Effective adsorbent was prepared from Egyptian Muscovite by activation with H₂O₂, HCl and/or H₂O₂ / HCl. The prepared adsorbents were applied for the removal of cadmium and lead from polluted water. Raw Muscovite powder was activated by different treatments using 30% H₂O₂, HCl, and/or HCl /H₂O₂. Optimum adsorption conditions of pH, adsorbent dose, initial metal concentration, stirring time and solution temperature were optimized for the maximum adsorption of Cd and Pb. The results reveal that the Muscovite adsorbent prepared with a mixture of HCl /H₂O₂ shows the higher adsorption of Cd and Pb than that with HCl or H₂O₂. The maximum adsorption of Cd and Pb by the developed adsorbent was 97.8% and 98.1%, respectively at 60 min ,25°C, initial metal concentration 50 ppm, adsorbent dose 2g/50 mL solution and pH 6 for lead and pH7 for cadmium. Adsorption isotherms and kinetic models were investigated and ended to that the adsorption of Pb and Cd fitted well Langmuir adsorption isotherm.