Chromatography Forum

Hi, can someone help me?
I'm trying to develop a method for residual solvents(Methanol and Ethanol) in a solid sample. I am using HeadSpace Turbo matrix 16 coupled to GC HP6890 5973Mass Selective detector. I was using different methods that I have found online, but I don't get any signal.
MeOH and EtOH standards been made up in Water and 1ml of it been transfered to the Head SPsce vial, I heat it for 20 min at 80 degrees. If i'm running just water blank I get the same result,no differences. To me seems like there might be something wrong in the system, the tune evaluation looks perfect, no leaks.
I have checked the gas and looks alright through HeadSpace transfer line and I was running a standard using just the GCMS to see if there is any blockage in the system and I got poor sensitivity. Can someone advise me what might be the problem?
Thank you
Lumi
MET

Without knowing the details of your method its hard to say but I'm going to throw out a wild guess as I once ran into a similar problem that was fixed by checking the scan range of the MS and making sure it reached down into the ions that ethanol and methanol throw off.

I'm with Gizmo. For those compounds FID would work better.

Hi, thank you for your answers
My method has a scan range 25-100amu, I'm only looking for MeOH and EtOH.

Based on a what's been indicated so far I'd start looking at the injector - change the liner, septum, etc. etc. and make sure I got an appropriate response with just a directly injected standard without the headspace system hooked up.

Think you need to scan down to 10.