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Novel composites of iron oxide encapsulated in macroporous silica with excellent arsenic adsorption performance have been successfully developed. Macroporous silica foams with large pore sizes of ≈100 nm and a high pore volume of 1.6 cm³ g⁻¹ are chosen as the porous matrix. Electron tomography technique confirms that γ‐Fe₂O₃ nanoparticles with an average particle size of ≈6 nm are spatially well‐dispersed and anchored on the pore walls at even a high γ‐Fe₂O₃ content of 34.8 wt%, rather than forming aggregates inside the pores or on the external surface. The open large‐pore structure, high loading amount, and the non‐aggregated nature of γ‐Fe₂O₃ nanoparticles lead to increased adsorption sites and thus high adsorption capacities of both As (V) and As (III) without pre‐treatment (248 and 320 mg g⁻¹, respectively). Moreover, the composites can reduce the concentration of both As (V) and As (III …