ABSTRACT. In this study, optimisation of the photocatalytic behaviour of crystal violet (CV) by thiourea (Tu)-codoped TiO2 thin film in fixed bed photoreactor was investigated by central composite designs (CCDs). The effective variables were pH, the concentration of CV dye, flow rate and reaction time. The results of the CCD model showed a good agreement with experimental results, with R 2 = 0.9680 (p < 0.0001) and maximum degradation efficiency was obtained at the optimum conditions: dye concentration 8.5 mg/L, pH 9, flow rate 6 mL/min and reaction time 80 min. Subsequently, three absorbing chemical compounds presented in the degradation reaction were obtained by using singular value decomposition (SVD) method and evolving factor analysis (EFA). Then a multivariate curve resolution with alternating least squares (MCR-ALS) was performed to achieve the concentration and spectral profiles for each component. Finally, a hard modelling method was applied to determine the kinetic constants of distinct reactions occurred in the photocatalytic degradation process. The reaction rate constants were calculated for the first and second steps as k1 = 0.08327 (SD = ±0.0015) /min and k2 = 0.045 (SD = ±0.0006)/min, respectively.