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.
Topaz [Al2SiO4(F,OH)2] is one of the main fluorine-bearing silicates occurring in environments where variably acidic (F)/aqueous (OH) fluids saturate the silicate system. In this work we fully characterized blue topaz from Padre Paraíso (Minas Gerais, Brazil) by means of in situ synchrotron X-Ray and neutron powder diffraction measurements (temperature range 298–1273 K) combined with EDS microanalyses. Understanding the role of OH/F substitution in topaz is important in order to determine the hydrophilicity and the exchange reactions of fluorine by hydroxyl groups, and ultimately to characterize the environmental redox conditions (H2O/F) required for mineral formation. The fluorine content estimated from neutron diffraction data is ~ 1.03 a.f.u (10.34 wt%), in agreement with the chemical data (on average 10.0 wt%). The XOH [OH/(OH + F)] (0.484) is close to the maximum XOH value (0.5), and represents the OH- richest topaz composition so far analysed in the Minas Gerais district. Topaz crystallinity and fluorine content sharply decrease at 1170 K, while mullite phase starts growing. On the basis of this behaviour, we suggest that this temperature may represent the potential initial topaz’s crystallization temperature from supercritical fluids in a pegmatite system. The log(fH2O/fHF)fluid (1.27 (0.06)) is coherent with the fluorine activity calculated for hydrothermal fluids (pegmatitic stage) in equilibrium with the forming mineral (log(fH2O/fHF)fluid = 1.2–6.5) and clearly different from pure magmatic (granitic) residual melts [log(fH2O/fHF)fluid < 1]. The modelled H2O saturated fluids with the F content not exceeding 1 wt% may represent an anomalous water-dominant / fluorine-poor pegmatite lens of the Padre Paraíso Pegmatite Field.
<p>In the upper mantle, volatiles control its composition, partial melting conditions, as well as the ascent rate of the formed melts. As consequence, volatile composition of the mantle is, in turn, recorded in the melts and, therefore, in the erupted basaltic rocks. Despite their importance, origin, budget, and fluxes of the volatiles in the upper mantle are poorly constrained. It is well known that the main input of mantle volatiles, such as carbon (C) and sulphur (S), represents components released from the subducting slab, <em>e.g.</em>, oceanic rocks and sediments, whose have characteristic isotopic signatures. In this view, studies of isotopic ratios of volatiles of subduction-related magmatic rocks could be used to identify the chemical components released by the subducting slab metasomatizing the upper mantle. To confirm this hypothesis, we investigated the major and trace element composition, as well as the C and S elemental contents and isotopic ratios of subvolcanic and volcanic rocks of the Vardar ophiolites of North Macedonia, which represent remnants of the Mesozoic Tethyan oceanic lithosphere formed in supra-subduction zone tectonic settings.</p><p>The ophiolites were sampled at Lipkovo and Demir Kapija localities, in the northern and southern part of North Macedonia, respectively. Based on whole-rock major and trace element composition, two main groups of rocks can be distinguished: i) Group 1 rocks, which are subalkaline basalts with backarc affinity and ii) Group 2 rocks, which are calc-alkaline basalts with arc affinity. The petrogenetic modelling based on trace and Rare Earth Elements, indicates that Group 1 mantle sources were affected by limited metasomatic processes by slab-released components, in particular aqueous fluids and sediment melts, whereas the Group 2 mantle sources were strongly metasomatized by sediment melts and adakitic melts. Accordingly, the Group 1 rocks exhibit C-enriched and S-depleted isotopic signature, indicating a minor involvement of melts from the subducting sediments. On the other hand, the C-depleted and S-enriched isotopic signatures of the Group 2 rocks suggest a major involvement of melts derived from the subducting sediments rich in organic matter and sulphate phases Therefore, both geochemical and isotopic data of the subvolcanic and volcanic samples of the North Macedonia ophiolites show that the sub-arc mantle sources are more affected by slab-released fluids than those of the backarc basin, which are more distal from the trench. Thus, combining the geochemical and isotopic data of subvolcanic and volcanic samples of complex geological framework can contribute to reconstruct the geodynamic scenarios, such as that of the Vardar ophiolites in the Dinaric-Hellenic belt. In addition, this approach may be useful to better understand the global geodynamic cycles of volatiles reconstructing their origin, budget, and isotopic composition, and understand the impacts on climate and environment from local to global scale.</p>
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