The photocatalytic activity of four titanium dioxide samples (TiO2-P25 Degussa, PC105 Millennium, PC500 Millennium, and Anatase) was studied in the degradation of dyes (Congo Red (CR), Methyl Orange (MO), and Direct Red 23 (DR23)) using cost-effective smartphone-based analysis. The obtained kinetic curves are well described by the first-order kinetic model. It was established that the phase composition, the size of the particles, and the specific surface area of ​​the catalyst have a significant effect on the photocatalytic activity of the studied TiO2 samples. It was investigated that the Millennium PC500 sample is the most effective photocatalyst due to a large specific surface area and a small particle size (8 nm). TiO2-P25 Degussa and Anatase also demonstrate a high photocatalytic activity in the degradation of CR and DR23 dyes, which can be explained by the accelerated process of electron transfer between the anatase and rutile phases. For the PC105 sample, a higher CR photodegradation efficiency is observed compared to PC500. It can be concluded that heterogeneous photocatalysis is an effective method for the removal of toxic dyes from wastewater. With the use of smartphone-based analysis, it is possible monitoring the photodegradation kinetics in real-time.