In this study, we introduce the validation of the analysis guidelines through preliminary experiments of the draft analysis guidelines before analyzing waste materials (non-combustible). This validation data was applied the accuracy and efficiency of the separation and analysis for the waste such as steel generated from NPP. Steel (non-flammable) was leached the mixed acid and the leaching solution was separated by using the separation guidelines. Steel was corroded with radioactive RM (Co-60, Cs-137) and mixed acid. After drying, the corroded steel was measured the initial radioactivity by a HPGe detector (10,000 seconds). The sample was inserted in a beaker and leached with mixed acid (10 M HNO3 + 4 M HCl) for 2 hours. In this solution, it added 2 ml of H2O2 to increase the leaching effect. The ultrasonic device was adjusted so that the temperature does not exceed 60°C. After elution, the surface of the sample was washed with pure water. The weight of the sample was measured accurately, and recorded the weight loss rate after infiltration. The leaching sample was measured radioactivity by a HPGe detector (10,000 seconds). It was calculated the recovery rate based on the difference in total radioactivity before and after leaching. Before the test, radioactive RM (Co-60, Cs-137) was radioactive deposited by corrosion, but Cs- 137 was not detected in the initial gamma measurement and only Co-60 nuclides were deposited. The recovery rate test results were confirmed to be about 100%.