Hostname: page-component-78c5997874-xbtfd Total loading time: 0 Render date: 2024-11-10T11:58:08.216Z Has data issue: false hasContentIssue false
  • English
  • Français

23Na 2D 3QMAS NMR and 29Si, 27Al MAS NMR investigation of Laponite and synthetic saponites of variable interlayer charge

Published online by Cambridge University Press:  09 July 2018

L. Delevoye ,
J . -L. Robert  and
J . Grandjean
L. Delevoye*
Affiliation:
Bruker S. A. Solid-stateNMR ApplicationLab., F-67166 Wissembourg, France
J . -L. Robert
Affiliation:
ISTO, UMR 6113, CNRS -Université Orleans, F-45071 Orléans Cedex 2, France
J . Grandjean
Affiliation:
University of Liege, Institute of Chemistry B6a, COSM, Sart-Tilman, B-4000 Liege, Belgium
*
*E-mail: j.grandjean@ulg.ac.be
Get access Rights & Permissions [Opens in a new window]

Abstract

29Si, 27Al MAS NMR is used to characterize Laponite RD and synthetic saponites of variable interlayer charge. The Si/Al ratios are in good agreement with the calculated charge from chemical analysis except for the lowest-charged saponite. In contrast to the 29Si MAS NMR spectra in which resolved signals are detected, the 27Al MAS NMR spectra show one signal whose linewidth increases with the clay charge. The water content of the clay samples was obtained from 1H MAS NMR.

The 2D MQMAS NMR technique is required to obtain a high-resolution spectrum of nuclei with strong quadrupolar interaction. This method was applied to the 23Na nucleus of clay counterions and to the 27Al structural nucleus. One well-defined 23Na NMR signal is observed for all the clays studied except the highest-charged saponite. Possible explanations for this different behaviour are discussed. The calculated isotropic chemical shift evolves progressively with the clay charge whereas the deduced quadrupolar interaction does not change significantly. The 27Al 2D 3QMAS technique was not able to resolve more than one signal.

Keywords

2:1 phyllosilicatesaponiteLaponitesup1/supHsup23/supNasup27/supAl andsup29/supSi MAS NMR2D 3QMAS NMR
Type
Research Article
Information
Clay Minerals , Volume 38 , Issue 1 , March 2003 , pp. 63 - 69
Copyright
Copyright © The Mineralogical Society of Great Britain and Ireland 2003

Access options

Get access to the full version of this content by using one of the access options below. (Log in options will check for institutional or personal access. Content may require purchase if you do not have access.)

