Abstract
Analyses of the layer structure of Na-montmorillonite have been performed using 27Al MAS and 27Al MQMAS NMR techniques. Results of 27Al MAS NMR measurements at higher magnetic field strength (16.4 T) suggest that the 4-coordinated Al site in Na-montmorillonite has two different structures. This was confirmed by the fact that two peaks corresponding to 4-coordinated Al are observed in the 27Al MQMAS NMR at high magnetic field strength. The ratio of two 4-coordinated Al sites was found to be affected by water in the interlayer space because the area ratio of cross peaks corresponding to two 4-coordinated Al sites changes with the water content.
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Amoureux, J.P. (1993) High-resolution solid-state NMR for spin 3/2 and 9/2: the multi-quantum transitions method. Solid State Nuclear Magnetic Resonance, 2, 83–88.
Amoureux, J.P. and Fernandez, C. (1998) Triple, quintuple and higher order multiple quantum MAS NMR of quadrupolar nuclei. Solid State Nuclear Magnetic Resonance, 10, 212–223.
Amoureux, J.P., Fernandez, C. and Steuernagel, S. (1996) Z filtering in MQMAS NMR. Journal of Magnetic Resonance, A123, 116–118.
Behrens, H.J. and Schnabel, B. (1982) The second order influence of the nuclear quadrupole interaction on the central line in the NMR of quadrupolar nuclei using rapid sample spinning. Physica B, 114, 185–190.
Bharadwaj, R.K., Mehrabi, A.R., Hamilton, C., Trujillo, C., Murga, M., Fan, R., Chavira, A. and Thompson, A.K. (2002) Structure-property relationships in cross-linked polyesterclay nanocomposites. Polymer, 43, 3699–3705.
Campanati, M., Casagrande, M., Fagiolino, I., Lenarda, M., Storaro, L., Battagliarin, M. and Vaccari, A. (2002) Mild hydrogenation of quinoline 2. A novel Rh-containing pillared layered clay catalyst. Journal of Molecular Catalysis A: Chemical, 184, 267–272.
Drachman, S.R., Roch, G.E. and Smith, M.E. (1997) Solid state NMR characterization of the thermal transformation of Fuller’s Earth. Solid State Nuclear Magnetic Resonance, 9, 257–267.
Fernandez, C. and Amoureux, J.P. (1995) 2D multiquantum MAS-NMR spectroscopy of 27Al in aluminophosphate molecular sieves. Chemical Physics Letters, 242, 449–454.
Ferris, J.P. and Ertem, G. (1993) Montmorillonite catalysis of RNA oligomer formation in aqueous solution. A model for the prebiotic formation of RNA. Journal of American Chemical Society, 115, 12270–12275.
Frydman, L. and Harwood, J.S. (1995) Isotropic spectra of half-integer quadrupolar spins from bidimensional magic-angle-spinning NMR. Journal of American Chemical Society, 117, 5367–5368.
Fukushima, Y. (1984) X-ray diffraction study of aqueous montmorillonite emulsions. Clays and Clay Minerals, 32, 320–326.
Hannus, I., Pálinkó, I., Lázaár, K., Nagy, J.B. and Kiricsi, I. (1995) The chemical state of Sn in Sn-montmorillonite; A multinuclear MAS NMR and 119Sn Mössbauer spectroscopic study. Journal of Molecular Structure, 349, 179–182.
Hawkins, R.K. and Egelstaff, P.A. (1980) Interfacial water structure in montmorillonite from neutron diffraction experiments. Clays and Clay Minerals, 28, 19–28.
Janes, N. and Oldfield, E. (1985) Prediction of silicon-29 nuclear magnetic resonance chemical shifts using a group electronegativity approach: applications to silicate and aluminosilicate structures. Journal of American Chemical Society, 107, 6769–6775.
Kanehashi, K. and Saito, K. (2002) Structural analysis of boron compounds using 11B-3QMAS solid state NMR. Journal of Molecular Structure, 602, 105–113.
Kanehashi, K., Saito, K. and Sugisawa, H. (2000) Structural analysis of boron carbide using 2D 11B-MQMAS NMR. Chemistry Letters, 588–589.
Khan, M.M.T., Samad, S.A., Siddiqui, M.R.H., Bajaj, H.C. and Ramachandraiah, G. (1991) Formation of a rhodium(II) monohydrido complex derived from Wilkinson’s complex RhCl(PPh3)3 in the interlamellar spaces of montmorillonite and catalytic hydrogenation of cyclohexene. Polyhedron, 10, 2729–2736.
Kundla, E., Samoson, A. and Lippmaa, E. (1981) Highresolution NMR of quadrupolar nuclei in rotating solids. Chemical Physics Letters, 83, 229–232.
Lippmaa, E., Mägi, M., Samson, A., Engelhardt, G. and Grimmer, A.R. (1980) Structural studies of silicates by solid-state high-resolution 29Si NMR. Journal of American Chemical Society, 102, 4889–4893.
Massiot, D., Touzo, B., Trumeau, D., Coutures, J.P., Virlet, J., Florian, P. and Grandinetti, P.J. (1996) Two-dimensional magic-angle spinning isotropic reconstruction sequences for quadrupolar nuclei. Solid State Nuclear Magnetic Resonance, 6, 73–83.
Mastalir, Á., Király, Z., Szörgy, G. and Bartók, M. (2001) Stereoselective hydrogenation of 1-phenyl-1-pentyne over low-loaded Pd-montmorillonite catalysts. Applied Catalysis A: General, 213, 133–140.
Mooney, R.W., Keenan, A.G. and Wood, L.A. (1952) Adsorption of water vapor by montmorillonite. II. Effect of exchangeable ions and lattice swelling as measured by X-ray diffraction. Journal of American Chemical Society, 74, 1371–1374.
Muller, D., Gessner, W., Behrens, H.J. and Scheler, G. (1981) Determination of the aluminium coordination in aluminium-oxygen compounds by solid-state high-resolution 27Al NMR. Chemical Physics Letters, 79, 59–62.
Rocha, J. (1999) Single- and triple-quantum 27Al MAS NMR study of the thermal transformation of kaolinite. Journal of Physical Chemistry B, 103, 9801–9804.
Saito, K., Kanehashi, K. and Komaki, I. (2001) Applications of NMR techniques to coal science. Annual reports on NMR Spectroscopy, 44, 23–72.
Staunton, S. and Quiquampoix, H. (1994) Adsorption and conformation of bovine serum albumin on montmorillonite: modification of the balance between hydrophobic and electrostatic interactions by protein methylation and pH variation. Journal of Colloid and Interface Science, 166, 89–94.
Stebbins, J.F., Zhao, P., Lee, S.K. and Oglesby, J.V. (2001) Direct observation of multiple oxygen sites in oxide glasses: recent advances from triple-quantum magic-angle spinning nuclear magnetic resonance. Journal of Non-Crystalline Solids, 293, 67–73.
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Ohkubo, T., Kanehashi, K., Saito, K. et al. Observation of Two 4-Coordinated Al Sites in Montmorillonite using High Magnetic Field Strength 27Al MQMAS NMR. Clays Clay Miner. 51, 513–518 (2003). https://doi.org/10.1346/CCMN.2003.0510505
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DOI: https://doi.org/10.1346/CCMN.2003.0510505