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Arsenic [As(III) and As(V)] adsorption on aluminum substituted cobalt ferrite (Co−Al−Fe) ternary metal oxide adsorbent is reported by means of qualitative and quantitative spectroscopy tools. IR and Raman active signals were observed around 810–920 cm–1band indicate different As−OHcomplexedand As−Ouncomplexedstretching vibrations on to the adsorbent. The adsorption behavior of arsenic (III and V) onto these adsorbents is studied as a function of contact time, different concentrations, and pH conditions. The kinetics study on adsorption were performed to understand nature of adsorption which supports the Pseudo Second Order (PSO) model. The adsorption isotherms study indicates Freundlich type of adsorption. The maximum adsorption capacity of Co−Al−Fe adsorbent is observed around 130 and 76 mg g–1for As(III) and As(V) systems, respectively. Detailed XPS study of As 3d, Fe 2p, Co 2p, and O 1s spectra has been reported in explaining the redox behavior and ligand exchange reactions in supporting arsenic adsorption mechanism.