Thanks much for all the feedback about absolute shifts of TMS
with temperature, solvent, and/or concentration. I received
enough requests for a summary that I've decided to do a general
posting of the few papers we've found to be most useful.
Tom Stringfellow is the student, one of the best I've
ever worked with, and is doing some very precise work under the
direction of T. Farrar.
Jeff Walton, UC-Davis, sent a nice compliation (we haven't been
able to work through yet) of refs. for Xe which I'm sure he would
not mind my forwarding if you request (or you can ask him directly
at jhwalton@ucdavis.edu).
Please forgive us if we've missed something important:
1. M. R. Bacon and G. E. Maciel, J. Am. Chem. Soc. 95, 2413-
2426, 1973.
Authors extend the work of Becconsal, et al. [JACS 92, 430,
1970] to study the apparent and intrinsic solvent shifts of
1H, 13C, and 29Si of TMS and cyclohexane in 38 solvents (+
other work).
2. F. G. Morin, M. S. Solum, J. D. Withers, D. M. Grant and
D. K. Dalling, JMR 48, 138-142, 1982.
Authors investigated the 1H and 13C (TMS) chemical shift
and bulk susceptibility, temperature dependences. Results
show a 0.267 ppm shift in 1H chem.shift of TMS over the range
293-213 K, and for 13C TMS shifts of about 0.4 ppm.
3. C. J. Jameson, A. K. Jameson and S. N. Cohen, JMR 19, 385-392,
1975.
Authors determine temp dependence of chem shift for 6 reference
solvents (neat) using 129Xe resonance frequency. Data fit
to a quadratic dependence on temp for 1H in TMS over range
-53 to 27 C, showing ~ 0.3 ppm shift over that range.
4. P. Laszlo, Prog. Nucl. Magn. Reson. Spectro. 3, 231-402,
1967. "Solvent Effects and Nuclear Magnetic Resonance"
Extensive review article; includes a chapter about the
referencing (400+ references)
5. D. J. Frost and G. E. Hall, Mol. Phys. 10, 191-200, 1965.
Authors explained and compared spherical vs. cylindrical sample
tube for chem. shift reference in terms of magnetic susceptibility
and shape factor.
6. J. K. Becconsall, G. D. Daves, W. R. Anderson, Jr., JACS 92,
430-432, 1970.
Authors report a scheme for a "Reference Independent NMR Solvent
Shift."
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Charlie Fry TEL: 608-262-3182
Director, MR Facility FAX: 608-262-0381
Chem. Dept., Univ. Wisconsin
Madison, WI 53706 USA e-mail: fry@chem.wisc.edu
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