The United States Congress enacted the Comprehensive Environmental Response, Compensation, and Liability Act (CERCLA), commonly known as the Superfund, in 1980, with the purpose of dealing effectively with the dangers posed by the nation's hazardous waste sites (HWS). In this research, we evaluated lead levels in soil, sediment, and surface water collected from selected locations near a HWS in Mississippi, and estimated the potential ecological health risk associated with the presence of lead in these environmental matrices. Monthly samples were collected for a period of 12 months, at four different stations selected with respect to the HWS, and analyzed for their lead content by AA or UWVisible spectrometry following a sample preparation by microwave -assisted acid digestion, or by mild digestion on hot plate. Other physical and chemical parameters including BOD, COD, conductivity, DO, nitrate, pH, sulfate, temperature, TDS, TSS, and turbidity were also assessed. Levels of lead in soil, sediment, and water collected from the sampling site (Site 1) closest to the controlled HWS were significantly higher (p < 0.05) than the other three sampling sites. While lead levels in soil and sediment were found to fall below the screening level (500 mg/kg), its concentrations in water samples exceeded the required criterion (3.2 ug/L) set by EPA for protection of aquatic life from chronic toxicity. No significant difference was found in the values of nitrate, pH and temperature at the 4 sampling sites; however, there were significantly (p < 0.05) lower levels of DO, and higher levels of BOD, COD, conductivity, sulfate, TDS, TSS, and turbidity, at Site 1 compared with Sites 2, 3, and 4.