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Thu, 16 Feb 2006 17:27:46 -0500 |
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Hello Isotopers,
We've been attempting to use our Gas Bench to do hydrogen analysis of
waters using platinum catalysts and headspace equilibration at about
32degreesC. When we started, we got acceptable numbers with good within
analysis (10 peaks) standard deviations. Values plotted sensibly along (or
very near) the meteoric water line. As time went on, our standard
deviations have gotten much worse (as much as 7 permil) and our data very
seldom plot reasonably close to the meteoric water line. Often, hydrogen
data plot well above the meteoric water line. We have gotten great results
from oxygen analyses of the same samples.
We've just spent a great deal of time and effort to ensure that our sample
gas is totally dry before it enters the mass spectrometer. I also let the
catalysts sit in our oven (60degreesC) for two days before placing them
into the vials with our water samples. We got better standard deviations
for our analyses this time (between 2 and 3), but still have unreasonable
scatter around the meteoric water line.
Questions:
1) What is a generally acceptable standard deviation for d2H from water?
2) Could the problem be with our catalysts? I thought that, by definition,
catalysts were reusable .. but maybe not. We've only done about 5 analyses
with each catalyst.
3) Are we going to have this same problem when we start running waters
using our TC/EA instead? or are we going to be happy that we made the change?
If anyone out there in cyberspace has dealt with and corrected this
problem, we would love to hear from you!
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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