The sorption properties of the MnO2/mechanically activated graphite composite with respect to As(III) compounds were studied. The static sorption capacity relative to As(III) compounds of the MnO2/mechanically activated graphite composite was 22.7 mg g–1, which exceeds the sorption properties of MnO2. The effect of solution pH in the range of 1–5, sorbent dose, and sorption time on the recovery of As(III) compounds was studied. It is shown that the process of As(III) sorption on the composite is described by the Freundlich model. The MnO2/mechanically activated graphite composite can be recommended for the removal of As(III) compounds from aqueous solutions.