDE , 3,3, 4,4, 5-hexa BDE 3 BDE , 3, 4,4, 5, 6-hexa BDE 4 BDE Standard Suppliers: 1=AccuStandard, Inc. New aven CT. USA, 2=Ultra Scientific, North Kingstown, RI. USA, 3=Wellington Laboratories, ntario, Canada, 4=Cambridge Isotope Laboratories, Andover, MA. USA

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