In order to assess the spatial distribution and the potential pollution risk of nickel (Ni) and vanadium (V) in Shuangtaizi Estuary in China, the water and the surface sediments were collected to determine V and Ni content in specified sites. The data indicated that the estuary was contaminated by Ni, while V content was low. Total concentrations of V in river water ranged from 0.212 to 0.374 μg/L, and in surface and bottom seawater from 0.214 to 0.559 μg/L and 0.231 to 0.684 μg/L, respectively. V content in river sediments ranged from 0.093 to 0.119 μg/g and in ocean sediments were 0.032 to 0.123 μg/g. Total Ni concentrations in river waters ranged from 23.667 to 118.667 μg/L, and in surface and bottom seawaters were 32.000 to 90.323 μg/L and 42.000 to 100.333 μg/L, respectively. Ni content in sediments of river ranged from 15.303 to 21.732 μg/g and in sediments of ocean were 11.197 to 21.107 μg/g. Ni content was higher than that of V. An ecological risk assessment study shows that Ni has potential ecological risk in water and no risk in sediment. V has no potential ecological risk in Shuangtaizi Estuary. V and Ni concentrations increased from the inner estuary to the outer estuary. The anthropogenic emissions from land are the main sources of Ni and V in the study area.