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Vacuum Degasser contamination

Posted: Wed Apr 18, 2007 9:22 pm
by james little
We have a vacuum degasser which has become contaminated. Apparently it occured when we were doing a normal phase separation in Agilent 1100 system.

We were using a solvent mixture containing heptane and toluene. The toluene is showing up on every run of our system in the diode array trace (not in the LC-MS electrospray trace).

We took it apart and could smell the toluene and see the characteristic UV spectrum of toluene.

Anyone have any ideas how to clean up the degasser?

Not OK to run toluene as solvent in this type of system?

Thanks

Posted: Thu Apr 19, 2007 3:17 am
by tom jupille
The hollow fibers are (I think) fluorocarbon polymer; I wouldn't be surprised if toluene gets adsorbed/absorbed to some extent. If it were my problem, I'd replace either the entire degasser (or at least the fibers), and then try to clean up the old one "off-line" (maybe with warm air?). That way you'd be up and running quickly while you sorted out the fix at your leisure.

Posted: Thu Apr 19, 2007 8:03 am
by gcguy
You could try running neat IPA through the degasser at a low flow rate overnight and check the waste in the morning for toluene content.

Posted: Sat Apr 21, 2007 1:48 am
by james little
thanks for the suggestions, will try your suggestions.

Posted: Sat Apr 21, 2007 12:34 pm
by AA
The pumping IPA trick is a good thing to try, I would be more inclined to try the same technique, but with hexane or iso-octane, they should be able to get rid of the toluene, and any residue left from them is UV transparent.

Posted: Mon Apr 23, 2007 6:20 pm
by DR
Hexane soak, hexane rinse, then thorough MeOH flush. That's what I'd try.

Posted: Wed Apr 25, 2007 6:03 am
by Jackus
Hexane soak, hexane rinse, then thorough MeOH flush. That's what I'd try.
But methanol is not miscible with hexane.