In this paper, a sealed in-situ reaction system and infrared spectroscopy (IR) were used to study the gas releasing mechanism of 2,6-diamino-3,5-dinitropyrazine-1-oxide (LLM-105) at different temperatures. Three characteristic stages of LLM-105 during the heating process to 400°C were detected by the moving-window two-dimensional correlation spectroscopy (MW2D). Two-dimensional correlation infrared spectroscopy (2DCOS) was employed to examine changes of gas concentration in the sealed system at each stage. We found that in the first stage, LLM-105 first released H 2 O and NH 3 . In the second stage, the decomposition is intensified, the explosive molecule first undergoes the decomposition reaction of releasing H 2 O, and CO 2 , subsequently chemical reaction producing several nitrogen gases, such as NO, N 2 O, HCN, NO 2 and NH 3 . In the third stage, the decomposition process mainly releases CO 2 and NH 3 , and the concentrations of HCN and NO 2 decreased gradually. 2DCOS proven to be a very sensitive method for detecting thermal decomposition mechanisms and monitoring gas changes in sealed system.