Posted: Tue Sep 15, 2009 10:00 pm
Alrighty, after much research, got it working. Will list all the settings in case anyone with the same setup is having issues.
Clarus 500 GC
Turbomatrix 40 Headspace Sampler (pressure-balanced)
Clarus 500 Settings:
Column: 30m x 0.53mm id x 3 micron film of DB-624
Zero dilution outer/inner split/splitless liners used instead of standard 4mm id split liner
Injector, detector, and oven temperature programs as per USP
Carrier flow: 3 ml/min He
Split: 5:1
Hydrogen flow: 45 ml/min
Air flow: 450 ml/min
Turbomatrix 40 Headspace Settings:
Carrier Pressure: 48 psi
Oven Temp: 80
Needle Temp: 105
Transfer Temp: 110
Thermostat Time: 20
Pressurize Time: 2.0
Inject Time: 0.12
Withdraw Time: 0.1
Vial Venting: On
Operating Mode: Constant
Injection Mode: Time
Transfer line: deactivated fused silica line 0.32 mm id
Chromatography is beautiful...even better than the sample chromatograms I had on hand. As far as I can see, the biggest changes that made it function properly were the installation of the zero dilution liners, use of the bigger id column (though I suspect that my 0.32 mm id column might just have gone bad), and the headspace carrier pressure increase to 48 psi to ensure maximal headspace transfer.
Clarus 500 GC
Turbomatrix 40 Headspace Sampler (pressure-balanced)
Clarus 500 Settings:
Column: 30m x 0.53mm id x 3 micron film of DB-624
Zero dilution outer/inner split/splitless liners used instead of standard 4mm id split liner
Injector, detector, and oven temperature programs as per USP
Carrier flow: 3 ml/min He
Split: 5:1
Hydrogen flow: 45 ml/min
Air flow: 450 ml/min
Turbomatrix 40 Headspace Settings:
Carrier Pressure: 48 psi
Oven Temp: 80
Needle Temp: 105
Transfer Temp: 110
Thermostat Time: 20
Pressurize Time: 2.0
Inject Time: 0.12
Withdraw Time: 0.1
Vial Venting: On
Operating Mode: Constant
Injection Mode: Time
Transfer line: deactivated fused silica line 0.32 mm id
Chromatography is beautiful...even better than the sample chromatograms I had on hand. As far as I can see, the biggest changes that made it function properly were the installation of the zero dilution liners, use of the bigger id column (though I suspect that my 0.32 mm id column might just have gone bad), and the headspace carrier pressure increase to 48 psi to ensure maximal headspace transfer.