In this study, batch adsorption experiments were carried out for the removal of nickel ions from aqueous solutions using an agricultural waste biomass (olive pulp) as adsorbent. Response surfacemethodologywas performed to optimize the adsorption process. Plackett-Burman design (PBD) was used in the first step to evaluate the effects of five independent variables on the yield adsorption of metal. Among these variables, initial pH of the medium, initial concentration of the nickel ions and the dose of the adsorbent were screened as significant variables and were then further optimized using response surface methodology based on a Box-Behnken design (BBD). Very high value of regression coefficient (R2=0.9780) indicates excellent evaluation of experimental data by second-order polynomial regression model. The optimum conditions formaximumremoval of nickel ions fromaqueous solutionwere found to be as follows: pH(4.43), adsorbent dose (18.40 g/L) and initial concentration of nickel ions (15.76 mg/L).