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Flowerlike α-Fe₂O₃ nanostructures were synthesized via a template-free microwave-assisted solvothermal method. All chemicals used were low-cost compounds and environmentally benign. These flowerlike α-Fe₂O₃ nanostructures had high surface area and abundant hydroxyl on their surface. When tested as an adsorbent for arsenic and chromium removal, the flowerlike α-Fe₂O₃ nanostructures showed excellent adsorption properties. The adsorption mechanism for As^V and Cr^VI onto flowerlike α-Fe₂O₃ nanostructures was elucidated by X-ray photoelectron spectroscopy and synchrotron-based X-ray absorption near edge structure analysis. The results suggested that ion exchange between surface hydroxyl groups and As^V or Cr^VI species was accounted for by the adsorption. With maximum capacities of 51 and 30 mg g^–1 for As^V and Cr^VI, respectively, these low-cost flowerlike α-Fe₂O₃ nanostructures are …