We develop a fast analytical method for nickel-iron electrodeposition system. Due to the double working electrode nature characteristics of RRDE which can individually control ring and disk potential, we can evaluate the alloy composition and the stability of the plating bath. The content of the study includes : (i) Measurement of the Ni-Fe alloy partial current densities by stripping the deposited alloy on the disk. Part of the stripping charges are collected by the ring by oxidizing Fe(II) to Fe(III). With the concept of collection efficiency, one can calculate the individual reaction rates. (ii) Determine the complexation rate of the metal ions by stripping the disk nickel-iron alloy on the complexant-containing solution. We may evaluate the effects of various complexants on Fe(II) or Ni(II) and to find the method to improve the bath stability.