Subject: | |
From: | |
Reply To: | |
Date: | Fri, 21 Apr 2006 09:25:38 -0700 |
Content-Type: | text/plain |
Parts/Attachments: |
|
|
Hello Everyone,
I have a rather interesting/annoying problem with
my Isoprime-Multicarb system. Essentially,
during a run no gas is getting from the reaction
vial to the first coldfinger (CF2). At first we
thought it was a problem with CF2 (e.g., either
it was plugged or not cooling properly) but the
problem still persisted after changing to a new
coldfinger. If we simply inject CO2 into the
vial (bypassing the calcite-phosphoric acid
reaction) we are able to get CO2 from the vial to
CF2 and trap it correctly. However, this works
only if we are using a lot of CO2 gas. If we use
only a small amount (as if we reacted 100 ug
calcite) it does not work. I have confirmed that
CO2 gas is being produced (i.e., no problem with
the addition of acid to the vial). So
essentially, it appears that CF2 does not have
the ability to "pull" the CO2 from the reaction
vial or the CO2 gas is being trapped / lost
somewhere along the way. I have considered the
possibility that the water trap is too cold (and
that the thermocouple is reading incorrectly) and
will check this today.
Here are a few more details. I've checked the
system for leaks with Argon and everything looks
OK. The needle and stainless steel tubing
leading from the needle to the inlet system are
not plugged with acid (...those of you with the
multicarb know this is a common problem). We
have confirmed that the heated rack is at about
90°C. We are using a new batch of acid, but it
worked fine for a few runs so I don't think this
is the problem. We also have the re-designed
multicarb needle, but again we used this for a
few runs without problem.
Any suggestions would be greatly appreciated.
Jennifer
--
Post-doctoral Researcher
Centre GEOTOP, Universite du Quebec a Montreal
C.P. 8888, succursale Centre-Ville
Montreal, Quebec, Canada
H3C 3P8
GEOTOP: 514-987-4080
Office: 514-987-3000 (1718)
Lab: 514-987-3000 (7028)
Fax: 514-987-3635
E-mail: [log in to unmask] (or [log in to unmask])
|
|
|