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Volume 62, Issue 3
  • ISSN: 2056-5135
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  • oa Dynamic Nuclear Polarisation Enhanced Solid-State Nuclear Magnetic Resonance Studies of Surface Modification of γ-Alumina

    Enhanced solid-state NMR technique significantly reduces experiment time for surface studies

  • Authors: Marco Mais1, Subhradip Paul2, Nathan S. Barrow3 and Jeremy J. Titman1
  • Affiliations: 1 School of Chemistry, University of NottinghamNottingham, NG7 2RDUK 2 Nottingham DNP MAS NMR Facility, Sir Peter Mansfield Imaging Centre, University of NottinghamNG7 2RDUK 3 Johnson MattheyBlounts Court, Sonning Common, Reading, RG4 9NHUK
  • Source: Johnson Matthey Technology Review, Volume 62, Issue 3, Jul 2018, p. 271 - 278
  • DOI: https://doi.org/10.1595/205651318X696765
    • Published online: 01 Jan 2018

Abstract

Dynamic nuclear polarisation (DNP) gives large (>100-fold) signal enhancements in solid-state nuclear magnetic resonance (solid-state NMR) spectra the transfer of spin polarisation from unpaired electrons from radicals implanted in the sample. This means that the detailed information about local molecular environment available for bulk samples from solid-state NMR spectroscopy can now be obtained for dilute species, such as sites on the surfaces of catalysts and catalyst supports. In this paper we describe a DNP-enhanced solid-state NMR study of the widely used catalyst γ-alumina which is often modified at the surface by the incorporation of alkaline earth oxides in order to control the availability of catalytically active penta-coordinate surface Al sites. DNP-enhanced 27Al solid-state NMR allows surface sites in γ-alumina to be observed and their 27Al NMR parameters measured. In addition changes in the availability of different surface sites can be detected after incorporation of barium oxide.

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2018-01-01
2024-12-22
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References

