Depending on the ambient environmental conditions, different gaseous species could get entrapped in uranium metal ingots or pellets. On heating, melting or vapourising uranium metal, these get released and depending on the composition, may cause detrimental effects either within the metal matrix itself or on the surrounding materials/environment. For instance, these gases may affect the performance of the uranium metal, which is used as fuel in the heavy water moderated research reactors, CIRUS and DHRUVA. Hence, detailed investigations have been carried out on the release of gases over a temperature range 875–1500 K employing hot vacuum extraction technique, in specimen uranium pellets made from uranium rods/ingots. Employing an on-line quadrupole mass spectrometer, the analysis of released gases was carried out. The isobaric interference between carbon monoxide and nitrogen at m/e = 28 in the mass spectrometric analysis has been resolved by considering their fragmentation patterns. Since no standards are available to evaluate the results, only the reproducibility is tested. The precision (relative standard deviation at 3s level) of the method is ±5%. The minimum detectable gas content employing the method is 5.00 x 10^-09 m³. About 4 x10^-04 m³/kg of gas is released from uranium pellets, with hydrogen as the main constituent. The gas content increases with storage in air.