The simultaneous spectrophotometric method is described for the determination of Cu(II) and Co(II) by 5-bromosalicylaldehyde thiosemicarbazone (5-BSAT) using partial least squares regression method. .cm −1 , respectively. Partial least squares (PLS) regression method is proposed for the simultaneous determination of these ions with the spectrophotometric absorbance data between wavelengths 370 and 446 nm at an interval of 4 nm. A training set was generated and its accuracy was tested in a test set. The test set garnered a root mean square error (RMSE) of 0.192 for copper and 0.489 for cobalt. The relatively small RMSE suggests only a small difference between predicted versus measured concentrations, demonstrating the accuracy of our model. The proposed method is successfully employed in the analysis of water sample for determining concentrations of copper and cobalt.