Analytical methods

ExperimentID EXA000764
ChemicalID CH0000818
Chemical Name Σtetra-CBs
Official Method No
Chromatography GC
Chromatography mfr. 6890, Agilent; 7890, 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 Extracted with Acetone; Shaken for 10 min., Sonicated for 15min., then Centrifugated (3,000rpm, 10 min.); Repeated these three times
Clean-up 1st Column cleanup
Clean-up 1st Details Silica Gel, Silica Gel Sulfate, Anhydrous sodium sulfate, Copper powder; Eluted with Hexane (First fraction), Dichloromethane/Hexane (20:80) (Second fraction)
Clean-up 2nd GPC
Clean-up 2nd Details 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, #202
Derivatization
Recovery Correction
Instrument Detection Limit
Instrument Quantification Limit
Method Detection Limit 0.3 pg/g dry
Method Quantification Limit 0.8 pg/g dry
Repeatability
Standard
Recovery (CRM)
Recovery (spiked)
Recovery (IS)
Protocol https://www.env.go.jp/chemi/kurohon/2021/shosai/5_3_2.pdf
Remarks Analysis method: p.3; Resolution: 10,000
RegisterDate 2023/2/15
UpdateDate 2023/2/15