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GC/MS contamination peak

Posted: Wed Aug 18, 2021 8:16 pm
by Trishia
Recently did full maintenance on GC/MS; cleaned the source, replaced the gold seal, inlet liner, septa as well as installed a new column with a new guard column (we were starting to observe lots of ghost peaks and bleed since it had been in use for now a while). I'm observing a contamination peak with 129 and 147 main ions, which seems to correspond to Bis(2-ethylhexyl) adipate - https://imgur.com/us01aBd - both in split and splitless mode. Pretty confident it's from the GC side since if I do a run while keeping the temperatures of the inlet and oven low (50-60), I do not observe this peak.

Interestingly enough, when running a method with a higher starting oven temperature, the abundance of the peak decreases until it pretty much disappears if the starting temperature is above ~175-200 degC. The peak also seems to be absent if I run while heating the oven, but keeping the inlet temperature off. So, thinking this might be an inlet issue, I then replaced the split vent trap, cleaned the inlet itself, as well as cleaned the vent line - also baked out the column some before re-installing. I am still seeing this contamination peak!

At this point, I feel I have replaced everything what am I missing? Anyone know what this peak could be characteristic of?

Re: GC/MS contamination peak

Posted: Wed Aug 18, 2021 9:45 pm
by James_Ball
Have you performed a run without a physical injection, just hitting the start button or with the syringe removed?

That will let you know if it is in the inlet itself or possibly a contamination in the solvent.

Re: GC/MS contamination peak

Posted: Thu Aug 19, 2021 1:34 pm
by Consumer Products Guy
Wrap the septum in aluminum foil and try some runs without injections.

Re: GC/MS contamination peak

Posted: Thu Aug 19, 2021 2:14 pm
by Trishia
Meant to mention that all runs were done without injections. Peak is still there with septa wrapped in foil...