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The degradation of the antibiotic thiamphenicol has been studied by photoelectro-Fenton (PEF) process with UVA light using pyrite particles as catalyst source. Pyrite is a sulfide mineral that naturally acidifies the reaction medium and releases Fe2+, thus promoting the effective generation of OH from Fenton's reaction. The assays were made in an IrO2/air-diffusion cell, which yielded similar results to a boron-doped diamond (BDD)/air-diffusion one at a lower cost. In dark conditions, electro-Fenton (EF) process showed an analogous abil