An advanced oxidation process, anodic Fenton treatment (AFT), and a mixed microbial culture were used to degrade metribuzin [4-amino-6-tert-butyl-3-methylthio-1,2,4- triazin-5(4H)-one], a broad-use triazinone herbicide. Complete and rapid removal of metribuzin was demonstrated. The appearance and subsequent degradation of metribuzin oxidation products--deaminated metribuzin (DA), diketo metribuzin (DK), as well as the production of deaminated diketo metribuzin (DADK)--were observed. To support the use of AFT as a chemical pretreatment, the ratio of 5-day biochemical oxygen demand (BOD5) as measured in the standard test to chemical oxygen demand (COD) was investigated, and an increase from 0.03, a nonbiodegradable solution, to 0.35, a biodegradable solution, was observed. This increase in biodegradability was associated with decreased metribuzin, DA, and DK concentrations and increased DADK concentration. AFT effluent was inoculated with either an enriched microbial culture or Polyseed, a commercially available inoculum. Although there was minimal biodegradation of the remaining metribuzin, there was a significant decrease in DA concentration in inoculated incubations compared with sterile controls after 5- and 10-minute AFT treatment. The enrichment inoculate appeared more adapted toward the less-oxidized, 5-minute-treated effluent, whereas the Polyseed culture, developed to degrade complex waste solutions, appeared to be more effective in a moreoxidized, 10-minute-treated, and potentially more complex effluent. This research supports the continued investigation of AFT and biodegradation as a binary treatment of aqueous pesticide wastes.