Two methods for the simultaneous determination of ascorbic acid (Asc) and L-cysteine (Cys) from kinetic spectrophotometric data are described and compared. The first is the two-rate method (TRM), and the second, the differential kinetic method (DKM). Present in an excess amount, iron(III) is quantitatively reduced by Asc or Cys to iron(II) that, in turn, interacts with phenanthroline (Phen) to form a colored product, representing a Fe(II) -Phen complex that possesses a maximum absorbance at l max = 510 nm. The first method is based on the measurement of reaction rates at two points in the course of successive reactions, and the second method is based on the difference in kinetics of the Asc and Cys oxidation reactions at different pH values. Both oxidation reactions have been studied by fitting the kinetic curves (absorbance versus time) to suitable reaction rate equations. It is established that the Cys + Fe(III) reaction obeys simple first-order kinetics, while the Asc + Fe(III) is a successive two-step process. Under the conditions studied, both Asc and Cys are determined in the 0.5 -5.0 ppm range with satisfactory accuracy. The two methods under consideration have been successfully used for the analysis of model and real samples. The RMSEP values for the determination of Cys and Asc by the two kinetic methods (TRM, DKM) are 0.121, 0.120 and 0.131, 0.303 and the corresponding REP values are 5.15, 5.12% and 5.18, 11.98%, respectively. 44 0091-150X/06/4001-0044