Aqueous NH 4 OH-treated and subsequently calcined forms of local natural zeolitic tuff were characterized by different techniques including scanning electron microscopy (SEM), X-ray powder diffraction, inductively coupled plasma-atomic emission spectroscopy (ICP-AES), volumetric N 2 adsorption at À196 C, thermogravimetry (TG), differential scanning calorimetry (DSC), and transmittance infrared spectroscopy. The dehydration behavior of the samples was investigated using an in situ temperature-programmed diffuse reflectance Fourier transform infrared spectroscopy (TP-DRIFTS) method under vacuum. The DRIFTS spectra recorded yielded information about the effect of the NH 4 OH treatment and subsequent calcination on the dehydration behavior of the natural zeolite. Changes in the infrared bands corresponding to vibrations of the OÀH and NÀH bonds upon in situ heating under vacuum were analyzed.Keywords Ammonium hydroxide treatment; Characterization;Clinoptilolite; Dehydration; DRIFTS
INTRODUCTIONNatural zeolites constitute a group of minerals having open aluminosilicate frameworks containing channels and cavities that accommodate cations and water molecules. Generally, these cations are exchangeable and the water molecules can be removed or replaced reversibly without disrupting the framework. The presence of water in the pores hinders adsorption of other molecules; thus adsorption and catalytic properties of zeolites are directly related to their water content. Water is adsorbed into zeolites by filling oxygen-lined channels and hydrating the cations present in the channels. The observed macroscopic thermal behavior of a zeolite depends on the type, amount, and position of the extraframework cations within the structure, their coordination to water molecules, their interactions with framework oxygen atoms, the presence of other water molecules, Si=Al ratio, time, temperature, pressure, and heating rate.Dehydration behaviors of clinoptilolite have been investigated by various analytical techniques including