AbstractAdsorptive removal of manganese and fluoride from wastewater by waste tire‐derived activated carbon impregnated with iron and cobalt has been presented in this article. The surface properties of bimetallic activated carbon were characterized in scanning electron microscopy (SEM), Brunauer–Emmett–Teller (BET), and X‐ray diffraction (XRD). The newly developed adsorbent was used for simultaneous removal of fluoride and manganese from aqueous solution. Present work focuses on the optimization of process parameters using response surface method (RSM) technique employing significant parameters, namely, adsorbent dosage, initial fluoride and manganese concentrations, contact time and pH. Central composite design in RSM was utilized for the levels of adsorbent dosage (0.5–1 g/L), initial fluoride concentration (20–40 ppm), initial manganese concentration (30–50 ppm), time (15–35 min), and pH (4–8) of the solution. The R2 value obtained from the statistics data was 96.25 and 97.57% for fluoride and manganese, respectively. The optimal values were determined as the adsorbent dosage of 1.25 g/L, initial fluoride concentration of 10 ppm, initial manganese concentration of 25.25 ppm, the contact time of 30.9 min and pH of solution of 2.0, under which 99.96% manganese and 85.34% fluoride removal efficiency could be accomplished.