The chemical composition of bottom sediments and their associated pore waters from the tidal Potomac River and Estuary was studied from May 1978 through June 1980. Pore waters were routinely analyzed for pH, Eh, alkalinity, and concentrations of sulfide, sulfate, phosphate, carbon, ammonium, silica, iron, manganese, chloride, sodium, potassium, calcium, and magnesium. Porosity, weight loss on ignition, and carbon, nitrogen, and phosphorus contents were determined for the solid sediments. The range of salinity and chemical composition encountered in the estuary frequently necessitated modifications of standard methods of analysis. Therefore, the methods used, their modifications, and their limitations are presented in some detail. The appendix lists the data obtained from six sampling periods. (USGS)