The DOI matches its Crossref record; 7 of the 7 references it cites were found in a registry or an index.
Measurement of sample temperatures under magic-angle spinning from the chemical shift and spin-lattice relaxation rate of 79Br in KBr powder
Open accessAbstract
Accurate determination of sample temperatures in solid state nuclear magnetic resonance (NMR) with magic-angle spinning (MAS) can be problematic, particularly because frictional heating and heating by radio-frequency irradiation can make the internal sample temperature significantly different from the temperature outside the MAS rotor. This paper demonstrates the use of 79Br chemical shifts and spin-lattice relaxation rates in KBr powder as temperature-dependent parameters for the determination of internal sample temperatures. Advantages of this method include high signal-to-noise, proximity of the 79Br NMR frequency to that of 13C, applicability from 20 K to 320 K or higher, and simultaneity with adjustment of the MAS axis direction. We show that spin-lattice relaxation in KBr is driven by a quadrupolar mechanism. We demonstrate a simple approach to including KBr powder in hydrated samples, such as biological membrane samples, hydrated amyloid fibrils, and hydrated microcrystalline proteins, that allows direct assessment of the effects of frictional and radio-frequency heating under experimentally relevant conditions.
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Cites
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Self-citationAdiabatic Rotational Splittings and Berry's Phase in Nuclear Quadrupole Resonance
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Sauvée, C., Rosay, M., Casano, G., Aussenac, F., Weber, R. T., Ouari, O., & Tordo, P. (2013) · Angewandte Chemie International Edition · doi:10.1002/anie.201304657 · Cited by 503
Sensitivity-enhanced solid-state NMR detection of expansin’s target in plant cell walls
Wang, T., Park, Y. B., Caporini, M. A., Rosay, M., Zhong, L., Cosgrove, D. J., & Hong, M. (2013) · Proceedings of the National Academy of Sciences · doi:10.1073/pnas.1316290110 · Cited by 234
Li, M., Mandal, A., Tyurin, V. A., DeLucia, M., Ahn, J., Kagan, V. E., & van der Wel, P. C. A. (2019) · Structure · doi:10.1016/j.str.2019.02.007 · Cited by 41
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Metadata
- Authors
- Thurber, K. R., & Tycko, R.
- Venue
- Journal of Magnetic Resonance
- Publisher
- Elsevier BV
- Published
- 2009-01
- Volume
- 196
- Issue
- 1
- Pages
- 84-87
- ISSN
- 1090-7807 (ISSN-L)
- OpenAlex
- W2073471770
- Cited by
- 323
- References
- 7
- FWCI
- 1.63
- Type
- journal article
- Language
- en
- Open access
- green
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- Thurber, K. R., & Tycko, R. (2009). Measurement of sample temperatures under magic-angle spinning from the chemical shift and spin-lattice relaxation rate of 79Br in KBr powder. Journal of Magnetic Resonance. https://doi.org/10.1016/j.jmr.2008.09.019
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