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Zirconium oxide (ZrO2)-carbon nanofibers (ZCN) were fabricated and batch experiments were used to determine antimonite (Sb(III)) and antimonate (Sb(V)) adsorption isotherms and kinetics. ZCN have a maximum Sb(III) and Sb(V) adsorption capacity of 70.83 and 57.17 mg/g, respectively. The adsorption process between ZCN and Sb was identified to be an exothermic and follows an ion-exchange reaction. The application of ZCN was demonstrated using tap water spiked with Sb (200 μg/L). We found that the concentration of Sb was well below the maximum contaminant level for drinking water with ZCN dosages of 2 g/L. X-ray photoelectron spectroscopy (XPS) revealed that an ionic bond of Zr–O was formed with Sb(III) and Sb(V). Based on the density functional theory (DFT) calculations, Sb(III) formed Sb–O and O–Zr bonds on the surface of the tetragonal ZrO2 (t-ZrO2) (111) plane and monoclinic ZrO2 planes (m-ZrO2) (111) plane when it adsorbs. Only an O–Zr bond was formed on the surface of t-ZrO2 (111) plane and m-ZrO2 (111) plane for Sb(V) adsorption. The adsorption energy (E ad) of Sb(III) and Sb(V) onto t-ZrO2 (111) plane were 1.13 and 6.07 eV, which were higher than that of m-ZrO2 (0.76 and 3.35 eV, respectively).