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USP <467> Residual Solvents Class 3 MIx A on Rxi-624Sil MS

GC_PH1178
PeakstR (min)Conc.
(µg/mL)
1.n-Pentane2.715000
2.Ethanol2.825000
3.Diethyl ether2.965000
4.Acetone3.315000
5.Ethyl formate3.515000
6.2-Propanol3.525000
7.Methyl acetate3.705000
8.Methyl tert-butyl ether4.125000
9.1-Propanol4.685000
10.2-Butanone5.225000
11.Ethyl acetate5.295000
12.2-Butanol5.485000
PeakstR (min)Conc.
(µg/mL)
13.Isopropyl acetate6.255000
14.Isobutanol6.435000
15.n-Heptane6.775000
16.1-Butanol7.235000
17.Propyl acetate8.015000
18.4-Methyl-2-pentanone9.395000
19.3-Methyl-1-butanol9.655000
20.Isobutyl acetate10.165000
21.1-Pentanol10.945000
22.Butyl acetate11.545000
23.Dimethyl sulfoxide13.245000
24.Anisole13.565000
ColumnRxi-624Sil MS, 30 m, 0.32 mm ID, 1.80 µm (cat.# 13870)
SampleResidual Solvents Class 3 - Mix A (cat.# 36013)
Conc.:5000 µg/mL split 100:1
Injectionheadspace-loop split (split ratio 100:1)
Liner:Topaz 1 mm Split (cat.# 23333)
Headspace-Loop
Inj. Port Temp.:200 °C
Instrument:Tekmar HT-3
Inj. Time:1.0 min
Transfer Line Temp.:105 °C
Valve Oven Temp.:105 °C
Standby flow rate:50 mL/min
Sample Temp.:80 °C
Platen temp equil. time:80 min
Sample Equil. Time:1.0 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 psi
Loop Fill Time:2.0 min
Oven
Oven Temp.:35 °C (hold 3 min) to 60 °C at 24 °C/min to 80 °C at 3 °C/min to 280 °C at 25 °C/min
Carrier GasHe, constant flow
Flow Rate:2.7 mL/min
Linear Velocity:41 cm/sec
DetectorFID @ 300 °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