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Dynamic Headspace USP <467> solvents on Rtx-1301 (G43)

GC_PH00811
PeakstR (min)sample concentration (µg/ml)
1.Dichloromethane5.13712.0
2.Chloroform9.2601.2
3.Benzene11.1450.04
4.Trichloroethylene14.6011.6
5.1,4-Dioxane17.3497.6
ColumnRtx-1301 (G43), 30 m, 0.53 mm ID, 3.00 µm (cat.# 16085-126)
SampleUSP <467> Calibration Mixture #5 (cat.# 36007)
Diluent:DMSO stock standard
Conc.: To each 22mL headspace vial 5ml water, ~ 1.0g of sodium sulfate and 100µL of stock standard were added. The preparations yielded the concentrations above.
Injectionheadspace-trap split
Oven
Oven Temp.:40 °C (hold 20 min) to 240 °C at 25 °C/min (hold 10 min)
Carrier GasHe, constant flow
Flow Rate:5 mL/min
DetectorFID @ 250 °C
Make-up Gas Flow Rate:45 mL/min
NotesDetector:
Hydrogen flow: 40 mL/min
Air flow: 450 mL/min

Dynamic Headspace (Trap) Conditions:
Instrument: Teledyne Tekmar HT3
Valve oven temp.: 150°C
Transfer line temp.: 150°C
Standby flow rate: 10mL/min.
Trap standby temp.: 40°C
Platen/sample temp.: 80°C
Sample equil. time: 15.00 min.
Mixer time: 2.00 min.
Mixing level: 5
Mixer stabilize time: 0.50 min.
Sweep flow rate: 75mL/min.
Sweep flow time: 3.00 min.
Dry purge time: 5.00 min.
Dry purge flow: 50mL/min.
Dry purge temp.: 25°C
Desorb preheat: 245°C
Desorb temp.: 250°C
Desorb time: 1.00 min.
Trap bake temp.: 300°C
Trap bake time: 6.00 min.
Trap bake flow: 450mL/min.