Multicomponent nanoparticles containing two or more different types of functionalities show unique physical and chemical properties, leading to significantly enhanced performance. In this study, we have developed a new one-pot method to prepare Fe/FeS nanoparticles using dithionite at room temperature. The FeS precipitates on the Fe surface are formed by the interaction between dissolved iron species and hydrogen sulfide, one of the decomposition products of dithionite in solution. The resulting Fe/FeS nanoparticles have high surface area, good electrical conductivity, and strong magnetic responsivity. In addition, the Fe/FeS shows a much higher reactivity toward contaminants than the pure Fe nanoparticles. The above synthesized nanoparticles are successfully applied for the rapid removal of trichloroethylene (TCE) from water. The study reveals that Fe/FeS nanoparticles are a promising candidate for the efficient removal of pollutants.