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Previous works (Beccari et al. 1999b; Beccari et al. 2001a; Beccari et al. 2001b)on the anaerobic treatment of olive oil mill effluents (OME) have shown: (a) apre-treatment based on the addition of Ca(OH)₂ and bentonite was able toremove lipids (i.e. the most inhibiting substances present in OME) almostquantitatively; (b) the mixture OME – Ca(OH)₂ – bentonite, fed to amethanogenic reactor without providing an intermediate phase separation,gave way to high biogas production even at very low dilution ratios; (c) theeffluent from the methanogenic reactor still contained significant concentrationsof residual phenolic compounds (i.e. the most biorecalcitrant substances present inOME). Consequently, this paper was aimed at evaluating the fate of the phenolicfractions with different molecular weights during the sequence of operations(adsorption on bentonite, methanogenic digestion, activated sludge post …