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Cerium oxide (CeO2) nanoparticles of size 3–5 nm and surface area 257 m2 g−1 were synthesized using simple, single‐pot, and surfactant‐free aerogel process. Efforts were made to tune the surface area and porosity of CeO2 nanoparticles by changing the concentration of precursors. CeO2 nanoparticles were characterized by TEM, SEM, XRD, N2‐BET, and FTIR. Prepared CeO2 was used to remove As(III) and As(V) from water at variable contaminant concentrations (25–100 ppm) and pH (3–10). The adsorption process found extremely fast for the first few minutes of exposure. CeO2 nanoparticles indicated adsorption capacities of 71.9 and 36.8 mg g−1 against As(III) and As(V), respectively. The adsorption data best fitted with Redlich–Peterson model, depicting monolayer adsorption. The adsorption followed pseudo‐second‐order kinetics and intraparticle diffusion with three‐step diffusion process. The effect of co‐existing anions (H2 PO 4 −, SO 4 2 −, and HCO 3 −) indicated 80–96% reduction in adsorption capacity. © 2017 American Institute of Chemical Engineers Environ Prog, 37: 221–231, 2018 [ABSTRACT FROM AUTHOR]