The adsorption technique for the process of extracting or separating heavy metal contaminants from solutions was more effective. Activated carbon produced from watermelon rind (ACWR), Borokly clay (BoC) and Aswany clay (AsC) were identified by FT-IR spectroscopy, electron microscope (SEM) and X-ray fluorescence which used to separate Manganese(II) and iron(III) from an aqueous systems. pH, sorbent weights, contact time, temperature and initial concentration of Manganese(II) & iron(III) were studied to obtain the most favorable conditions for removment of these ions. The results were clear that the removal of metal ions raised with increasing of contact time and sorbent weights. Also, the removal percentage decreased as the initial concentration of the two metals increased. The overall adsorption capacities of ACWR, BoC and AsC for Manganese(II) were 35.40, 32.73 and 33.37 mg/L and for iron(III) were 35.99, 36.95 and 37.87 mg/L. The results showed that the removal of Manganese(II) and iron(III) was enhanced under the following optimal conditions: pH 5, contact time 35 minutes, sorbent weight 0.4 g, and temperature 50 °C. The Three sorbent materials could be effectively regenerated by using bidistilled water for more than five cycles. Adsorption kinetics followed the pseudo-first-order model, and Langmuir isotherm provided a good fit to the experimental data.