Concrete is one of the largest wastes, by volume, generated during the decommissioning of nuclear facilities, which significantly influences the projected costs for the disposal of decommissioning wastes. Concrete consists of aggregates and a cement binder. In radioactive concrete, the radioisotopes are mainly associated with the cement component. If the radioactive isotope can be separated from the concrete to below the clearance criteria, the volume of radioactive concrete waste could be reduced effectively. We were studied to separate the radioactive materials from the concrete by using the thermomechanical and chemical treatment processes, sequentially. From the study, separated aggregate could be treated to achieve the clearance level. However, these processes generate a large volume of secondary acidic radioactive wastewater, which might be a critical problem to reduce the volume of radioactive concrete waste. In this research, separating the 137Cs and 90Sr from dissolved concrete wastewater to below the discharge criteria by precipitation method, it would be released to the environment under industrial waste guidelines. The experiments were conducted to using a simulated radioactive wastewater, formed by the dissolution of concrete within HCl, which was spiking the 137Cs and 90Sr, respectively. In addition, we applied the chemical precipitation methods with wastewater, using ferrocyanide for 137Cs and BaSO4 coprecipitation for 90Sr. As a result, targeted radionuclides could be removed to the discharge level (137Cs: 0.05 Bq·ml−1, 90Sr: 0.02 Bq·ml−1) by precipitation method. Therefore, it could reduce the secondary wastewater effectively by precipitation method and enhance the additional volume reduction for radioactive concrete waste.