The simultaneous determination of cobalt,copper and nickel using 1-(2-thiazolylazo)-2-naphthol (first figure of this article) by spectrophotometric method is a difficult problem in analytical chemistry,due to spectral interferences.By multivariate calibration methods,such as partial least squares (PLS) regression,it is possible to obtain a model adjusted to the concentration values of the mixtures used in the calibration range.Orthogonal signal correction (OSC) is a preprocessing technique used for removing the information unrelated to the target variables based on constrained principal component analysis.OSC is a suitable preprocessing method for PLS calibration of mixtures without loss of prediction capacity using spectrophotometric method.In this study,the calibration model is based on absorption spectra in the 550-750-nm range for 21 different mixtures of cobalt,copper and nickel.Calibration matrices were formed from samples containing 0.05-1.05,0.05-1.30 and 0.05-0.80 μg mL-1 for cobalt,copper and nickel,respectively.The root mean square error of prediction (RMSEP) for cobalt,copper and nickel with OSC and without OSC were 0.007,0.008,0.011 and 0.031,0.037,0.032 μg mL-1,respectively.This procedure allows the simultaneous determination of cobalt,copper and nickel in synthetic and real samples and good reliability of the determination was proved.