Analytical methods

ExperimentID EXA000430
ChemicalID CH0000107
Chemical Name BDE99
Official Method No
Chromatography GC
Chromatography mfr. 6890, Agilent; 7683, Agilent
Column BPX-DXN 30 m x 0.25 mm or BP-1 15 m x 0.25 mm, 0.1 μm
Column mfr. Trajan; Trajan
Detector HRMS
Detector mfr. AutoSpec Ultima, Waters; AutoSpec Premier, Waters
Ionization SIM-EI
Extraction Solvent Extraction
Extraction Details Ultrasonic extraction: Extracted with Acetone. After filtration, wash the residue in Acetone.; Soxhlet Extraction: Extracted with Toluene.
Clean-up 1st Malti-layer column cleanup
Clean-up 1st Details Malti-layer column cleanup: Silica Gel, Copper powder, Silica Gel Sulfate, Anhydrous sodium sulfate; Eluted with Hexane (First fraction), Dichloromethane/Hexane (20:80) (Second fraction)
Clean-up 2nd GPC; Multi-layer column cleanup
Clean-up 2nd Details Gel permeation chromatography: Acetone/Cyclohexane (20:80), Precolumn: Shodex EV-G AC; Column: Shodex EV-2000 AC; Multi-layer column cleanup: Active carbon-dispersed silica gel, Sodium sulfate; Eluted with Dichloromethane/Hexane (25:75)
Clean-up Spike 13C12-PBDE#3, #15, #28, #47, #99, #126, #153, #154, #183, #197, #207 or #209
Syringe Spike PBDE#138; PBDE#206
Recovery Correction
Instrument Detection Limit
Instrument Quantification Limit
Method Detection Limit 1 pg/g dry
Method Quantification Limit 3 pg/g dry
Recovery (CRM)
Recovery (spiked)
Recovery (IS)
Remarks Analysis method: p2-3; Resolution: 10,000
RegisterDate 2022/7/12
UpdateDate 2022/7/12