Isotachophoresis was applied to the quantitative analysis of phosphorus in Ni-P and Co-P alloy deposits, thereby increasing the speeding of analysis. Sample fimls were dissolved in a solution of 40%HNO3 and the solution was demineralized by electrodialysis using an ion-exchange membranes. This pretreatment redurced the timer equired for analysis to less than 1 hour. Isotachophoresis resulted in higher accuracy and reproducibility than could be obtained with other analytical methods, and it is also applicable to the analysis of boron in such alloy deposit films.