The formation constants and the concentration of [M] and [MLi] in complex solutions of Ni2+ and Zn2+ with xylenol orange were determined by spectrophotometric method and principal component analysis. In this way, the spectral data were used to calculate the formation constants of complexes between ions Ni2+ and Zn2+ with xylenol orange using algorithm of principal component analysis (PCA) in DATAN. The concentration values of Ni2+ and Zn2+ in synthetic solutions resulting from this technique using xylenol orange (XO) at pH agree well with experimental data. This method can be applied to simultaneous determination of Ni2+ and Zn2+ in the industrial waste waters. | Simultaneous spectrophotometric determination of Zn2+, Ni2+ with xylenol orange in some industrial waters