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USP <467> Residual Solvents on Rtx-1301 (G43) by Static Headspace

PeakstR (min)Conc.
(µg/mL)
1.Dichloromethane 5.11012.0
2.Chloroform9.2851.2
3.Benzene 11.1730.04
4.Trichloroethylene 14.6471.6
5.1,4-Dioxane17.4367.6
image
GC_PH00810
ColumnRtx-1301 w/5m Integra-Guard, 30 m, 0.53 mm ID, 3.00 µm (cat.# 16085-126)
SampleUSP <467> Calibration Mixture #5 (cat.# 36007)
Diluent:DMSO
Conc.: To each 22 mL headspace vial 5ml water, ~ 1.0g of sodium sulfate and 100µL of stock standard were added.
Injectionheadspace-loop split (split ratio 2:1)
Headspace-Loop
Inj. Port Temp.:180 °C
Instrument:Teledyne Tekmar HT3
Inj. Time:1.0 min
Transfer Line Temp.:150 °C
Valve Oven Temp.:150 °C
Standby flow rate:10 mL/min
Sample Temp.:80 °C
Platen temp equil. time:2.0 min
Sample Equil. Time:15.0 min
Mixer time:2.0 min
Mixing level:5
Mixer stabilize time:0.5 min
Vial Pressure:15 psi
Pressurize Time:2.0 min
Pressure Equilibration Time:0.5 min
Loop Pressure:5 psi
Loop Fill Time:2.0 min
Loop fill equil. time:0.5 min
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
NotesFID conditions:
hydrogen flow: 40 mL/min.
air flow: 450 mL/min.
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