Layered Double Hydroxides of Mg–Al–Fe and their mixed metallic oxides of high specific surface area were synthesized by the coprecipitation method. A natural zeolite from a regional quarry with high clinoptilolite content was conditioned and modified. Initially, an acid treatment was applied and subsequently Fe(III) was incorporated by the wet impregnation method. Then the prepared solid materials were characterized by XRD, N2 adsorption–desorption at 77 K, SEM, DRS UV–Vis, and MP-AES to determine their physicochemical properties. Finally, the solid materials were evaluated as adsorbents for arsenic removal in water. The tracking of As and its species concentration at trace levels was carried out by cathodic stripping Square-wave voltammetry, which has proved to be a highly selective and sensitive electrochemical method. High levels of effectiveness in terms of removal were achieved, particularly with the natural zeolites and mixed oxides of highest iron content.Fil: CITeQ-CONICET, Facultad Regional Córdoba, Universidad Tecnológica Nacional, Maestro Marcelo López esq. Cruz Roja Argentina, Ciudad Universitaria, X5016ZAA, Córdoba, Argentina Angélica Heredia, Jenny Gómez Avila, Ariel Vinuesa, Clara Saux & Mónica Crivello CONICET, Facultad Regional Reconquista, Universidad Tecnológica Nacional, Reconquista, Argentina Sandra M. Mendoza INFIQC-CONICET, Departamento de Físico Química, Facultad de Ciencias Químicas, Universidad Nacional de Córdoba, Pabellón Argentina, Ciudad Universitaria, X5000HUA, Córdoba, Argentina Fernando GarayPeer Reviewed