This article proposes a novel technology combining electrochemical and ultrasonic methods to produce nanoscale zero valent iron (NZVI). With platinum placed in the cathode and the presence of the dispersion agent, 0.2g/l cetylpyridinium chloride (CPC), a cation surfactant, in the solution, the nanoscale iron particle was successfully produced with diameter of 1–20 nm and specific surface area of 25.4m2/g. The produced NZVI was tested in batch experiments for nitrate removal. The results showed that the nitrate reduction was affected by pH. Al low pH, nitrate was shown faster decline and more reduction in term of g NO3−–N/g NZVI. The reaction was first order and kinetic coefficients for the four pHs were directly related to pH with R 2 >0.95. Comparing with microscale zero-valent iron (45μm, 0.183m2/g), microscale zero-valent iron converted nitrate to ammonia completely, but NZVI converted nitrate to ammonia partially from 36.2 to 45.3% dependent on pH. For mass balance of iron species, since the dissolved iron in the solution was very low (<1mg/l), Electron Spectroscopy for Chemical Analysis (ESCA) was used for identification of oxidation state of the surface species on the NZVI and Fe2O3 was recognized. Thus the reaction mechanisms can be determined.