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This work evaluates the scope of alternative sources of iron i.e. Foundry Sand (FS), Fly Ash (FA) and mixture of FS and FA in heterogeneous photo-Fenton process for the degradation and decolourization of the dye Reactive Black5 (RB5). SEM-EDS characterization of FS and FA confirmed the presence of iron and aluminium which are required for photo-Fenton. In case of FS as an iron source, results confirmed the degradation and decolourization efficiency of 90% in 70 min and 45 min respectively when the reaction parameters were H2O2 = 2.2 mm, FS dose = 0.5 g, ph 3. With FA 90% degradation was achieved within 30 min and 93% decolourization rate within 15 min. When a mixture of FS (0.1 gm) and FA (0.05 gm) is used as source of iron 99% degradation and decolourization of the dye was achieved under the reaction conditions where H2O2 = 2.2 mm, FA:FS  = 1:2, ph 3.