  1. Q. Z. Ni, E. Daviso, T. V. Can, E. Markhasin, S. K. Jawla, T. M. Swager, R. J. Temkin, J. Herzfeld, R. G. Griffin, Acc. Chem. Res., 2013, 46, (9), 1933 LINK https://doi.org/10.1021/ar300348n [Google Scholar]
  2. A. J. Rossini, A. Zagdoun, M. Lelli, A. Lesage, C. Copéret, L. Emsley, Acc. Chem. Res., 2013, 46, (9), 1942 LINK https://doi.org/10.1021/ar300322x [Google Scholar]
  3. T. V. Can, Q. Z. Ni, R. G. Griffin, J. Magn. Reson., 2015, 253, 23 LINK https://doi.org/10.1016/j.jmr.2015.02.005 [Google Scholar]
  4. D. Lee, S. Hediger, G. De Paëpe, Solid State Nucl. Magn. Reson., 2015, 66–67, 6 LINK https://doi.org/10.1016/j.ssnmr.2015.01.003 [Google Scholar]
  5. R. I. Hunter, P. A. S. Cruickshank, D. R. Bolton, P. C. Riedi, G. M. Smith, Phys. Chem. Chem. Phys., 2010, 12, (22), 5752 LINK https://doi.org/10.1039/C002251A [Google Scholar]
  6. T. F. Kemp, H. R. W. Dannatt, N. S. Barrow, A. Watts, S. P. Brown, M. E. Newton, R. Dupree, J. Magn. Reson., 2016, 265, 77 LINK https://doi.org/10.1016/j.jmr.2016.01.021 [Google Scholar]
  7. M. Rosay, L. Tometich, S. Pawsey, R. Bader, R. Schauwecker, M. Blank, P. M. Borchard, S. R. Cauffman, K. L. Felch, R. T. Weber, R. J. Temkin, R. G. Griffin, W. E. Maas, Phys. Chem. Chem. Phys., 2010, 12, (22), 5850 LINK https://doi.org/10.1039/C003685B [Google Scholar]
  8. W. R. Grüning, A. J. Rossini, A. Zagdoun, D. Gajan, A. Lesage, L. Emsley, C. Copéret, Phys. Chem. Chem. Phys., 2013, 15, (32), 13270 LINK https://doi.org/10.1039/C3CP00026E [Google Scholar]
  9. R. L. Johnson, F. A. Perras, T. Kobayashi, T. J. Schwartz, J. A. Dumesic, B. H. Shanks, M. Pruski, Chem. Commun., 2016, 52, (9), 1859 LINK https://doi.org/10.1039/C5CC06788J [Google Scholar]
  10. F. A. Perras, U. Chaudhary, I. I. Slowing, M. Pruski, J. Phys. Chem. C, 2016, 120, (21), 11535 LINK https://doi.org/10.1021/acs.jpcc.6b02579 [Google Scholar]
  11. T. Kobayashi, F. A. Perras, U. Chaudhary, I. I. Slowing, W. Huang, A. D. Sadow, M. Pruski, Solid State Nucl. Magn. Reson., 2017, 87, 38 LINK https://doi.org/10.1016/j.ssnmr.2017.08.002 [Google Scholar]
  12. F. A. Perras, J. D. Padmos, R. L. Johnson, L.-L. Wang, T. J. Schwartz, T. Kobayashi, J. H. Horton, J. A. Dumesic, B. H. Shanks, D. D. Johnson, M. Pruski, J. Am. Chem. Soc., 2017, 139, (7), 2702 LINK https://doi.org/10.1021/jacs.6b11408 [Google Scholar]
  13. M. A. Hope, D. M. Halat, P. C. M. M. Magusin, S. Paul, L. Peng, C. P. Grey, Chem. Commun., 2017, 53, (13), 2142 LINK https://doi.org/10.1039/C6CC10145C [Google Scholar]
  14. G. Busca, ‘Structural, Surface, and Catalytic Properties of Aluminas’, in “Advances in Catalysis”, ed. F. C. Jentoft, 57, Elsevier Inc, San Diego, USA, 2014, pp. 319–404 [Google Scholar]
  15. N. S. Barrow, A. Scullard, N. Collis, Johnson Matthey Technol. Rev., 2016, 60, (2), 90 LINK https://www.technology.matthey.com/article/60/2/90-97/ [Google Scholar]
  16. M. Shelef, H. S. Gandhi, Platinum Metals Rev., 1974, 18, (1), 2 LINK https://www.technology.matthey.com/article/18/1/2-14/ [Google Scholar]
  17. M. Haouas, F. Taulelle, C. Martineau, Prog. Nucl. Magn. Reson. Spectrosc., 2016, 94–95, 11 LINK https://doi.org/10.1016/j.pnmrs.2016.01.003 [Google Scholar]
  18. H. D. Morris, P. D. Ellis, J. Am. Chem. Soc., 1989, 111, (16), 6045 LINK https://doi.org/10.1021/ja00198a012 [Google Scholar]
  19. D. Coster, A. L. Blumenfeld, J. J. Fripiat, J. Phys. Chem., 1994, 98, (24), 6201 LINK https://doi.org/10.1021/j100075a024 [Google Scholar]
  20. H. J. Kim, H. C. Lee, J. S. Lee, J. Phys. Chem. C, 2007, 111, (4), 1579 LINK https://doi.org/10.1021/jp0651945 [Google Scholar]
  21. D. Lee, N. T. Duong, O. Lafon, G. De Paëpe, J. Phys. Chem. C, 2014, 118, (43), 25065 LINK https://doi.org/10.1021/jp508009x [Google Scholar]
  22. J. H. Kwak, J. Z. Hu, D. H. Kim, J. Szanyi, C. H. F. Peden, J. Catal., 2007, 251, (1), 189 LINK https://doi.org/10.1016/j.jcat.2007.06.029 [Google Scholar]
  23. R. Wischert, P. Florian, C. Copéret, D. Massiot, P. Sautet, J. Phys. Chem. C, 2014, 118, (28), 15292 LINK https://doi.org/10.1021/jp503277m [Google Scholar]
  24. Y. Rozita, R. Brydson, T. P. Comyn, A. J. Scott, C. Hammond, A. Brown, S. Chauruka, A. Hassanpour, N. P. Young, A. I. Kirkland, H. Sawada, R. I. Smith, ChemCatChem, 2013, 5, (9), 2695 LINK https://doi.org/10.1002/cctc.201200880 [Google Scholar]
  25. V. Vitzthum, P. Miéville, D. Carnevale, M. A. Caporini, D. Gajan, C. Copéret, M. Lelli, A. Zagdoun, A. J. Rossini, A. Lesage, L. Emsley, G. Bodenhausen, Chem. Commun., 2012, 48, (14), 1988 LINK https://doi.org/10.1039/C2CC15905H [Google Scholar]
  26. A. Zagdoun, G. Casano, O. Ouari, M. Schwarzwälder, A. J. Rossini, F. Aussenac, M. Yulikov, G. Jeschke, C. Copéret, A. Lesage, P. Tordo, L. Emsley, J. Am. Chem. Soc., 2013, 135, (34), 12790 LINK https://doi.org/10.1021/ja405813t [Google Scholar]
  27. J.-B. d’Espinose de la Caillerie, C. Fretigny, D. Massiot, J. Magn. Reson., 2008, 192, (2), 244 LINK https://doi.org/10.1016/j.jmr.2008.03.001 [Google Scholar]
  28. H. Kraus, M. Müller, R. Prins, A. P. M. Kentgens, J. Phys. Chem. B, 1998, 102, (20), 3862 LINK https://doi.org/10.1021/jp972909i [Google Scholar]
  29. S. E. Ashbrook, S. Wimperis, J. Magn. Reson., 2000, 147, (2), 238 LINK https://doi.org/10.1006/jmre.2000.2174 [Google Scholar]
  30. G. Czjzek, J. Fink, F. Götz, H. Schmidt, J. M. D. Coey, J.-P. Rebouillat, A. Liénard, Phys. Rev. B, 1981, 23, (6), 2513 LINK https://doi.org/10.1103/PhysRevB.23.2513 [Google Scholar]
  31. G. Le Caër, R. A. Brand, J. Phys.: Condens. Matter, 1998, 10, (47), 10715 LINK https://doi.org/10.1088/0953-8984/10/47/020 [Google Scholar]
  32. D. Massiot, F. Fayon, M. Capron, I. King, S. Le Calvé, B. Alonso, J.-O. Durand, B. Bujoli, Z. Gan, G. Hoatson, Magn. Reson. Chem., 2002, 40, (1), 70 LINK https://doi.org/10.1002/mrc.984 [Google Scholar]
  33. J. H. Kwak, J. Hu, D. Mei, C.-W. Yi, D. H. Kim, C. H. F. Peden, L. F. Allard, J. Szanyi, Science, 2009, 325, (5948), 1670 LINK https://doi.org/10.1126/science.1176745 [Google Scholar]
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Dynamic Nuclear Polarisation Enhanced Solid-State Nuclear Magnetic Resonance Studies of Surface Modification of γ-Alumina
Johnson Matthey Technology Review 62, 271 (2018); https://doi.org/10.1595/205651318X696765
/content/journals/10.1595/205651318X696765
/content/journals/10.1595/205651318X696765
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