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Date: | Mon, 6 Mar 2006 08:36:09 -0800 |
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We recently overcame a high mass 46 background on a Delta Plus. After moving the GP interface we apparently jostled it enough to loosen the bottom of the open split. After leak checking with Argon, we isolated the leak, applied Polyimide resin. Fixed. Good luck.
andy
Andrew Schauer
Stable Isotope Facility for Environmental Research
Department of Biology
University of Utah
257 S. 1400 E.
Salt Lake City, UT 84112 USA
----- Original Message ----
From: Penny Higgins <[log in to unmask]>
To: [log in to unmask]
Sent: Monday, March 6, 2006 7:57:19 AM
Subject: [ISOGEOCHEM] High Mass 46 background
Hi all,
We've been running carbonates (CO2) on our Delta Plus XL, via the Gasbench
and PAL, for nearly a year now. Everything has been running smoothly.
Alas, in the past few weeks I've noticed that the mass 46 background has
increased dramatically from 10-20mV to nearly 50mV (sometimes more). Our
standard deviation on d18O (based on ten peaks) has increased to 0.15 or
much higher. Carbon is still running very well, and I am certain that water
in the sample is not getting to the mass spectrometer source. We check
linearity every day before running analyses, so I know that the instrument
is performing magnificently and is linear. The mass 46 background on the
reference peaks is generally much lower than that of the sample peaks,
though these days still tops 20mV.
Does anyone know where the excess mass 46 is coming from. There appears to
still be a clear separation between the nitrogen peak and the carbon
dioxide peak coming out of the GC column. However, I wonder if the GC
column may yet be bad. We did once draw phosphoric acid into the GasBench
(a procedural problem we have since fixed). I wonder if this may have
damaged the GC column?
Any other thoughts?
Thanks,
~Penny
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Dr. Pennilyn Higgins
Research Associate
"SIREAL"
Stable Isotope Ratios in the Environment Analytical Laboratory
Department of Earth and Environmental Sciences
University of Rochester
227 Hutchison Hall
Rochester, NY 14627
[log in to unmask]
Office: 209b Hutchison Hall Lab: 209 Hutchison Hall
Voice : (585) 275-0601 Outer lab: (585) 273-1405
FAX : (585) 244-5689 Inner lab: (585) 273-1397
http://www.earth.rochester.edu/SIREAL/index.html
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