The primary objective of this research is to propose and compile a specific protocol for photocatalytic measurements of modified TiO2 particles under visible-light irradiation. Nitrogen-modified titanium dioxide (N-TiO2) powder was synthesized by the sol–gel method and characterized by X-ray Diffraction Analysis (XRD), Field Emission Scanning Electron Microscopy (FESEM), Transmission Electron Microscopy (TEM), X-ray Photoelectron Spectroscopy (XPS), Raman Spectroscopy (micro-Raman), and Ultraviolet–visible Spectroscopy (UV-Vis). Photocatalytic tests were performed on a specially designed photocatalytic batch reactor to test the ability of the powder to degrade hazardous toxic compounds. Via the Taguchi method, nine experiments (L9) were compiled to examine the factors that affect the photocatalytic activity of the nano-sized powder. The N-TiO2 particles were characterized by the dominance of the crystalline anatase phase, exhibiting crystals in the nano-scale. The Taguchi method was designed to control four selected parameters (pollutant selection among azo dyes, amount of catalyst to pollutant, distance of the photocatalytic cell from the radiation source, and time protocol) with three levels/options each. Conclusions were drawn regarding the way each parameter affects the final degradation of the pollutant. The parameter that proved to affect the degradation of the pollutant to a greater extent was the choice of pollutant, followed by the amount of catalyst. The other two factors almost slightly affect the process, with a similar percentage. Taking into account the abovementioned results, a photocatalytic protocol for testing TiO2 nano-powder activity under visible light irradiation is proposed by using a batch, horizontal, rectangular, vis-LED equipped reactor with reflective walls.