Radionuclide analysis methods must be secured in the event of emergencies such as the discovery of unknown nuclear material or nuclear accidents in neighboring countries or Korea. Most institutions in Korea are in their early stages of radionuclide analysis method development and do not even have Radiation Controlled Areas where they can handle the samples safely. Some institutions such as the Korea Atomic Energy Research Institute have the ability to perform radionuclide analysis for nuclear facilities or verification of nuclear activities. In Korea, it is necessary to secure nuclide analysis technology to enable independent verification in times of emergency or need. This paper analyzes uranium as the target nuclide using alpha spectrometer and TIMS. Alpha spectrometer detects alpha particles emitted from uranium samples and measures the concentration of uranium isotopes. This method has a high selectivity that distinguishes it from other elements, and accurate measurements can be made even when uranium samples are mixed with other elements. In addition, there is minimal interference from other radioactive isotopes in the sample, and the sample preparation is simple, resulting in relatively short analysis times. In contrast, TIMS detects ionized uranium ions by heating the uranium sample. This method may have potential interference from other elements and may take relatively longer analysis times. However, TIMS has high sensitivity and accuracy and can detect various elements other than uranium, making it suitable for various analyses. Therefore, when analyzing uranium, it is recommended to select and use the appropriate device according to the purpose, as both alpha spectrometer and TIMS have their pros and cons. Furthermore, by using both devices in parallel, more accurate and reliable results can be obtained. This paper aims to compare the analysis methods of alpha spectrometer and thermal ionization mass spectrometry, which are widely used for nuclide analysis in unknown nuclear materials.