Power plants burning coal generate a large amount of fly ash as waste matter. The objective of this study is to produce zeolitic adsorbents that possesses high adsorptive capacity for toxic cations. The sample was first pretreated with a High Intensity Magnetic Separator for the removal of iron and magnetic materials (mainly Fe₂O₃ and TiO₂). The zeolitic adsorbents were prepared under the various conditions of NaOH concentration (1-5N), reaction time from 3 to 96 hours and at the various temperatures of 60, 80 and 100℃. The results of the experiment showed that the coal fly ash should be synthesized with 4 N NaOH for 48 hours at 100℃ in order to have good adsorptive capacity. The zeolitic adsorbents showed higher cation exchange capacity values than the natural zeolite in removing NH₄⁺, Pb²⁺, Ca²⁺ and Cd²⁺ ions.