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In this paper, we studied treatment of mixture of three azo dyes using homogeneous photoelectro-Fenton (PEF) combined with heterogeneous photocatalytic process (UV/TiO₂). Carbon nanotube immobilized onto graphite plate (CNT/graphite) electrode was used as cathode. The investigated photocatalyst was TiO₂ nanoparticles (Degussa P25) immobilized on glass plates. A rapid analytical methodology based on recording UV–Vis spectra during the photoelectro-Fenton/photocatalytic decolorization process and the data treatment using multivariate calibration methods such as partial least square (PLS) was developed. The three textile dyes (C.I. Acid Yellow 36 (AY36), C.I. Acid Red 14 (AR14) and C.I. Basic Yellow 28 (BY28)) were quantified simultaneously despite the overlap of their spectra. Also, the central composite design has been employed to the optimization of photoelectro-Fenton/photocatalytic …