Two-phase anaerobic digestion has often been considered beneficial for the treatment of high strength industrial wastewaters, especially when the first phase is used as a pre-treatment system known as pre-acidification. Several applications in the field of industrial wastewater treatment have been reviewed in order to evaluate the advantages of the pre-acidification process and its effects on the methanogenic reactor. Although pre-acidification has obvious advantages, complete acidification may be detrimental to the efficiency of the overall process. The use of balancing tanks at full-scale has been common practice for the pre-acidification of a wide range of wastewaters yet no accepted design criteria for acidogenic reactors have been formulated and two-phase applications are generally based upon previous experience. The paper summarizes the results of a two year investigation into pre-acidification at both bench- and pilot-scale, presents the results of instant coffee production wastewaters and discusses a wide range of parameters which have been evaluated. Operating criteria will be discussed and guidelines for the design of pre-acidification reactors will be presented. Finally alternatives to using the total VFA (volatile fatty acids) concentrations for expressing the efficiency of acidogenesis will be introduced.