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QuEChERS Extract of NIST SRM 2974a Freeze-Dried Mussel Tissue (GCxGC contour plot)

ColumnRxi-17Sil MS 30 m, 0.25 mm ID, 0.25 µm (cat.# 14123)
Rxi-1ms 1.2 m, 0.15 mm ID, 0.15 µm (cat.# custom)
SampleNIST SRM 2974a freeze-dried mussel tissue with incurred residues
Diluent:Acetonitrile
Injection
Inj. Vol.:1 µL splitless (hold 1 min)
Liner:Splitless taper (4 mm) w/semivolatiles wool (cat.# 20798-231.1)
Inj. Temp.:250 °C
Purge Flow:40 mL/min
Oven
Oven Temp.:Rxi-17Sil MS: 90 °C (hold 1 min) to 320 °C at 3.75 °C/min (hold 2.67 min)
Rxi-1ms: 95 °C (hold 1 min) to 325 °C at 3.75 °C/min (hold 2.67 min)
Carrier GasHe, corrected constant flow (2.2 mL/min)
Modulation
Modulator Temp. Offset:20 °C
Second Dimension Separation Time:3 sec
Hot Pulse Time:0.9 sec
Cool Time between Stages:0.6 sec
DetectorTOFMS
Transfer Line Temp.:300 °C
Analyzer Type:TOF
Source Temp.:250 °C
Electron Energy:70 eV
Mass Defect:-20 mu/100 u
Solvent Delay Time:5 min
Tune Type:PFTBA
Ionization Mode:EI
Acquisition Range:45 to 550 amu
Spectral Acquisition Rate:100 spectra/sec
InstrumentLECO Pegasus 4D GCxGC-TOFMS
NotesPAHs (shown in box) elute in a relatively narrow band and are identified by the white peak marker dots.