A typical wastewater effluent of a chemical process can contain several strong acids/bases, weak acids/bases as well as their salts. They must be neutralized before being discharged to the environment in order to protect aquatic life and human welfare. However, neutralization process is highly non&ndash / linear and has time&ndash / varying characteristics. Therefore, the control of pH is a challenging problem where advanced control strategies are often considered. In this study, the aim is to design a pH control system that will be capable of controlling the pH-value of a plant waste-water effluent stream having unknown acids with unknown concentrations using an on&ndash / line identification procedure. A Model Predictive Controller, MPC, and a Fuzzy Logic Controller, FLC, are designed and used in a laboratory scale pH neutralization system. The characteristic of the upstream flow is obtained by a small identification reactor which has ten times faster dynamics and which is working parallel to actual neutralization tank. In the control strategy, steady&ndash / state titration curve of the process stream is obtained using the data collected in terms of pH value from the response of the identification reactor to a pulse input in base flow rate and using the simulated response of the identification reactor for the same input. After obtaining the steady&ndash / state titration curve, it is used in the design of a Proportional&ndash / Integral, PI, and of an Adaptive Model Predictive Controller, AMPC. On the other hand, identification reactor is not used in the FLC scheme. The performances of the designed controllers are tested mainly for disturbance rejection, set&ndash / point tracking and robustness issues theoretically and experimentally. The superiority of the FLC is verified.