Sediment samples were collected from the lower Calcasieu River and estuary, Louisiana, in a study of the release of metals from sediments to the overlying water column. Whole samples were characterized by analyses that included: (1) determination of total sediment ammonium concentrations; (2) determination of total sediment Cr, Mn and Fe concentrations; (3) extraction of sediment with hydrogen peroxide followed by dilute hydrochloric acid to obtain recoverable metals, including oxides; and (4) extraction of sediment with hydrogen peroxide plus pyrophosphate at a pH of 7-8 to recover organically-bound Cr but not metal oxides. Concentrations of Cr, Mn and Fe in sediment interstitial water were determined. The concentrations of Cr in interstitial water could not be predicted from total sediment concentrations of Cr. Degradation of organic matter appeared to be the mechanism that caused elevated Cr concentrations in the interstitial water. Concentrations of Cr in interstitial water were positively correlated with total concentrations of ammonium in sediment. Concentrations of Cr in interstitial water that exceeded water-column concentrations of Cr were found when the total concentrations of ammonium in sediment exceeded 1 ??mol per gram wet weight. Concentrations of metals in interstitial water that are larger than metal concentrations in the water column create a potential for diffusive flux and metal enrichment of the overlying water column. ?? 1994.