GCMS drops in baseline with recovery during no-injection post maintenance

System specs:

Agilent 6890N with 5975 iMSD and MassHunter GCMS Acquisition/ Enhanced Chemstation Data Analysis

Split liner, helium carrier gas, flow=3ml/min during bake outs and 1mL/min all other time

 

The vacuum system failed over a weekend and was replaced with a refurbished unit. Pumped down and sat for a week at ambient temps. Then we changed the column (DB-1MS max temp 340'C) and septum as part of regular system maintenance. Air and water check passed with source and quad at 80'C. Baked column at 325'C attached to source for 2.5 hours. Checked condition of column (see attached document), then baked out MSD and ran a few no-injections with needle off. These are in full scan (50-550 mz) and look great minus the drops in baseline, which I have never seen before. Autotune looks good as well. Has anyone else ever seen this before? I don't know if you could call them negative peaks.

 

Any suggestions or comments would be greatly appreciated!

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  • Probably not helpful, but your background is relatively normal except that the 44 peak from CO2 is very high. Argon (40) is present in air at ~1% and C02 should be at ~400ppm (0.04%) a ratio of 25:1  Your ratios vary between ~14:1 and 7:1 the “wrong” way. The 207 siloxane peak only varies by <50% and the 281 siloxane peak seems to vary even less  - The CO2 may be adsorbed on an active surface between runs and desorbed as the system gets hot, so possible places are the injector/liner or injector trap filter. A stupid thought - You don’t have an instrument with liquid CO2 sub-ambient cooling, or another source of CO2 in the lab?

  • Thanks for the suggestion. It's unfortunate I can't find a scan to compare the CO2 and Argon to, because we usually scan only from 50-550 m/z. I have the injector off and replaced the inlet liner, but will check out the split vent trap. And no sources of CO2 in the lab.

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