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Class 1 Residual Solvents for USP <467> Water-Soluble Articles on Rxi-624Sil MS

GC_PH1160
PeakstR (min)Conc.
(µg/mL)
1.1,1-Dichloroethene3.5860.07
2.1,1,1-Trichloroethane8.5360.08
3.Carbon tetrachloride9.0420.03
4.Benzene9.7870.02
5.1,2-Dichloroethane10.1120.04
* DMSO interference
ColumnRxi-624Sil MS, 30 m, 0.32 mm ID, 1.80 µm (cat.# 13870)
Standard/SampleResidual Solvents - Class 1 (cat.# 36279)
Diluent:water
Injectionheadspace-loop split (split ratio 5:1)
Liner:1mm Split (cat.# 20972)
Headspace-Loop
Inj. Port Temp.:140 °C
Instrument:Tekmar HT3
Inj. Time:1 min
Transfer Line Temp.:110 °C
Valve Oven Temp.:110 °C
Sample Temp.:80 °C
Sample Equil. Time:60 min
Vial Pressure:10 psi
Pressurize Time:0.5 min
Pressure Equilibration Time:0.05 min
Loop Pressure:5 psi
Loop Fill Time:0.1 min
Oven
Oven Temp.:40 °C (hold 20 min) to 240 °C at 10 °C/min (hold 20 min)
Carrier GasHe, constant flow
Linear Velocity:35 cm/sec
Dead Time:1.45 min @ 40 °C
DetectorFID @ 250 °C
Data Rate:5 Hz
InstrumentAgilent/HP6890 GC
NotesColumns were run under identical conditions.
AcknowledgementTeledyne Tekmar