Heterogeneous photocatalysis, using photocatalysts in suspension to eliminate diverse contaminants, including textile wastewater, has several advantages. Nevertheless, current absorbance and decolorization measurements imply sample acquisition by extraction at a fixed rate with consequent photocatalyst removal. This study presents online monitoring for the decolorization of six azo dyes, Orange PX-2R (OP2), Remazol Black B133 (RB), Procion Crimson H-EXL (PC), Procion Navy H-EXL (PN), Procion Blue H-EXL (PB), and Procion Yellow H-EXL (PY), analyzing the spectrum measured in situ by using the light scattering provided by the photocatalyst in suspension. The results obtained have corroborated the feasibility of obtaining absorbance and decolorization measurements, avoiding disturbances in the process due to a decrease in the volume in the reactor.