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GC/MS sticky sample prep
Posted: Sun Jun 14, 2009 3:02 am
by Contextions
I am trying to find ways to recycle tires and when I turn them into liquids I create a very sticky mess. I am afraid if I put these through the GC/MS the column will become clogged. May someone please offer some different suggestions of ways to analyze these concoctions?
Posted: Sun Jun 14, 2009 8:28 am
by bhuvfe
Can you dissolve easily your sticky sample in a good GC solvent to decrease the viscosity (chloroform, toluene, isooctane, THF, etc…)?
I inject sticky samples all the time (such as glue components) and the only thing you have to do is to choose a good liner with glass wool and to rinse a lot your syringe. This liner will have to be changed more often than a“normalâ€
Posted: Sun Jun 14, 2009 4:04 pm
by Consumer Products Guy
OK: if a component is volatile, it goes through column and comes out detector end.
If a component is non-volatile, it gets trapped on the glass wool in the liner, like "bhuvfe" stated. So it's really only the semi-volatile componets you need to be concerned with, the ones that might months to come out of the column. So go ahead and inject.
Posted: Sun Jun 14, 2009 8:33 pm
by Don_Hilton
I would suggest that you run the inlet a bit cooler than the maximum temperture of the column, if you can afford it. The compounds that elute very slowly through the column at the maximum will be more lilely to remain on the glass wool in the liner - as long as you change it frequently. (There are two schools of thought I've run into: first is run the liner hot and get everythign onto the column and second is run the liner cool and take the loss on analysis of high boilers - but save the column.)
Posted: Mon Jun 15, 2009 12:56 pm
by AICMM
Contextions,
There's pyrolysis if you want to spend some bucks. Complicated and subject to interpretation but provides additional information. There's temp programmable inlets which will give you some temperature speciation (again, if you want to spend some bucks...)
If just straight GC/MS, think about installing a guard column in front of your analytical column. A 5 meter length will give you a zone beyond your inlet that will tend to trap the really ugly stuff. Then trim this on a regular basis. Otherwise, trim your column on a regular basis and, as noted, pay attention to inlet maintenance.
Think about using different solvents for extraction. Use the extraction to help define the products....
Best regards.