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Solid-State Nuclear Magnetic Resonance Spectroscopy on Synthetic Ammonium/Aluminum-Saponites

Published online by Cambridge University Press:  28 February 2024

J. T. Kloprogge ,
J. Breukelaar ,
A. E. Wilson ,
J. W. Geus  and
J. B. H. Jansen
J. T. Kloprogge*
Affiliation:
Department of Geochemistry, Institute of Earth Sciences, University of Utrecht, Budapestlaan 4, P.O. Box 80.021, 3508 TA, Utrecht, The Netherlands
J. Breukelaar
Affiliation:
Koninklijke/Shell-Laboratorium Amsterdam (Shell Research B.V.), P.O. Box 3003, 1003 AA Amsterdam, The Netherlands
A. E. Wilson
Affiliation:
Koninklijke/Shell-Laboratorium Amsterdam (Shell Research B.V.), P.O. Box 3003, 1003 AA Amsterdam, The Netherlands
J. W. Geus
Affiliation:
Department of Inorganic Chemistry, University of Utrecht, P.O. Box 80.083, 3508 TB Utrecht, The Netherlands
J. B. H. Jansen*
Affiliation:
Department of Geochemistry, Institute of Earth Sciences, University of Utrecht, Budapestlaan 4, P.O. Box 80.021, 3508 TA, Utrecht, The Netherlands
*
**Present address: TNO-Institute of Applied Physics TU Delft, Department of Inorganic Materials Chemistry, P.O. Box 595, 5600 AN Eindhoven, The Netherlands
***Present address: Bowagemi B.V., Prinses Beatrixlaan 20, 3972 AN Driebergen, The Netherlands
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Abstract

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Ammonium-saponite is hydrothermally grown at temperatures below 300°C from a gel with an overall composition corresponding to (NH4)0.6Mg3Al0.6Si3.4O10(OH)2. Using 27Al and 29Si solid-state Magic Angle Spinning NMR techniques it is demonstrated that synthetic ammonium-saponites have a rather constant Si/AlIV ratio (≈ 5.5) and an AlIV/AlVI ratio that varies between 1.5 and 3.8. The above ratios are independent of the synthesis temperature, although an increasing amount of Si, N, and, to a lesser extent, Al are incorporated in an amorphous phase with increasing temperature. 27Al MAS-NMR is unable to differentiate between Al at octahedral and Al3+ at interlayer sites. CEC, XRD, and the inability to swell prove the AlVI to be mainly on the interlayer sites. Based on the NH4- exchange capacity, X-ray fluorescence, 27Al and 29Si MAS-NMR, it is possible to calculate a relatively accurate structural formula.

Keywords

27Al/29Si MAS-NMRSaponiteSynthesis
Type
Research Article
Information
Clays and Clay Minerals , Volume 42 , Issue 4 , August 1994 , pp. 416 - 420
Copyright
Copyright © 1994, Clay Minerals Society

Footnotes

*

This paper is a joint contribution from the Debye Institute, University of Utrecht, The Netherlands, and Shell Research B.V.

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