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This study aimed to propose a mathematical method to investigate and optimize the simultaneous elimination process of multiple organic pollutants using the Fenton process. Hence, the treatment of rhodamine B (R and acid red 14 (AR14) dyes in their binary solution was studied. Multivariate curve resolution alternating least square (MCR-ALS), a novel chemometric method, was applied along with correlation constraints to resolute the UV-Vis spectrophotometric data, enabling quantification of investigated dyes despite a high spectral overl