This thesis focuses on determination of the Optimum carbonization temperature for both rice husk and spent coffee by pyrolysis at temperatures of 200, 500 and 900 degrees centigrade .Initial dye concentration and contact time as factors of as adsorption we re investigated by using the ACs prepared at the three different temperatures as the adsorbent for methyl orange solutions and the residual solutions' dye concentration assessed using the UV spectrophotometer at 468nm.Based on the comprehensive experiments on the effects of contact time and initial dye concentration, results were as presented below in the report. The removal efficiencies of the Activated Carbons were compared by applying the ACs treatment of a wastewater sample and determining percentage removal. The results showed that percentage removal for both RH-AC and SP-AC decreased as the pyrolysis Temperature increased, giving 200 degrees centigrade as the best carbonization temperature for each.