Solid state NMR study of oxygen site exchange and Al-O-Al site concentration in analcime

Abstract

Oxygen isotope exchange between natural analcime and water vapor at low pressure is studied by 17O NMR, which can distinguish Si-O-Si and Si-O-Al sites and provide information on site specific exchange kinetics and mechanisms. Si-O-Al sites in analcime are found to exchange faster than Si-O-Si sites at lower temperature (400 °C). At higher temperature (500 °C), the exchange rates for the two types of site are similar, suggesting that the exchange process for Si-O-Si has a higher activation energy, as predicted by published theoretical calculations. The overall exchange reaction appears to be controlled largely by reaction at sites, not diffusion. Static 17O spectra show an anomalously high ratio of Si-O-Si to Si-O-Al sites, suggesting the presence of a few percent of Al-O-Al sites, which are indeed resolved and observed in triple quantum magic-angle spinning (3QMAS) spectra.