Pharmaceutical active compounds, including hundreds of different substances, are counted among the emerging contaminants in waterbodies, whose presence raises a growing concern for the ecosystem. Drugs are metabolized and excreted mainly through urine as an unchanged active ingredient or in the form of metabolites. These emerging contaminants are not effectively removed with the technologies currently in use, making them a relevant environmental problem. This study proposes the treatment of urine and water at the source that can allow an easier removal of dissolved drugs and metabolites. The treatment of synthetic urine, with dissolved ibuprofen as a model compound, by adsorption, using various classes of inorganic materials, such as clays, hierarchical zeolites and ordered mesoporous silica (MCM-41), is presented. A multi-technique approach involving X-ray powder diffraction, solid-state NMR, UV-Vis and Raman spectroscopies was employed to investigate the adsorption process in inorganic adsorbents. Moreover, the uptake, the ensuing competition, the efficiency and selectivity as well as the packing of the model compound in ordered mesoporous silica during the incipient wetness impregnation process were all thoroughly monitored by a novel approach, involving combined complementary time-resolved in situ 1H and 13C MAS NMR spectroscopy as well as X-ray powder diffraction.
This manuscript deals with the thermal and chemical modification of a natural kaolinite that shows excellent performance in the capture of a cationic organic pollutant from the aqueous phase. Kaolinite was calcined at 700 °C and treated with HCl to remove aluminium and to obtain a siliceous material. The structural changes and the physico-chemical properties of the materials at different stages of thermal and chemical modification were investigated with several techniques, including XRPD, MAS-NMR, SEM-EDX, FT-IR, and N2 physisorption at 77 K. The ability of the parent kaolinite and siliceous material to capture the organic dye, Rhodamine B, from the aqueous phase was investigated by means of UV-Vis spectroscopy. The siliceous material exhibited better adsorption capacity with respect to the parent kaolinite. Finally, the functional stability of the siliceous material was tested over three cycles of regeneration and adsorption.
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