Analytical methods

ExperimentID EXA000804
ChemicalID CH0000096
Chemical Name ΣPCBs
Official Method No
Chromatography GC
Chromatography mfr. 7890, Agilent
Column RH-12ms 60 m x 0.25 mm
Column mfr. INVENTX
Detector HRMS
Detector mfr. AutoSpec Premier, Waters
Ionization SIM-EI
Extraction Soxhlet Extraction
Extraction Details Air collection: QFF, PUF and ACF; Extracted with Acetone and Toluene (QFF, ACF), with Acetone (PUF)
Clean-up 1st Column cleanup
Clean-up 1st Details Column cleanup[1-1]: Supelclean Sulfoxide 6 g; Remove interfering substance with Hexane; Eluted with Acetone; Colum cleanup[2]: Florisil、Eluted with Dichloromethane/Hexane (50:50)
Clean-up 2nd Column cleanup
Clean-up 2nd Details Colum cleanup[1-2]Silica gel, Sulfuric acid/Silica gel (22:78), Sulfuric acid/Silica gel (44:56), Silica gel, Potassium hydroxide/Slica gel (2:98), Silica gel; Eluted with Hexane
Clean-up Spike Sampling spike: 13C12-PCB#1, #3, #4, #15, #19, #37, #54, #77, #81, #104, #105, #114, #118, #123, #126, #155, #156, #157, #167, #169, #188, #189, #202, #205, #206, #208 or #209; Cleanup spike (for PUF): 13C12-Dicofol
Syringe Spike Syringe Spike for Cleanup[1]: 13C12-PCB#9, #52, #70, #101, #138, #194; Syringe Spike for Cleanup[2]: 13C12-PCB#70
Derivatization
Recovery Correction
Instrument Detection Limit
Instrument Quantification Limit
Method Detection Limit 0.6 pg/m3
Method Quantification Limit 1.8 pg/m3
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.6; Resolution: 10,000
RegisterDate 2023/3/08
UpdateDate 2023/3/08