Skip to main content
Log in

Observation of Two 4-Coordinated Al Sites in Montmorillonite using High Magnetic Field Strength 27Al MQMAS NMR

  • Published:
Clays and Clay Minerals

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.

This is a preview of subscription content, log in via an institution to check access.

Access this article

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Similar content being viewed by others

References

  • 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.

    Article  Google Scholar 

  • 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.

    Article  Google Scholar 

  • Amoureux, J.P., Fernandez, C. and Steuernagel, S. (1996) Z filtering in MQMAS NMR. Journal of Magnetic Resonance, A123, 116–118.

    Article  Google Scholar 

  • 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.

    Article  Google Scholar 

  • 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.

    Article  Google Scholar 

  • 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.

    Article  Google Scholar 

  • 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.

    Article  Google Scholar 

  • Fernandez, C. and Amoureux, J.P. (1995) 2D multiquantum MAS-NMR spectroscopy of 27Al in aluminophosphate molecular sieves. Chemical Physics Letters, 242, 449–454.

    Article  Google Scholar 

  • 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.

    Article  Google Scholar 

  • 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.

    Article  Google Scholar 

  • Fukushima, Y. (1984) X-ray diffraction study of aqueous montmorillonite emulsions. Clays and Clay Minerals, 32, 320–326.

    Article  Google Scholar 

  • 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.

    Article  Google Scholar 

  • Hawkins, R.K. and Egelstaff, P.A. (1980) Interfacial water structure in montmorillonite from neutron diffraction experiments. Clays and Clay Minerals, 28, 19–28.

    Article  Google Scholar 

  • 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.

    Article  Google Scholar 

  • Kanehashi, K. and Saito, K. (2002) Structural analysis of boron compounds using 11B-3QMAS solid state NMR. Journal of Molecular Structure, 602, 105–113.

    Article  Google Scholar 

  • Kanehashi, K., Saito, K. and Sugisawa, H. (2000) Structural analysis of boron carbide using 2D 11B-MQMAS NMR. Chemistry Letters, 588–589.

    Google Scholar 

  • 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.

    Article  Google Scholar 

  • Kundla, E., Samoson, A. and Lippmaa, E. (1981) Highresolution NMR of quadrupolar nuclei in rotating solids. Chemical Physics Letters, 83, 229–232.

    Article  Google Scholar 

  • 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.

    Article  Google Scholar 

  • 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.

    Article  Google Scholar 

  • 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.

    Article  Google Scholar 

  • 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.

    Article  Google Scholar 

  • 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.

    Article  Google Scholar 

  • 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.

    Article  Google Scholar 

  • Saito, K., Kanehashi, K. and Komaki, I. (2001) Applications of NMR techniques to coal science. Annual reports on NMR Spectroscopy, 44, 23–72.

    Article  Google Scholar 

  • 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.

    Article  Google Scholar 

  • 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.

    Article  Google Scholar 

Download references

Author information

Authors and Affiliations

Authors

Corresponding author

Correspondence to Yasuhisa Ikeda.

Rights and permissions

Reprints and permissions

About this article

Cite this article

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

Download citation

  • Received:

  • Revised:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1346/CCMN.2003.0510505

Key Words

Navigation