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Sediment from the upper Detroit and lower Rouge Rivers in southeastern Michigan, USA, were analyzed to examine the distribution of polychlorinated naphthalenes (PCNs), biphenyls (PCBs), dibenzo-p-dioxins (PCDDs), and dibenzofurans (PCDFs) as well as polycyclic aromatic hydrocarbons (PAHs) and alkylphenolic compounds such as butylphenol, octylphenol, and nonylphenol (NP). Sediments from a non-point source location in Lake Michigan were also analyzed for target compounds. Concentrations of target compounds in the upper Detroit and lower Rouge Rivers varied considerably among locations, and notable spatial variation existed. Concentrations of PCNs and PCDDs/PCDFs in sediments from the upper Detroit and lower Rouge Rivers ranged from 0.08 to 187 ng/g and 69 to 1420 pg/g dry weight, respectively. Total PCBs, PAHs, and NP concentrations ranged from 8 to 25,000, 17 to 44,000, and < 10 to 60,000 ng/g dry weight, respectively. Concentrations of all target compounds except PCNs were significantly correlated with total organic carbon content of sediments. Similarly, concentrations of PCBs, PCDDs, and PCDFs were significantly correlated with each other. The distribution of organic contaminants in the upper reaches of the Detroit River and lower Rouge River suggested the presence of localized, but multiple, sources of contamination for each compound class. Conners Creek combined sewer overflow has been identified as one of the potential sources for the upper Detroit River, where the highest concentrations PCBs and PCDDs/PCDFs were found. Polycyclic aromatic hydrocarbon and NP concentrations were consistently high in sediment from the lower Rouge River. Analysis of data from selected locations suggested that PCNs contributed a greater proportion of the dioxin-like activity than PCBs and PCDDs/PCDFs contributed.