Analytical methods

ExperimentID EXA000801
ChemicalID CH0001180
Chemical Name ΣChlorinated tridecanes
Official Method No
Chromatography GC
Chromatography mfr. 6890, Agilent; 7890, Agilent
Column DB-5ms 15 m x 0.25 mm
Column mfr. Agilent
Detector TOF-MS
Detector mfr. AutoSpec Ultima, Waters; AutoSpec Premier, Waters
Ionization EI or NICI
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 Column cleanup
Clean-up 2nd Details Column cleanup: Florisil, Anhydrous sodium sulfate; Eluted with Dichloromethane/Hexane (20:80)
Clean-up Spike 1,5,5,6,6,10-Hexachlorinated decanes-13C10
Syringe Spike Naphthalene-d8; Acenaphtene-d10; Phenanthrene-d10; Fluoranthene-d10; Chrysene-d12
Derivatization
Recovery Correction
Instrument Detection Limit
Instrument Quantification Limit
Method Detection Limit 500 pg/g dry
Method Quantification Limit 1200 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.3-4; Resolution: 10,000
RegisterDate 2023/2/15
UpdateDate 2023/2/15