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Thermometers for low temperature Magic Angle Spinning NMR

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Kemp, Thomas F., Balakrishnan, Geetha, Pike, Kevin J., Smith, Mark E. and Dupree, Ray. (2010) Thermometers for low temperature Magic Angle Spinning NMR. Journal of Magnetic Resonance, Vol.204 (No.1). pp. 169-172. ISSN 1090-7807

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Official URL: http://dx.doi.org/10.1016/j.jmr.2010.02.018

Abstract

The measurement of temperature in a Magic Angle Spinning NMR probe in the temperature range 85-300 K is discussed. It is shown that the shift of the Sn-119 resonance of Sm2Sn2O7 makes a good thermometer with shift being given by delta = 223 - 9.54 x 10(4)/T ppm and a potential precision of better than 0.5 K over the entire temperature range. The sensitivity is such (e.g. 4.2 ppm/K at 150 K) that small temperature gradients across the sample can readily be measured. Furthermore, since the spin-lattice relaxation time is very short, measurements can be made in similar to 1 s enabling relatively rapid temperature changes to be followed. Values for the chemical shift of Pb-207 in Pb(NO3)(2) down to similar to 85 K are also presented. Although the Pb-207 shift variation is approximately linear near room temperature (we find a slope 0.725 +/- 0.002 ppm/K over the range 293-153 K), it clearly deviates from linearity below similar to 130 K.

Item Type: Journal Article
Subjects: Q Science > QC Physics
Divisions: Administration > Vice Chancellor's Office
Faculty of Science > Physics
Library of Congress Subject Headings (LCSH): Nuclear magnetic resonance spectroscopy -- Methodology, Temperature measuring instruments
Journal or Publication Title: Journal of Magnetic Resonance
Publisher: Academic Press
ISSN: 1090-7807
Date: May 2010
Volume: Vol.204
Number: No.1
Number of Pages: 4
Page Range: pp. 169-172
Identification Number: 10.1016/j.jmr.2010.02.018
Status: Peer Reviewed
Publication Status: Published
Access rights to Published version: Restricted or Subscription Access
Funder: Engineering and Physical Sciences Research Council (EPSRC)
Grant number: EP/D045967 (EPSRC)
References: [1] A. Bielecki, D.P. Burum, Temperature dependence of 207Pb MAS spectra of solid lead nitrate: an accurate, sensitive thermometer for variable-temperature MAS, J. Magn. Reson. 116 (A) (1995) 215–220. [2] L.C.M. Van Gorkom, J.M. Hook, M.B. Logan, J.V. Hanna, R.E. Wasylishen, Solidstate lead-207 NMR of lead(II) nitrate: localized heating effects at high magic angle spinning speeds, Magn. Reson. Chem. 33 (1995) 791–795. [3] D.B. Ferguson, J.F. Haw, Transient methods for in situ NMR of reactions on solid catalysts using temperature jumps, Anal. Chem. 67 (1995) 3342–3348. [4] T. Takahashi, H. Kwashima, H. Sugisawa, T. Baba, 207Pb chemical shift thermometer at high temperature for magic angle spinning experiments, Solid State Nucl. Magn. Reson. 15 (1999) 119–123. [5] K.R. Thurber, R. Tycko, Measurement of sample temperatures under magicangle spinning from the chemical shift and spin-lattice relaxation rate of 79Br in KBr powder, J. Magn. Reson. 196 (2009) 84–87. [6] C.P. Grey, A.K. Cheetham, C.M. Dobson, Temperature-dependent solid-state 119Sn-MAS NMR of Nd2Sn2O7, Sm2Sn2O7, and Y1.8Sm0.2Sn2O7. Three sensitive chemical-shift thermometers, J. Magn. Reson. 101 (1993) 299–306. [7] C. Dybowski, G. Neue, Solid state 207Pb NMR spectroscopy, Prog. NMR Spectrosc. 41 (2002) 153–170. [8] O. Dmitrenko, S. Bai, P.A. Beckmann, S. van Bramer, A.J. Vega, C. Dybowski, The relationship between 207Pb NMR chemical shift and solid-state structure in Pb(II) compounds, J. Phys. Chem. A 112 (2008) 3046–3052. [9] M. Concistre, A. Gansmuller, N. McLean, O.G. Johannessen, I.M. Montesinos, P.H.M. Bovee-Geurts, P. Verdegem, J. Lugtenburg, R.C.D. Brown, W.J. DeGrip, M.H. Levitt, Double-quantum 13C nuclear magnetic resonance of bathorhodopsin, the first photointermediate in mammalian vision, J. Am. Chem. Soc. 130 (2008) 10490–10491 (Supplementary information).
URI: http://wrap.warwick.ac.uk/id/eprint/6074

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