A sensitive derivative adsorption chronopotentiometric method was developed to determine trace amounts of Fe3+. The influence of preconcentration time, pH of solution and constant reducing current of the peak height is discussed. The detection limit and the linear range are 5.0 × 10−10 and 2.0 × 10−9∼3.0 × 10−6 mol L−1, respectively. The method was used to determine trace Fe3+ in KH2PO4 crystals (KDP).