Contamination on GC-FID

Hi Everyone

I work with an Agilent GC6890N and since the beginning of the week, we have a contamination (one peak) in our system which I have no idea where it comes from. I have a picture:

This is a blank run with solvent MTBE (2-Methoxy-2-methylpropan). On RT 1.25 you can clearly see the contamination. 

First i did, was an instrument blank run (split injection), which was clean.So i assumed it comes from the injection or outside my system.

Here is what i tried:

- Fresh/other solvent

- Syringe cleaned/replaced

- Septa and liner replaced

- Wash vials, ans septas cleaned/replaced

- cleaned the inlet

I even did an run with empty vial and the peak is still present, so no solvent issue.

Has anyone another idea, from where this peak can come from?

Thanks in advance and have a nice day! 

Parents Reply
  • Hi!

    Try to bake out your column and condition it. 

    Try to reverse your column, install the injection side to detector side. Sometimes column will shoot stationary phase to the detector, because of sample and age of column.

    What is your configuration. Is this only column installed in-between evaporator and detector, or is there any switching valves installed?  

Children
  • Hi Beka

    We solved the problem. At the end, we just replaced the column. After baking out, cleaning the column and cutting it.
    But yes, it was the only column installed and no switching valves.

    I just wonder, why we could not see that on the blank run, any idea?

    Thanks and KR, GCarmen

  • Hi Carmen,

    Visually check your column in signs of contamination of stationary phase. It looks like your column was too old. In that case you could just reverse the column direction, and put for for long term conditioning at room temperature, then condition it at maximum temperature with desired flow for efficient analysis, then try to run with sample. Contamination of stationary phase at the end of column could break your peaks and shoot it as peak, or stationary phase could carryover with peak! If this column worked for many years usually nothing helps instead of changing to new column. Also, depends on your detector. FID should be cleaned at least once in a 6 month, what is the ceramic isolators condition, is there any electrical noises caused from electrometer, analog board all things need to be checked, sometimes just rebooting your instrument and PC could solve the problem. Your instrument has very simple configuration, so that is thy the solution should be very simple. 

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