In this work we found that there were five decomposition products of di-t-butyl peroxide at 320 degrees C by GC-MS. The peak area of acetone as a chief product in the thermal decomposition was related to di-t-butyl peroxide concentration in a linear manner. The range was from 22.91 to 114.93 microg (r=0.9997, n=4). By use of the calibration, we can possibly determine the content of the peroxide rapidly. The present method is more suitable for the determination of peroxide that is liable to decompose and difficult to be vaporized.