Abstract
Solid-state NMR observations of low-gamma half-integer quadrupolar nuclei, 35Cl and 37Cl, were demonstrated using a 24 T hybrid magnet (1H resonance frequency of 1.02 GHz) comprised of the high-temperature (HTS) and low-temperature (LTS) superconductors, and compared with results using a 14.1 T standard NMR magnet. While at 24 T the linewidth is 1.7 times narrower than that at 14.1 T, the gain in the sensitivity is 7.0 times because of enhanced polarization, reduced linewidth, and the use of larger rotor. A simple theoretical model was used to rationalize the sensitivity enhancements. The ratio of 35Cl and 37Cl quadrupolar couplings agrees well with the ratio of quadrupolar moments, and no isotopedependent chemical shift has been observed. In addition, the 3QMAS spectrum of 35Cl is shown to demonstrate the high sensitivity rendered by the 24 T spectrometer.
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References
K. Schmidt-Rohr and H. W. Spiess, “Multidimensional Solid-state NMR and Polymers”, 1994, Academic Press, Berlin.
A. E. McDermott and T. Polenova, “Solid State NMR Studies of Biopolymers”, 2012, John Wiley & Sons.
M. Mehring, “High Resolution NMR Spectroscopy in Solids”, 1976, Springer-Verlag, Berlin.
R. Tycko, Annu. Rev. Phys. Chem., 2011, 62, 279.
M. Hong, Y. Zhang, and F. Hu, Annu. Rev. Phys. Chem., 2012, 63, 1.
A. Ramamoorthy (ed.), “NMR Spectroscopy of Biological Solids”, 2010, CRC Press.
M. E. Smith and E. R. H. van Eck, Prog. Nucl. Magn. Reson. Spec., 1999, 34, 159.
C. Fernandez and M. Pruski, Top. Curr. Chem., 2012, 306, 119.
S. E. Ashbrook, Phys. Chem. Chem. Phys., 2009, 11, 6892.
S. E. Ashbrook and S. Sneddon, J. Am. Chem. Soc., 2014, 136, 15440.
A. Samoson, E. Lippmaa, and A. Pines, Mol. Phys., 1988, 65, 1013.
E. W. Wooten, K. T. Mueller, and A. Pines, Acc. Chem. Res., 1992, 25, 209.
A. Llor and J. Virlet, Chem. Phys. Lett., 1988, 152, 248.
K. T. Mueller, B. Q. Sun, G. C. Chingas, J. W. Zwanziger, T. Terao, and A. Pines, J. Magn. Reson., 1990, 86, 470.
A. Medek, J. S. Harwood, and L. Frydman, J. Am. Chem. Soc., 1995, 117, 12779.
Z. Gan, P. Gor’kov, T. A. Cross, A. Samoson, and D. Massiot, J. Am. Chem. Soc., 2002, 124, 5634.
Y. Yanagisawa, H. Nakagome, K. Tennmei, M. Hamada, M. Yoshikawa, A. Otsuka, M. Hosono, T. Kiyoshi, M. Takahashi, T. Yamazaki, and H. Maeda, J. Magn. Reson., 2010, 203, 274.
K. Hashi, S. Ohki, S. Matsumoto, G. Nishijima, A. Goto, K. Deguchi, K. Yamada, T. Noguchi, S. Sakai, M. Takahashi, Y. Yanagisawa, S. Iguchi, T. Yamazaki, H. Maeda, R. Tanaka, T. Nemoto, H. Suematsu, T. Miki, K. Saito, and T. Shimizu, J. Magn. Reson., 2015, 256, 30.
D. L. Bryce and E. B. Bultz, Chem. Eur. J., 2007, 13, 4786.
C. M. Widdifield, R. P. Chapman, and D. L. Bryce, Ann. Rep. NMR Spec., 2009, 66, 195.
D. L. Bryce and G. D. Sward, Magn. Reson. Chem., 2006, 44, 409.
C. Gervais, R. Dupree, K. J. Pike, C. Bonhomme, M. Profeta, C. J. Pickard, and F. Mauri, J. Phys. Chem. A, 2005, 109, 6960.
D. L. Bryce, G. D. Sward, and S. Adiga, J. Am. Chem. Soc., 2006, 128, 2121.
D. L. Bryce, M. Gee, and R. E. Wasylishen, J. Phys. Chem. A, 2001, 105, 10413.
J. Viger-Gravel, S. Leclerc, I. Korobkov, and D. L. Bryce, J. Am. Chem. Soc., 2014, 136, 6929.
C. M. Widdifield and D. L. Bryce, Can. J. Chem., 2011, 89, 754.
D. L. Bryce and G. D. Sward, J. Phys. Chem. B, 2006, 110, 26461.
K. J. D. MacKenzie and M. E. Smith, “Multinuclear SolidState NMR of Inorganic Materials”, 2002, Pergamon.
A. Abragam, “The Principle of Nuclear Magnetism”, 1961, Clarendon Press, Oxford.
D. I. Hoult and R. E. Richards, J. Magn. Reson., 1976, 24, 71.
M. Bak, J. T. Rasmussen, and N. C. Nielsen, J. Magn. Reson., 2000, 147, 296.
R. P. Chapman and D. L. Bryce, Phys. Chem. Chem. Phys., 2007, 9, 6219.
E. A. C. Lucken, “Nuclear Quadrupole Coupling Constants”, 1969, Academic Press, London.
R. Zhang, M. K. Pandey, Y. Nishiyama, and A. Ramamoorthy, Sci. Rep., 2015, 5, 11810.
M. K. Pandey, R. Zhang, K. Hashi, S. Ohki, G. Nishijima, S. Matsumoto, T. Noguchi, K. Deguchi, A. Goto, T. Shimizu, H. Maeda, M. Takahashi, Y. Yanagisawa, T. Yamazaki, S. Iguchi, R. Tanaka, T. Nemoto, T. Miyamoto, H. Suematsu, K. Saito, T. Miki, A. Ramamoorthy, and Y. Nishiyama, J. Magn. Reson., 2015, 261, 1.
P. K. Madhu, A. Goldbourt, L. Frydman, and S. Vega, Chem. Phys. Lett., 1999, 307, 41.
S. P. Brown and S. Wimperis, J. Magn. Reson., 1997, 128, 42.
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This research was supported by the Japan Science and Technology Agency, JST, under the Strategic Promotion of Innovative Research and Development Program and under the Development of Systems and Technology for Advanced Measurement and Analysis.
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Pandey, M.K., Hashi, K., Ohki, S. et al. 24 T High-Resolution and -Sensitivity Solid-State NMR Measurements of Low-Gamma Half-Integer Quadrupolar Nuclei 35Cl and 37Cl. ANAL. SCI. 32, 1339–1345 (2016). https://doi.org/10.2116/analsci.32.1339
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DOI: https://doi.org/10.2116/analsci.32.1339