The Korea Research Institute of Standards and Science has developed certified reference materials (concrete, soil, and metal radioactive liquid) for measuring gamma-emitting radionuclides to improve and maintain the quality assurance and quality control of the radioactivity measurement in decommissioning nuclear power plants. The raw materials that make up each CRM were mixed in an appropriate ratio with radionuclides. For certification and homogeneity assessment, 10 bottles were randomly selected, two sub-samples were collected from each bottle, and radionuclides were measured via HPGe gamma spectrometry. The results of the homogeneity tests using a one-way analysis of variance on the radionuclides in the CRMs fulfilled the requirements of ISO Guide 35. Coincidence summing and self-absorption correction were performed on measurement results by introducing the Monte Carlo efficiency transfer code and Monte Carlo N-Particle transport code. In concrete analysis, the reference values for five radionuclides (60Co, 241Am, 134Cs, and 137Cs) in the CRM were in the range of 15-40 Bq/kg, and the expanded uncertainty was within 10% (k = 2). In soil analysis, the reference values for the 137Cs and 60Co were 118.7 and 124.4 Bq/kg, and the expanded uncertainty was within 10% (k = 2). In metal radioactive liquid analysis, the reference values for 134Cs, 137Cs and 60Co in the CRM were in the range of 200-270 Bq/kg, and the expanded uncertainty was within 7% (k = 2).