This study focuses on Pb2+ and As(V) adsorption on mineral heterostructures based on a mixture of Si, Fe, and Ti oxides (MOHs). Various techniques were performed to analyze the morphological and structural properties of the synthesized metal oxide samples. In addition to the experimental optimization of the parameters determined by the response surface method (RSM), the effects of pH, adsorbent dosage, temperature, and contact duration on the batch and column system adsorption efficiency of single-component and simultaneous lead and arsenate removal were tested. The pseudo-second-order kinetic model and Weber–Morris model were more relevant to the adsorption on the metal(loid)s. The adsorption of Pb2+ was related to the Langmuir isotherm model, while the adsorption of As(V) was fitted to the Freundlich isotherm model. The thermodynamic parameters indicate the spontaneity of the adsorption process with a low endothermic character. The MOHs were more effective in removing Pb2+ and As(V) in the multi-component system (87.7 and 46.1%, respectively) than in the single-component system (56.3 and 23.4%, respectively). This study demonstrates that mineral heterostructures can be effectively used to remove cations and anions from water systems, and due to their fast kinetics, they can be applied to the needs of rapid interventions after pollution.
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