Applied Magnetic Resonance

, Volume 47, Issue 11, pp 1193–1205 | Cite as

Random Distribution of EFG Parameters in 27Al MAS NMR Spectra of AlOx/SiO2 Catalysts and Related Systems

  • Aleksandr A. Shubin
  • Victor V. Terskikh
  • Evgeniy Papulovskiy
  • Olga B. Lapina
Original Paper

Abstract

27Al magic angle spinning (MAS) nuclear amgnetic resonance (NMR) spectroscopy is one of the primary tools in the structural characterization of a variety of alumina-based catalysts. However, the controversy still exists on the proper interpretation of 27Al NMR spectra due to difficulties associated with distribution of NMR parameters and by the experimental limitations. In this work, we present analysis of the 27Al MAS NMR spectra containing signals from Al(4), Al(5) and Al(6) species on the surface of AlOx/SiO2 catalysts and demonstrate several characteristic tell-tale properties of these signals caused by the random distribution of the EFG tensor parameters and by the partial excitation of NMR spectra.

Notes

Acknowledgments

Russian authors gratefully acknowledge the Russian Science Foundation (RSF Grant 14-23-00037) for the financial support. Dr. Z. Gan (NHMF, Florida) is thanked for his help with MQMAS experiments. Prof. I. Wachs is thanked for supplying the samples. Access to the 21.1 T NMR spectrometer was provided by the National Ultrahigh-Field NMR Facility for Solids (Ottawa, Canada), a national research facility funded by a consortium of Canadian Universities, supported by the National Research Council Canada and Bruker BioSpin, and managed by the University of Ottawa (http://nmr900.ca).

Supplementary material

723_2016_837_MOESM1_ESM.pdf (1.2 mb)
Supplementary material 1 (PDF 1266 kb)

