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Dear Cap,
As you rightly suspect, the purification of samples like these is a
rather messy and frustrating business. Depending on the flow
parameters I would even suspect some CO2 to be trapped together
with the water in your proposed -90 C cold trap. CO2 quite happily
"dissolves" in water, the more so the lower the temperature.
I don't know what your instrument setup is, so my suggestion has to
be taken with a pich of salt. If you can hook up a GC to your IRMS,
no problem. If not, a little improvisation might be needed.
I wonder if you could condense all volatiles into a liquid N2 cold
trap and transfer (after flash heating) the condensables with a He
stream of 3 ml/min into a PoraPLOT Q GC column. Under isothermal
conditions, e.g. 50 C, you should be able to separate the CO2 as a
nice concentrated peak from all the other junk and "heart-cut" this
peak into your system.
I envisage a setup that purges He through your sample in flask A and
condenses the purged compounds in a coiled cold trap B which can be
resistance heated (SGE makes very nice glass lines SS tubing which is
well suited for such a purpose). A short transfer line connects the
cold trap with the PoraPLOT Q column which can be placed e.g. in a
thermostatic water bath if you are short one GC. The connection of
the column to your IRMS must allow to heart-cut the desired CO2 peak
whilst flushing all the undesirables to atmosphere.
Hope, you don't find this approach not to far-fetched.
Good luck.
Wolfram
*****************************
Dr. W. Meier-Augenstein
Hon. Lecturer in Chemistry
University of Dundee
Dept. of Anatomy & Physiology
Small's Wynd
DUNDEE DD1 4HN
United Kingdom
Tel.: +44-(0)1382-34/5124, /4968
+44-(0)468 -314563
Fax: +44-(0)1382-34/5514
e-mail: [log in to unmask]
URL: http://www.dundee.ac.uk/AnatPhys/wolfram.htm
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