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The photo‐Fenton degradation of a highly chlorinated aromatic solvent, 1,2,4‐trichlorobenzene (124‐TCB), for conditions of natural pH and using a Vis‐LED as the radiation source is presented. A D‐optimal design combined with response surface methodology (RSM) was combined to simultaneously evaluate the effect of the main reaction variables: hydrogen peroxide concentration (HP), iron dosage (Fe), and radiation level (Rad), on 124‐TCB conversion. It was found that the photo‐Fenton process is effective in the degradation of the chlorinated solvent employing a Vis‐LED source when ferrioxalate is used as the catalyst source. Operating the system with high radiation levels (I=0.15Wcm‐2 ), the conversion of 124‐TCB after 180 min of the reaction was higher than 75% over the full range of working HP and Fe concentrations. Being maximum (96.24 %), the obtained for conditions of Fe=5 ppm and HP=305 ppm.
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