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htGC of fullerenes

Posted: Tue Feb 19, 2008 12:23 am
by GeoChris
Hi,

I tried to analyse a toluene extract of fullerene soot by high temperature GC-FID; unfortunately without success...

I used a 30m Inferno column (phase similar to DB-1) with He & ramped from 60 with 10/min to 200, then 5/min to 430 and held isotherm for 40 minutes. Inj. & FID were both at 400. Splitless Injection.

With similat T-programmes, others were able to detect n-alkanes up to I believe C100! A C60 fullerene should theoretically elute before nC60...

Does anyone have an idea what might be going wrong here?

Many thanks in advance,
Chris

Posted: Tue Feb 19, 2008 3:36 am
by chromatographer1
Do you know the temperature stability and reactivity of fullerenes?

I don't so I cannot help you answer the question but the answer to that question may be the answer to your question.

I hope that made sense. It is late tonight.

best wishes,

Rod

Posted: Tue Feb 19, 2008 4:01 am
by GeoChris
I know that they're fairly T stable. They're formed at high energies so I suppose that 430 C in a GC oven would not harm them.
I'm not fully sure about the reactivity, but they're basically a carbon ball, and their reactivity (on theoretical considerations) shouldn't be significantly higher than that of other higher-molecular weight PAH such as eg coronene, which GC very well...