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The photocatalytic degradation of Acid Red 26 was examined utilizing a graphitic carbon nitride (g-C₃N₄) catalyst and a UV-A light in this study. We investigated how successfully the photocatalytic approach removed Acid Red 26 from synthetic and actual municipal wastewater. Both aqueous matrices allowed for extremely high clearance rates. Wastewater degraded at a slower rate than the other matrices, this might be ascribed to the wastewater’s complicated chemical composition. Using a liquid chromatography-mass spectrometry (LC-MS), the IPs in both synthetic and actual municipal effluent were determined. The photocatalytic degradation mechanisms of Acid Red 26 are hypothesised to comprise oxidation, dealkylation, and methoxy group cleavage based on the observed intermediate products (IPs). Using proven scavengers, we were also able to investigate the role of reactive species in the degradation process and illustrate the significance of h⁺ and O₂^• in the reaction. <i>Chlorococcum</i> sp. and <i>Dunaliella tertiolecta</i> microalgae were also utilised to assess the development of ecotoxicity. We observed low toxicity throughout the process when clean water was used as the matrix, with no production of hazardous IPs. In the case of actual municipal wastewater, there was an early rise in toxicity, which scientists believe was caused by the matrix’s chemical make-up. To lower the toxicity, a heterogeneous photocatalysis was used, and at the end of the treatment, nearly full detoxification was obtained.