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Characterization of synthetic Cs-Li cancrinite grown in a butanediol-water system: An NMR spectroscopic and Rietveld refinement study

¹ Institut für Mineralogie, Universität Hannover, Welfengarten 1, 30167 Hannover, Germany
² University of British Columbia, Department of Chemistry, 2036 Main Mall, Vancouver, B.C. V6T 1Z1, Canada
³ University of British Columbia, Department of Earth and Ocean Sciences, 6339 Stores Road, Vancouver, B.C. V6T 1Z4, Canada

Correspondence: ^* E-mail: M.Fechtelkord{at}mineralogie.uni-hannover.de

A Cs-Li-analogue of cancrinite has been synthesized from tetraethoxysilane and Al sec-butoxide in a mixture of 1,3-butanediol and water. Cs and Li were introduced as hydroxides. Synthesis was done at autogeneous pressure and T = 473 K for 100 h. The synthesis product was characterized by powder X-ray diffraction, IR-spectroscopy, thermogravimetry, ¹H, ⁶Li, ⁷Li, ¹³³Cs, ²⁷Al, ²⁹Si MAS, and {¹H} ¹³C CPMAS NMR and Rietveld structure refinement. ²⁹Si MAS NMR and ²⁷Al MAS NMR spectroscopy show a framework with strong alternating order of the SiO₄ and AlO₄ tetrahedra and an Si/Al ratio of one. ⁶Li MAS NMR suggests the existence of two different signals that cannot be resolved in the ⁷Li MAS NMR spectrum. ¹³³Cs MAS NMR shows only a single resonance. The thermogravimetric analysis reveals a continuous weight loss in several steps, indicating the evaporation of water of hydration. IR spectroscopy shows evidence for hydroxyl anions and water included in the cancrinite framework. The Rietveld structure refinement is consistent with a completely ordered alumosilicate framework with an Si/Al ratio of one and the presence of both molecular water and hydroxyl groups in the hexagonal channel, a result different from the previously published structure. Cs is exclusively located in the -cages; Li ions are located in the channels and are coordinated by water molecules.

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				M. FECHTELKORD, B. POSNATZKI, and J.-C. BUHL Characterization of basic cancrinite synthesized in a butanediol-water system European Journal of Mineralogy, June 1, 2003; 15(3): 589 - 598. [Abstract] [Full Text] [PDF]