Abstract:A new method based on spectrophotometric-partial least-squares procedure was proposed for simultaneously determination of thorium and zirconium using SPADNS (4,5-Dihydroxy-3-(p-sulfophenylazo)-2,7-naphthalene disulfonic acid, trisodium salt) as a color reagent. Absorbance measurements were made in the range of λ = 541÷620 nm with 1.0 nm steps in buffered solutions at pH 3.5. The linear ranges were obtained for 0.5÷11.5 and 1.5÷14.5 µg cm -3 for Th 4+ and Zr 4+ ions, respectively. The limits of detection were determined 0.4 and 1.2 µg cm -3 for thorium and zirconium, respectively. The standard deviation (n = 3) and recovery percent of 10 samples in the prediction set were obtained in the amplitude 0.22÷0.38 µg cm -3 and 91.3÷109.2, respectively. The proposed method was used for simultaneously determination of mentioned ions in spiked real water samples and wastewater. The results show that the method is applicable for the analysis of samples with similar matrix.