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Carbondioxide problems in GCMS chromatogram

Discussions about GC and other "gas phase" separation techniques.

3 posts Page 1 of 1
Hi,
I have some problems with carbondioxide in my chromatogram from GCMS and I do not know why. Is there anyone that has experience with this and know how to remove it?
Is it in the GC column or in the MS? We recently changed GC column but it did not get better.

(We use dynamic headspace to collect volatiles and thermal desorption to transfer the volatiles to the coldtrap)

Best regards Therese
There are two possibilities for getting carbon dioxide into your instrument. The first is a leak in the GC/MS system, which would give a continuous signal for CO2. The other would be related to your sampling system, which would introduce CO2 with the sample and would give a chromatographic peak for CO2. (And, with a cold trap a leak in the GC system ahead of the cold trap can give a signal for CO2 when the trap is warm and reduced signal for CO2 when the trap is cold, if the trap is cold enough.)

I assume this is a continuous CO2 signal?

Some things to look at in that case:

The first thing to do is to be sure the instrument is leak tight. How does your air/water profile look on the instrument? Depending on the vendor you may be able to ratio the m/z 28 peak from air to a reference, such as m/z 69 in PFTBA to evaluate this.

If the instrument shows CO2 as a continuous background, it is a reasonable assumption that the CO2 is coming from the air. You should see a corresponding signal of m/z 18 from water if you will scan that low. With the instrument showing a profile on the display and the peak for m/z 18 showing, turn a can of "dust-off" or a similar product upside down and spray a short burst across the column a few cm from the detector end of the column so that a bit of frost forms on the column. Do this away from the ferrules - we do not want to cause thermal expansion/contraction. If the intensity of the signal drops, the water was coming through the column. If there was no effect on the m/z 18 signal, the water is not passing by that cold spot. Look for a leak downstream - the mass spectrometer. (Note that the frost will disappear and trapped water will be released and you will see a brief spike in signal.)

I have heard of a thermal desorbtion system that gave the user continuous trouble with leaks. I know they removed the thermal desorbtion unit, but that decision may have been made for unrelated reasons.
look for ions 18 (H2O), 28 (N2), 32 (O2), and of course 44 (CO2). The N2:O2 ratio will be about 4:1 for an atmospheric leak. If you are tuning using PFTBA the abundance of O2, N2, H2O should be 2-3% compared to ion 69.

If you see nitrogen and CO2 but not O2 you have a leak before your O2 filters on the carrier gas.
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