A kinetic spectrophotometric method for the simultaneous determination of iodate and periodate in mixtures was proposed. The method was based on the reaction of periodate and iodate with pyrogallol red in sulfuric acid media. The reaction was monitored spectrophotometrically by measuring the decrease in absorbance of pyrogallol red at 470 nm. Kinetic data collected at 470 nm were processed by principle com ponent artificial neural network (PC–ANN) method. The constructed model was able to predict the concen tration of two species in the range of 0.1–15.0 and 0.1–17.0 μg/mL for iodate and periodate, respectively. The proposed method was applied to the simultaneous determination of iodate and periodate in several real sam ples with satisfactory results