The optimization conditions of preparation of activated carbons based Balanites aegytiaca shells by chemical activation was investigated. The effects of three parameters of preparation namely, the activation temperature (600-800 °C), impregnation ratio (1:4-3:8) and residence time (60-120 min) were thoroughly studied on the activated carbon yield (Yld, Y1), iodine number (ION,Y2) and methylene blue number (MBN, Y3) using the Methodology of Experimental Design (MED). The analysis of variance (ANOVA) under the experimental domain revealed that, the activation temperature of 800 °C, residence time of 02hrs and impregnation ratio of 1:2 were the optimum conditions of preparation leading to activated carbon yield of 23.0%, iodine number of 889.0 mg/g and methylene blue number of 9.7 mg/g. The polynomial equation showed that the three parameters were both synergetic and antagonistic on the responses retained. The higher values of iodine numbers obtained alongside the experimental matrix is an indication that the activated carbons so prepared were mainly microporous.