694
GC CHROMATOGRAMS |
PHARMACEUTICAL
Organic Volat i le Impur i t ies/Residual Solvents
Class 1 Residual Solvents for Water-Soluble Articles on Rxi®-624Sil MS
GC_PH1144
Conc.
Peaks
RT (min.)
(µg/mL)
1. 1,1-Dichloroethene
3.586
0.07
2. 1,1,1-Trichloroethane
8.536
0.08
3. Carbon tetrachloride
9.042
0.03
4. Benzene
9.787
0.02
5. 1,2-Dichloroethane
10.112
0.04
* DMSO Interference
Column
Rxi
®
-624Sil MS, 30 m, 0.32 mm ID, 1.80 µm (cat.# 13870)
Sample
Residual Solvents - Class 1 (cat.# 36279)
Diluent:
water
Injection
headspace-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 Gas
He, constant flow
Linear Velocity:
35 cm/sec.
Dead Time:
1.45 min. @ 40 °C
Detector
FID @ 250 °C
Data Rate:
5 Hz
Instrument
Agilent/HP6890 GC
Acknowledgement Teledyne Tekmar
GC_PH1146
Class 2 - Mix A Residual Solvents for Water-Soluble Articles on Rxi®-624Sil MS
Conc.
Peaks
RT (min.) (µg/mL)
1. Methanol
2.281
25.00
2. Acetonitrile
4.009
3.42
3. Dichloromethane
4.313
5.00
4.
trans
-1,2-Dichloroethene 4.798
7.83
5.
cis
-1,2-Dichloroethene
7.028
7.83
6. Tetrahydrofuran
7.706
5.75
7. Cyclohexane
8.708
32.33
8. Methylcyclohexane
14.099
9.83
9. 1,4-Dioxane
15.054
3.17
10. Toluene
22.018
7.42
11. Chlorobenzene
26.570
3.00
12. Ethylbenzene
26.837
3.07
13.
m
-Xylene
27.147 10.85
14.
p
-Xylene
27.147
2.53
15.
o
-Xylene
27.927
1.63
Column
Rxi
®
-624Sil MS, 30 m, 0.32 mm ID, 1.80 µm (cat.# 13870)
Sample
Residual Solvents Class 2 - Mix A (cat.# 36271)
Diluent:
water
Injection
headspace-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 Gas
He, constant flow
Linear Velocity:
35 cm/sec.
Dead Time:
1.45 min. @ 40 °C
Detector
FID @ 250 °C
Data Rate:
5 Hz
Instrument
Agilent/HP6890 GC
Acknowledgement Teledyne Tekmar
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TelNo : 03 9762 2034 . . . in AUSTRALIA
Mar 2011
