Analytical methods

ExperimentID EXA000168
ChemicalID CH0000074
Chemical Name PCB167
Official Method No
Chromatography GC
Chromatography mfr. 6890, Agilent; 7683, Agilent
Column HT8-PCB 60 m x 0.25 mm
Column mfr. GL Sciences
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
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
Clean-up Spike 13C12-PCB#3, #8, #11, #28, #31, #52, #77, #81, #101, #105, #114, #118, #123, #126, #138, #153, #156, #157, #167, #169, #170, #180, #189, #206 or #209
Syringe Spike 13C12-PCB#9, #19, #70, #111, #155, #178 or #202
Derivatization
Recovery Correction
Instrument Detection Limit
Instrument Quantification Limit
Method Detection Limit 0.3 pg/g dry
Method Quantification Limit 0.7 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