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A rapid preparation method of TiO 2- x by thermal treatment using H 2 TiO 3 as the precursor was proposed compared with the static hydrogenation thermal treatment process. Its adsorption properties of arsenic under visible light were explored and investigated as well. Various colors of TiO 2- x were prepared and characterized via XRD, TEM, BET, and so on. The results indicate that the method of rapid preparation is feasible. The TiO 2- x exhibits a larger particle size that varied from 10 nm to 2 μm, and deeper color products were obtained as the treatment temperature increased from 600 to 900 °C. Light yellow TiO 2- x was prepared after increasing the temperature from 600 to 900 °C, Ti 4 O 7 and Ti 6 O 11 with a dark color were formed under a H 2 atmosphere at 1500 °C. The arsenic adsorption performances of some samples under visible light were tested, and reveal a high efficiency of TiO 2- x in the photocatalytic oxidation arsenic adsorption under visible light, the conversion ratio of As(III) photocatalytic oxidation fluctuates around 2.85 mgAsg -1 h -1 . In the absence of visible light, the adsorption capacities for As(III) and As(V) are 3.7 and 42.7 mg/g, respectively, at pH = 3. Under visible light condition, the adsorption capacity of As(III) increases sharply to 15.6 mg/g, which provides the foundation for a new application of TiO 2- x in the field of arsenic adsorption.