Analytical methods

ExperimentID EXA000136
ChemicalID CH0000497
Chemical Name Endosulfan-I
Official Method No
Chromatography GC
Chromatography mfr. 6890, Agilent / 7683, Agilent
Column RH-12ms 60 m x 0.25 mm
Column mfr. INVENTX
Detector HRMS
Detector mfr. AutoSpec Ultima, Waters; AutoSpec Premier, Waters
Ionization SIM-EI
Extraction SPE
Extraction Details Sequentially extracted with glass fiber filter GC50 and with SPE disk C18FF. GC50 filter residue: Ultrasonic extraction with acetone and Toluene; Samples captured by C18FF: Eluted with Methanol, Acetone and Toluene
Clean-up 1st Washing
Clean-up 1st Details Washed in 5% sodium chloride aqueous solution
Clean-up 2nd SPE (Envi Carb); Column cleanup
Clean-up 2nd Details Envi Carb: Eluted with Hexane; Column cleanup: Florisil, Sulfuric Acid/Silica Gel (50:50), Linced with Hexane, Eluted with Dichloromethane/Hexane (30:70)
Clean-up Spike 13C9alfa-Endosulfan
Syringe Spike 13C12-PCB#70, #111, #38, or #178
Derivatization
Recovery Correction
Instrument Detection Limit
Instrument Quantification Limit
Method Detection Limit 40 pg/L
Method Quantification Limit 120 pg/L
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.447; Resolution: 10,000
RegisterDate 2021/5/21
UpdateDate 2021/5/21