The Rio Grande and its tributaries represent a critical water source for both the human population and the ecological resources of the Rio Grande drainage basin. Manadas Creek, an urban tributary of the Rio Grande, is located in an industrialized area of Laredo, Texas, where warehouses, a major railroad, and a decommissioned antimony (Sb) smelter are located. Previous studies have found that the creek water is contaminated with heavy metals such as Sb and arsenic (As). However, data on the metal distribution in this creek are very limited. Herein, water and sediment core samples were collected from six sites along the creek in February, April, and May 2008. Samples were analyzed for dissolved and total metals in water, total metals in sediments, and available (soluble-exchangeable, surface adsorbed, and organically bound) fractions of metals associated with the sediments. Results show that concentrations of Sb in the water and sediment samples were significantly lower at the upstream control site compared to the two sites located near the decommissioned smelter. Decreasing levels of Sb were found at the sites located downstream. The As levels in the sediment remained constant at different depths, whereas Sb varied significantly. A high level, 420 mg/kg, of sediment Sb was found at the maximum sediment depth of 35.0 cm sampled. In addition, 65.7-76.9% Sb and 80.3-85.6% As were in their residual form, 15.0-22.5% Sb and 6.2-11.4% As were bound to organic matter, and the remaining As and Sb were in the soluble and surface adsorbed fractions. Pearson correlation analyses indicated that the distribution of Sb was only moderately correlated to iron and nickel in the sediment and its correlation with the sediment properties measured was insignificant. Cluster analyses only grouped the two Sb isotopes together for the sediments collected in May, indicating that sources other than natural occurrence were associated with Sb. The high level of sediment Sb observed indicates that the sediment bed of Manadas Creek was acting as a holding reservoir for Sb and a potential source for the Sb level in the stream water. Thus, the loss of the sediment Sb and the Sb level in the water column must be closely related to the mobility of the bed sediments and the fate of the sediment-associated Sb.