This report presents data for samples of periphyton and water collected in 1995 and 1996 from Water Conservation Areas, the Big Cypress National Preserve, and the Everglades National Park in south Florida. Periphyton samples were analyzed for concentrations of total mercury, methylmercury, nitrogen, phosphorus, organic carbon, and inorganic carbon . Water-column samples collected on the same dates as the periphyton samples were analyzed for concentrations of major ions.