This study performed to extract operation factors of major organic wastes, which were food wastes and waste activated sludge generated in industries in order to use them as a substrate for bio-H2 production. According to the results of experimental analysis for hydrogen production capacity by various organic concentrations, the hydrogen production yield was the highest at 80 g/L, and the efficiency was improved by the pretreatment of waste activated sludge (acid treatment, alkali treatment). Hydrogen production efficiency was improved by mixing food wastes and waste activated sludge if waste activated sludge was below than 30%, however, it was decreased when it was more than 50%. The impacts of heavy metals on the hydrogen production shows that the inhibition level depends on the concentration of Cr, Zn, and Cu, Fe was able to enhance the hydrogen production.