Leather tanning effluents are a source of severe environmental impacts. In particular, the unhairing stage, belonging to the beamhouse processes, generates an alkaline wastewater with high concentrations of organic matter, sulphides, suspended solids, and salts, which shows significant toxicity. The objective of this work was to evaluate the biodegradation of this industrial wastewater by combined oxidative and biological treatments. An advanced oxidation process (AOP) with Fenton's reagent was used as batch pretreatment. The relationships of H2O2/Fe2+ and H2O 2/COD were 9 and 4, respectively, reaching an organic matter removal of about 90%. Subsequently, the oxidised beamhouse effluent was fed to an activated sludge system, at increasing organic load rates (OLR), in the range of 0.4 to 1.6 g COD/L·day. The biological organic matter removal of the pre-treated wastewater ranged between 35% and 60% for COD, and from 60% to 70% for BOD. Therefore, sequential AOP pretreatment and biological aerobic treatment increased the overall COD removal up to 98%, compared to 60% without pretreatment. Bioassays with D. magna and D. pulex showed that this kind of treatment achieves only a partial toxicity removal of the tannery effluent. © IWA Publishing 2004.