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In the present study, Electrocoagulated Metal Hydroxide Sludge (EMHS) was analyzed as adsorbent material to remove both fluoride ion (F-) and arsenic V (As(V)) from aqueous effluents. This material was generated during an electrocoagulation process using Aluminum anode. It was characterized by using specific surface areas and the surface morphology was studied by scanning electron microscopy (SEM). Adsorbent fixed-beds are generally studied to remove different class of contaminants. EMHS was evaluated using a continuous flow rate column test with an experimental design. The effect of initial concentration of F- (2.5–10 mg L−1) and the Empty Bed Contact Time (EBCT (0.4–0.8 min)) was studied following a central composite design methodology. The experimented parameters had a significant influence on saturation time, breakthrough volume, and breakthrough time. A response surface analysis was a tool for analyzing the adsorption study, showing interactions that are complicated to identify by others methods. The results, here reported, revealed that EMHS is an efficient and promising adsorbent material in order to remove F- and As(V) from water contaminated by these pollutants.