Low sensitivity for higher MW components in GC

Hello,

 

I am using an Agilent 7890B with HP-1MS column SN19091S-913E.  Periodically (~25%), when installing a new column, i run into issue where components eluting >35minutes have severely reduced sensitivity. GC parameters at the bottom using splitless injection.  

 

i.e, one standard will have component not detected, while a standard that is 2x concentrated will have area count 100.  I am using multiple equipment and verify there is no problem in standard prep because the other equipment have normal sensitivity and linearity.

 

I have reviewed common problems and solutions here...

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1) Standard too cold/compounds precipitate.

      - Unlikely to be cause because other equipment is operating fine at the exact same time using same standards.              -Also, previous column installed on the now troublesome equipment showed normal sensitivity.

2) Componds are not properly vaporizing in the injection port.

      -Removed glass wool from the liner and reinjected same standards.  No improvement to sensitivity.  Are there other ways to see if this is happening?

3) Column has contamination.

      -Issue has been found multiple times when installing brand new column, probably not the root cause.

4) There is a cold sport somewhere.

      -Not sure if changing column could introduce cold spot somewhere somehow.

5) High column bleed

      -Not observed

6) Purge valve (split) time set too short.

      -This would be a method problem.  This method shows normal sensitivity on other equipment and has on this equipment before replacing column.

7) Missing insulation around injection port.

      -Insulation present.

 

GC parameters below.

 

Injector temp: 300C

Detector (FID): 350C

Gas Flow: H2 40mL/min

                 Air 400 mL/min

           Makeup (He): 20 mL/min

           Constant Pressure: 20 PSI

 

60C start temperature for 1 min

10C/min to 300C

2.5C/min to 325C

325C hold for 20 mins.

 

I have just reinstalled the same column backwards with the outlet side now at the inlet, and cut off ~1foot of the inlet and installed at the outlet.  I am reinjecting same standards to see if maybe problem was on inlet side of column.

 

Since this problem occurs regularly frequently when installing new columns, does anyone have advice what i could try for troubleshooting next?

 

Thank you in advance.

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  • Hi acraig

     First replace saptum until if you don't detected leak because sometime tiny leak in saptum cause low sensitivity. 

    Second sometimes over tightening the ferrule  connection of column to injector cause constriction the flow and reduce analyte at detector, so reinstall connection between column

       and injector and with FID

     Don't over tightening connection  

  • I see the comment above from Gchaplain mentioning to ensure ferrule are tightened enough, and your comment mentioning not to over-tighten.  Is there any more advice your should give on how to tell they are tightened correctly?

     

    My practice has been if the ferrule isn't really deformed, but the column is snug and doesn't easily move, then it is tightened properly.  If the ferrule is deformed i take that as a sign of tightened too much.  Would you agree with this, or is there a different way you check your ferrule tightness?

     

    Thank you very much for the response!

  • It could still be the septum, they can be over tightened and cause a leak. If you have a leak detector handy it's very good for detecting helium leaking from joints in the system

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