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Residual Solvents Class 2 — Mix A on Rxi-624Sil MS (G43) by USP <467>

GC_PH1175
PeakstR (min)Conc.
(µg/mL)
1.Methanol2.4715.00
2.Acetonitrile4.262.05
3.Methylene chloride4.573.00
4.trans-1,2-Dichloroethene5.074.68
5.cis-1,2-Dichloroethene7.394.68
6.Tetrahydrofuran8.083.60
7.Cyclohexane9.1019.40
8.Methylcyclohexane14.695.90
PeakstR (min)Conc.
(µg/mL)
9.1,4-Dioxane15.691.90
10.Toluene22.414.45
11.Chlorobenzene26.691.80
12.Ethylbenzene27.001.84
13.m-Xylene27.316.51
14.p-Xylene27.321.52
15.o-Xylene28.080.98
16.Cumene28.830.35
Conc. prepared according to USP <467> method.
ColumnRxi-624Sil MS, 30 m, 0.32 mm ID, 1.80 µm (cat.# 13870)
SampleResidual solvents Class 2 — Mix A (2013 Rev) (cat.# 36012)
Diluent:Water
Injection
Inj. Vol.:1000 µL headspace-loop split (split ratio 5:1)
Liner:Premium 1.0 mm ID straight inlet liner (cat.# 23333.1)
Headspace-Loop
Inj. Port Temp.:140 °C
Instrument:Tekmar HT-3
Inj. Time:1.0 min
Transfer Line Temp.:105 °C
Valve Oven Temp.:105 °C
Needle Temp.:85 °C
Sample Temp.:80 °C
Sample Equil. Time:60 min
Mixer time:5.0 min
Mixing level:5
Mixer stabilize time:0.50 min
Vial Pressure:10 psi
Pressurize Time:5.0 min
Pressure Equilibration Time:0.20 min
Loop Pressure:5.0 psi
Loop Fill Time:2.0 min
Oven
Oven Temp.:40 °C (hold 20 min) to 240 °C at 10 °C/min (hold 20 min)
Carrier GasHe, constant flow
Flow Rate:2.2 mL/min
DetectorFID @ 250 °C
Make-up Gas Flow Rate:45 mL/min
Make-up Gas Type:N2
Hydrogen flow:40 mL/min
Air flow:450 mL/min
Data Rate:20 Hz
InstrumentAgilent/HP6890 GC