Fe 2 O 3 /TiO 2 composite has been extensively studied for heavy metals removal and photocatalysis. In photocatalysis, this composite was used for the degradation of organic dye pollutants. Herein, we reported a green approach to fabricate Fe 2 O 3 /TiO 2 nanoparticles from ilmenite ore. The Fe 2 O 3 /rutile was synthesized by one-step reaction of ilmenite at 700 °C in 3 h, the raw Fe 2 O 3 /rutile composite was, then, grounded by a ball-milled process in 4 h to obtain nanostructured composite. The obtained Fe 2 O 3 /rutile nanoparticles have the diameter of 50-100 nm with the BET surface area of 7 m 2 g −1 . The adsorption behaviour of the nanostructured Fe 2 O 3 /TiO 2 composite as adsorbent toward arsenic (particularly, oxidized form of arsenic [As(V)]) was investigated by carrying out batch adsorption. The adsorption isotherm was investigated by using both the Langmuir and Freundlich models. The sorption kinetics of adsorbent toward arsenic adsorption was found to be pseudo-second order. The Fe 2 O 3 /TiO 2 composite exhibited fast and high adsorption capacity of 47.12 mg g −1 toward arsenic in various solution pHs. The composite was also found to be durable and recyclable for arsenic adsorption. Therefore, this as-prepared Fe 2 O 3 /TiO 2 composite could be promising and cost-effective adsorbent for effective removal of arsenic contaminant from aqueous environment.