GC/MS contamination peak

Recently did full maintenance on GC/MS; cleaned the source, replaced the gold seal, inlet liner, septa as well as eventually 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 (plus the peak is consistent in its retention time).

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 the vent line, and replaced both septa and liner again - also baked out the column some before re-installing. I am still seeing this contamination peak!  Note that all runs were conducted without actual injections.

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

Thanks!

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  • Our first priority to see all pattern is okay or not..As ions multiplied by horn after separation from mass filter.

    In tune, there is some leak showing.

    That leak may be possible from joint of guard column.

    We have to see the locatiin of  bleeding at high temp and that is possible to joint of column..column nut with interface etc..

  • So the tune shows higher values for nitrogen and oxygen but I ran about 5 air/water checks before and after that tune and they come up with much better values (around 1.9 and 0.6), so I'm not really sure why they showed up higher in the tune.  I did a thorough leak check with both argon and an electronic detector and I'm pretty confident there is no actual leak.  It looks like the impurity builds up over time - currently running a couple of tests to confirm - which seems to support that it's coming from the inlet or start of the column.  I will change the cylinder and bypass the trap today for another test, but I seriously doubt that's the the issue given the time they've been in use.

  • Yes..

    It could be impurity.

    It could be ferrule contamination.

    It could be joint contamination.

    It could be column nut.

    It could be helium impurities.

    It could be trap filter connected with helium line.

    So we have to think all possibilities..

    I am sure, problem will solve.

    Actually, online, i can only comment but if i am offline there then will not comment.

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