Analytical methods

ExperimentID EXA000124
ChemicalID CH0000107
Chemical Name BDE99
Official Method No
Chromatography GC
Chromatography mfr. 6890, Agilent / 7683, Agilent
Column BPX-DXN 30 m x 0.25 mm or BP-1 15 m x 0.25 mm, 0.1 μm
Column mfr. Trajan; Trajan
Detector MS
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 Column cleanup
Clean-up 2nd Details Florisil, Sulfuric Acid/Silica Gel (50:50), Eluted with Dichloromethane/Hexane (20:80)
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 2 pg/L
Method Quantification Limit 6.0 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.437; Resolution: 10,000
RegisterDate 2021/5/21
UpdateDate 2021/5/21