References

Alba, M.D., Becerro, A.I., Castro, M.A. & Perdigón, A.C. (2000) High-resolution 1H MAS NMR spectra of 2:1 phyllosilicates. Chemical Communications, 37–38.Google Scholar
Alma, N.C.M., Hays, G.R., Samoson, A.V. & Lippmaa, E.T. (1984) Characterization of synthetic dioctahedral clays by solid-state silicon-29 and aluminium-27 nuclear magnetic resonance. Analytical Chemistry, 56, 729–733.CrossRefGoogle Scholar
Amoureux, J.-P., Fernandez, C. & Steuernagel, S. (1996) Z-filtering in MQMAS NMR. Journal of Magnetic Resonance A, 123, 116–118.Google Scholar
Bergaoui, L., Lambert, J.F., Frank, R., Suquet, H. & Robert, J.-L. (1995) Al-pillared saponites part 3: Effect of parent clay layer charge on the intercalation-pillaring mechanism and structural properties. Journal of the Chemical Society Faraday Transaction s, 91, 2229–2239.Google Scholar
Boek, E.S., Coveney, P.V. & Skipper, N.T. (1995) Monte Carlo molecular modelling studies of Li-, Na- and Ksmectites: Understanding the role of potassium as a clay swelling inhibitor. Journal of the American Chemical Society, 117, 12608– 12617.Google Scholar
Fernandez, C., Delevoye, L., Amoureux, J.-P., Lang, D.P. & Pruski, M. (1997) 27Al﹛1H﹜ cross polarization triple-quantum magic angle spinning NMR. Journal of the American Chemical Society, 119, 6858–6862.Google Scholar
Gevers, C. & Grandjean, J. (2001) A multinuclear magnetic resonance study of synthetic clays suspended in water and in dodecyldimethylamine oxide solutions. Journal of Colloids and Interface Science, 236, 290– 294.Google Scholar
Grandjean, J. (2001) Interaction of a zwitterionic surfactant with synthetic clays in aqueous suspensions: A multinuclear magnetic resonance study. Journal of Colloids and Interface Science, 239, 27–32.CrossRefGoogle ScholarPubMed
Grandjean, J. & Robert, J.-L. (1999) 7Li double quantum filtered NMR and multinuclear relaxation rates of clay suspensions: The effect of clay concentration and nonionic surfactants. Journal of Magnetic Resonance, 138, 43–47.Google Scholar
Greathouse, J. & Sposito, G. (1998) Monte Carlo and molecular dynamics studies of interlayer structure in Li(H2O)3-smectites. Journal of Physical Chemistry B, 102, 2406–2414.Google Scholar
Hanaya, M. & Harris, R.K. (1998) Two-dimensional 23Na MQ MAS NMR study of layered silicates. Journal of Material Chemistry, 8, 1073–1079.Google Scholar
Herrero, C.P., Sanz, J. & Serratosa, J.M. (1989) Dispersion of charge deficits in the tetrahedral sheet of phyllosilicates. Analysis from 29Si NMR spectra. Journal of Physical Chemistry, 93, 4311– 4315.Google Scholar
Kim, Y. & Kirkpatrick, R.J. (1997) 23Na and 133Cs NMR study of cation adsorption on mineral surfaces: Local environments, dynamics, and effects of mixed cations. Geochimica et Cosmochimica Acta, 61, 5199–5208.Google Scholar
Kim, Y., Cygan, R.T. & Kirkpatrick, R.J. (1996) 133Cs NMR and XPS investigation of cesium adsorbed on clay minerals and related phases. Geochimica et Cosmochimica Acta, 60, 1041–1052.Google Scholar
Kinsey, R.E., Kirkpatrick, R.J., Hower, J., Smith, K.A. & Oldfield, E. (1985) High-resolution aluminium-27 and silicon-29 nuclear magnetic resonance study of layer silicates, including clay minerals. American Mineralogist, 70, 537–548.Google Scholar
Komadel, P., Madejová J., Janek, M., Gates, W.P., Kirkpatrick, R.J. & Stucki, J.W. (1996) Dissolution of hectorite in inorganic acids. Clays and Clay Minerals, 44, 228– 236.Google Scholar
Lambert, J.F., Prost, R. & Smith, M.E. (1992) 39K solidstate NMR studies of potassium tecto- and phyllosilicates: The in situ detection of hydratable K+ in smectites. Clays and Clay Minerals, 40, 253–261.Google Scholar
Laperche, V., Lambert, J.F., Prost, R. & Fripiat, J.J. (1990) High-resolution solid-state NMR of exchangeable cations in the interlayer surface of a swelling mica: 23Na, 111Cd, and 133Cs vermiculites. Journal of Physical Chemistry, 94, 8821– 8831.Google Scholar
Luca, V., Cardile, C.M. & Meinhold, R.H. (1989) Highresolution multinuclear NMR study of cation migration in montmor illonite. Clay Minerals, 24, 115– 119.Google Scholar
Mandair, J.-P.S., Michael, P.J. & McWhinnie, W.R. (1990) 29Si MAS NMR investigations of the the rmochemistry of laponite and hec torite. Polyhedron, 9, 517–525.CrossRefGoogle Scholar
McKenzie, K.J.D. & Meinhold, R.H. (1994) The thermal reactions of synthetic hectorite studied by 29Si, 25Mg and 7Li magic angle spinning nuclear magnetic resonance. Thermochimica Acta, 232, 85–94.CrossRefGoogle Scholar
Medek, A., Harwood, J.S. & Frydman, L. (1995) Multiplequantum magic-angle spinning NMR: A new method for the study of quadrupolar nuclei in solids. Journal of the American Chemical Soc ie ty, 117, 12779–12787.Google Scholar
Michot, L.J. & Villiéras, F. (2002) Assessment of surface energetic heterogeneity of synthetic Na-saponites. The role of layer charge. Clay Minerals, 37 39 – 57.CrossRefGoogle Scholar
Pruski, M., Wiench, J.W. & Amoureux, J.P. (2000) On the conversion of triple- to single-quantum coherences in MQMAS NMR. Journal of Magnetic Resonance, 147, 286– 295.CrossRefGoogle ScholarPubMed
Sanz, J. & Serratosa, J.M. (1984) 29Si and 27Al highresolution NMR spectra of phyllosilicates. Journal of the American Chemical Society, 106, 4790–4793.Google Scholar
Sanz, J. & Robert, J.-L. (1992) Influence of structural factors on 29Si and 27Al NMR chemical shifts of phyllosilicate s 2:1. Physics and Chemistry of Minerals, 19, 39–45.Google Scholar
Schroeder, P.A. & Pruett, R.J. (1996) Fe ordering in kaolinite: Insights from 29Si and 27Al MAS NMR spectroscopy. American Mineralogist, 81, 26–38.Google Scholar
Smith, M.E. & van Eck, E.R.H. (1999) Recent advances in experimental solid state NMR methodology for half-integer spin quadrupolar nuclei. Progress in Nuclear Magnetic Resonance Spectroscopy, 34, 159–201.Google Scholar
Sposito, G. & Prost, R. (1982) Structure of water adsorbed on smectites. Chemical Reviews, 82, 553–572.Google Scholar
Tkáč, I., Komadel, P. & Müller, D. (1994) Acid-treated montmorillonites – A study by 27Si and 29Al MAS NMR. Clay Minerals, 29, 11–19.Google Scholar