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In this work, the capability of two commercial high silica zeolites (HSZs), namely ZSM-5 and Y, for the removal of chlorobenzene (CB) from water was investigated by combining chromatographic and diffractometric techniques. The adsorption isotherms and kinetics of CB on ZSM-5 and Y zeolites were determined from batch tests. The adsorption kinetics were very fast; the time to reach equilibrium was less than 10 min. The equilibrium data of CB on the two HSZs showed dissimilarities that are particularly evident in the adsorption data concerning the low concentration range, where Y zeolite is characterized by low adsorption. On the contrary, at higher solution concentrations the adsorption capacity of Y is higher than that of ZSM-5. The crystalline structures of Y and ZSM-5 saturated with CB were investigated by X-ray diffraction (XRD) techniques. Rietveld refinement analyses of XRD data allowed for quantitative probing of the structural modifications of both zeolites after CB adsorption and provided insight into the preferred zeolite adsorption sites in both microporous materials. The refined framework-extraframework bond distances confirm that interactions between the selected organic contaminant and hydrophobic zeolites are mediated via co-adsorbed H2O. The occurrence of H2O -CB-framework oxygen oligomers explains variations in both the unit cell parameters and the shape of the channels, clearly confirming that water plays a very relevant role in controlling the diffusion and adsorption processes in hydrophobic zeolites. [ABSTRACT FROM AUTHOR]

The temperature-induced desorption of methyl tert-butyl ether (MTBE) from aqueous solutions onto hydrophobic ZSM-5 was studied by in situ synchrotron powder diffraction and chromatographic techniques. This kind of information is crucial for designing and optimizing the regeneration treatment of such zeolite. The evolution of the structural features monitored by full profile Rietveld refinements revealed that a monoclinic (P21/n) to orthorhombic (Pnma) phase transition occurred at about 100 °C. The MTBE desorption process caused a remarkable change in the unit-cell parameters. Complete MTBE desorption was achieved upon heating at about 250 °C. Rietveld analysis demonstrated that the desorption process occurred without any significant zeolite crystallinity loss, but with slight deformations in the channel apertures. [ABSTRACT FROM AUTHOR]

The adsorption of toluene from aqueous solutions onto hydrophobic zeolites was studied by combining chromatographic, thermal and structural techniques. Three beta zeolites (notated BEAs, since they belong to BEA framework type), with different SiO2/Al2O3 ratios (i.e., 25, 38 and 360), before and after calcination, were tested as adsorbents of toluene from aqueous media. This was performed by measuring the adsorbed quantities of toluene onto zeolites in a wide concentration range of solute. The adsorption data were fitted with isotherms whose models are based on surface heterogeneity of the adsorbent, according to the defective structure of beta zeolites. The thermal treatment considerably increases the adsorption of toluene, in the low concentration range, on all BEAs, probably due to surface and structural modifications induced by calcination. Among the calcined BEAs, the most hydrophobic zeolite (i.e., that with SiO2/Al2O3 ratio of 360) showed the highest binding constant, probably due to its high affinity for an organophilic solute such as toluene. The high sorption capacity was confirmed by thermogravimetric analyses on BEAs, before and after saturation with toluene. [ABSTRACT FROM AUTHOR]

The current study was designed to demonstrate the efficiency of selected zeolites in the immobilization of heavy metals and volatile organic compounds from water in the industrial area of Tito Scalo (Basilicata Region in Southern Italy). The efficiency of zeolite materials has been evaluated by analyzing real water samples, by a multi-technique approach. Gas chromatography (GC) and inductively coupled plasma optical emission spectrometry (ICP-OES) were selected for the detection of volatile organic compounds (VOCs) and heavy metals respectively, and then by thermal analysis (TG, DTA) and X-ray powder diffraction (XRD) to verify the presence of contaminants in the structural channels of the adsorbents. ZSM-5 zeolite (MFI topology) was suitable for volatile organic compounds, showing removal efficiencies 87%. 13X (FAU topology) was more selective for in situ abatements of heavy metals, with efficiencies up to 100%. After VOCs and heavy metals removal, structure refinements of loaded zeolites highlighted variations of both lattice parameters and extraframework content confirming the pollutants immobilization in the framework microporosities. The occurrence of these species was also confirmed by DTA curves showing different phenomena explained on the basis of the nature and number of extraframework species hosted in the zeolite micropores. [ABSTRACT FROM AUTHOR]

The present work focused on the use of high-silica commercial zeolites as sorbent media for pharmaceuticals in an aqueous matrix. As drug probes, ketoprofen, hydrochlorothiazide, and atenolol were selected, because of their occurrence in surface waters and effluents from wastewater treatment plants. Pharmaceuticals adsorption was evaluated for two Faujasite topology zeolites with Silica/Alumina Ratio 30 and 200. The selected zeolites were demonstrated to be efficient sorbents towards all investigated pharmaceuticals, thanks to their high saturation capacities (from 12 to 32% w/w) and binding constants. These results were corroborated by thermal and structural analyses, which revealed that adsorption occurred inside zeolite's porosities, causing lattice modifications. Finally, zeolites have been tested as a pre-concentration media in the dispersive-solid phase extraction procedure. Recoveries higher than 95% were gained for ketoprofen and hydrochlorothiazide and approximately 85% for atenolol, at conditions that promoted the dissolution of the neutral solute into a phase mainly organic. The results were obtained by using a short contact time (5 min) and reduced volume of extraction (500 µL), without halogenated solvents. These appealing features make the proposed procedure a cost and time saving method for sample enrichment as well as for the regeneration of exhausted sorbent, rather than the more energetically expensive thermal treatment. [ABSTRACT FROM AUTHOR]