Analytical methods

ExperimentID EXA000186
ChemicalID CH0000825
Chemical Name Σtetra-BDEs
Official Method No
Chromatography GC
Chromatography mfr. 6890, Agilent; 7683, Agilent
Column BPX-DXN 30 m x 0.25 mm or ENV-5ms 15 m x 0.25 mm, 0.1 μm
Column mfr. Trajan; Kanto Chemical
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 Sulfate treatment
Clean-up 1st Details Sulfate
Clean-up 2nd Multilayer column cleanup; GPC; Activated carbon column
Clean-up 2nd Details Multilayer column cleanup: Silica Gel, Copper powder, Silica Gel Sulfate, Anhydrous sodium sulfate. Washed/Eluted with Dichloromethane/Hexane (20:80); Gel permeation chromatography: Acetone/Cyclohexane (20:80), Precolumn: Shodex EV-G AC; Column: Shodex EV-2000 AC; Activated carbon column: Washed in Hexane. Eluted with 25% Dichloromethane/Acetone.
Clean-up Spike 13C12-PBDE#3, #15, #28, #47, #99, #126, #153, #154, #183, #197, #207 or #209
Syringe Spike 13C12-PBDE#138 or #206
Derivatization
Recovery Correction
Instrument Detection Limit
Instrument Quantification Limit
Method Detection Limit 6 pg/g dry
Method Quantification Limit 18 pg/g dry
Repeatability
Standard
Recovery (CRM)
Recovery (spiked)
Recovery (IS)
Protocol https://www.env.go.jp/chemi/kurohon/2019/shosai/3_7.pdf
Remarks Analysis method: p.438; Resolution: 10,000
RegisterDate 2021/5/24
UpdateDate 2021/5/24