Concentrations of total mercury and methyl mercury were determined in sediment and fish collected from estuarine waters of Florida to understand their distribution and partitioning. Total mercury concentrations in sediments ranged from 1 to 219 ng/g dry wt. Methyl mercury accounted for, on average, 0.77% of total mercury in sediment. Methyl mercury concentrations were not correlated with total mercury or organic carbon content in sediments. The concentrations of total mercury in fish muscle were between 0.03 and 2.22 (mean: 0.31) ??g/g, wet wt, with methyl mercury contributing 83% of total mercury. Methyl mercury concentrations in fish muscle were directly proportional to total mercury concentrations. The relationship of total and methyl mercury concentrations in fish to those of sediments from corresponding locations was fish-species dependent, in addition to several abiotic factors. Among fish species analyzed, hardhead catfish, gafftopsail catfish, and sand seatrout contained the highest concentrations of mercury. Filtered water samples from canals and creeks that discharge into the Florida Bay showed mercury concentrations of 3-7.4 ng/L, with methyl mercury accounting for <0.03-52% of the total mercury. Consumption of fish containing 0.31 ??g mercury/g wet wt, the mean concentration found in this study, at rates greater than 70 g/day, was estimated to be hazardous to human health.