References

  1. 1.
    A.P.M. Kentgens, Geoderma 80, 271 (1997)CrossRefGoogle Scholar
  2. 2.
    M.E. Smith, E.R.H. van Eck, Prog. Nucl. Magn. Reson. Spectrosc. 34, 159 (1999)CrossRefGoogle Scholar
  3. 3.
    P.P. Man, in Encyclopedia of Analytical Chemistry, ed. by R.A. Meyers (Wiley, Chichester, 2006)Google Scholar
  4. 4.
    J.W. Hennel, J. Klinowski, in Topics in Current Chemistry. New Tech. Solid-State NMR, vol. 246, ed. by J. Klinowski (Springer, Berlin, Heidelberg, 2005), pp. 1–14CrossRefGoogle Scholar
  5. 5.
    C. Fernandez, M. Pruski, in Topics in Current Chemistry. Solid State NMR, vol 306, ed. by J.C.C. Chan (Springer, Berlin, Heidelberg, 2012), pp. 119–188Google Scholar
  6. 6.
    R.E. Wasylishen, S.E. Ashbrook, S. Wimperis (eds.), NMR of Quadrupolar Nuclei in Solid Materials (Wiley, The Atrium, Southern Gate, Chichester, 2012)Google Scholar
  7. 7.
    X. Gao, I.E. Wachs, J. Catal. 192, 18 (2000)CrossRefGoogle Scholar
  8. 8.
    Z. Gan, H.-T. Kwak, J. Magn. Reson. 168, 346 (2004)ADSCrossRefGoogle Scholar
  9. 9.
    J.P. Amoureux, L. Delevoye, S. Steuernagel, Z. Gan, S. Ganapathy, L. Montagne, J. Magn. Reson. 172, 268 (2005)ADSCrossRefGoogle Scholar
  10. 10.
    R. Hajjar, Y. Millot, P.P. Man, Prog. Nucl. Magn. Reson. Spectrosc. 57, 306 (2010)CrossRefGoogle Scholar
  11. 11.
    I. Hung, J. Trébosc, G.L. Hoatson, R.L. Vold, J.-P. Amoureux, Z. Gan, J. Magn. Reson. 201, 81 (2009)ADSCrossRefGoogle Scholar
  12. 12.
    A.A. Shubin, O.B. Lapina, G.M. Zhidomirov, in IX-Th Ampere Summer School Abstracts Novosibirsk, 2026 Sept (Novosibirsk, 1987), p. 103Google Scholar
  13. 13.
    G. Czjzek, J. Fink, F. Götz, H. Schmidt, J. Coey, J.-P. Rebouillat, A. Liénard, Phys. Rev. B 23, 2513 (1981)ADSCrossRefGoogle Scholar
  14. 14.
    G. Le Caër, R.A. Brand, J. Phys.: Condens. Matter 10, 10715 (1998)Google Scholar
  15. 15.
    J.-B. d’Espinose de Lacaillerie, C. Fretigny, D. Massiot, J. Magn. Reson. 192, 244 (2008)ADSCrossRefGoogle Scholar
  16. 16.
    G. Le Caër, B. Bureau, D. Massiot, J. Phys.: Condens. Matter 22, 065402 (2010)ADSGoogle Scholar
  17. 17.
    F. Vasconcelos, S. Cristol, J.-F. Paul, L. Delevoye, F. Mauri, T. Charpentier, G. Le Caër, J. Phys.: Condens. Matter 25, 255402 (2013)ADSGoogle Scholar
  18. 18.
    A. Samoson, Chem. Phys. Lett. 119, 29 (1985)ADSCrossRefGoogle Scholar
  19. 19.
    P.P. Man, Phys. Rev. B 55, 8406 (1997)ADSCrossRefGoogle Scholar
  20. 20.
    K.J.D. MacKenzie, M.E. Smith, Multinuclear Solid-State Nuclear Magnetic Resonance of Inorganic Materials, Pergamon Materials Series, vol. 6 (Pergamon/Elsevier, Oxford, 2002)Google Scholar
  21. 21.
    R. Wischert, P. Florian, C. Copéret, D. Massiot, P. Sautet, J. Phys. Chem. C 118, 15292 (2014)CrossRefGoogle Scholar
  22. 22.
    Y. Ledemi, B. Bureau, G. Le Caër, L. Calvez, C. Roiland, G. Tricot, P. Florian, V. Nazabal, D. Massiot, J. Non. Cryst. Solids 383, 216 (2014)ADSCrossRefGoogle Scholar
  23. 23.
    A. Medek, J.S. Harwood, L. Frydman, J. Am. Chem. Soc. 117, 12779 (1995)CrossRefGoogle Scholar
  24. 24.
    J.-P. Amoureux, C. Fernandez, L. Frydman, Chem. Phys. Lett. 259, 347 (1996)ADSCrossRefGoogle Scholar
  25. 25.
    J. Jiao, J. Kanellopoulos, W. Wang, S.S. Ray, H. Foerster, D. Freude, M. Hunger, Phys. Chem. Chem. Phys. 7, 3221 (2005)CrossRefGoogle Scholar
  26. 26.
    X. Pardal, F. Brunet, T. Charpentier, I. Pochard, A. Nonat, Inorg. Chem. 51, 1827 (2012)CrossRefGoogle Scholar
  27. 27.
    A. Lesage, M. Lelli, D. Gajan, M.A. Caporini, V. Vitzthum, P. Miéville, J. Alauzun, A. Roussey, C. Thieuleux, A. Mehdi, G. Bodenhausen, C. Coperet, L. Emsley, J. Am. Chem. Soc. 132, 15459 (2010)CrossRefGoogle Scholar
  28. 28.
    A.J. Rossini, A. Zagdoun, M. Lelli, A. Lesage, C. Copéret, L. Emsley, Acc. Chem. Res. 46, 1942 (2013)CrossRefGoogle Scholar
  29. 29.
    M. Valla, A.J. Rossini, M. Caillot, C. Chizallet, P. Raybaud, M. Digne, A. Chaumonnot, A. Lesage, L. Emsley, J.A. van Bokhoven, C. Copéret, J. Am. Chem. Soc. 137, 10710 (2015)CrossRefGoogle Scholar
  30. 30.
    A.L. Blumenfeld, J.J. Fripiat, Top. Catal. 4, 119 (1997)CrossRefGoogle Scholar
  31. 31.
    M. Baca, E. de la Rochefoucauld, E. Ambroise, J.-M. Krafft, R. Hajjar, P.P. Man, X. Carrier, J. Blanchard, Microporous Mesoporous Mater. 110, 232 (2008)CrossRefGoogle Scholar
  32. 32.
    D. Iuga, S. Simon, E. de Boer, A.P.M. Kentgens, J. Phys. Chem. B 103, 7591 (1999)CrossRefGoogle Scholar

Copyright information

© Springer-Verlag Wien 2016

Authors and Affiliations

  1. 1.Boreskov Institute of CatalysisNovosibirskRussia
  2. 2.Novosibirsk State UniversityNovosibirskRussia
  3. 3.Department of ChemistryUniversity of OttawaOttawaCanada

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