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Several methods have been developed and applied in recent years in the characterization of the structure of microporous materials, in general, and of pillared clays, in particular. In the present article, the latest results obtained in the control of the microstructure developed in alumina-pillared clays and various approaches used to the evaluation of the porosity of these materials are reviewed. These include the control of the microstructure developed in pillared clays by adjusting the several parameters involved in the synthesis process, and the evaluation of the porosity of pillared clays. Emphasis is given to the methods to evaluate the pore size and pore size distribution (PSD) of these materials. Two separate sections are devoted to review mathematical modeling studies and 129 Xe NMR spectroscopy of physisorbed Xe to investigate the microporous structural properties of these materials.

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