A dynamic FT-IR method was used to determine the individual curing temperature ranges of the isoimide-imide isomerization and crosslinking reactions of an acetylene-terminated polyisoimide prepolymer. The individual curing temperature ranges of these two types of chemical reactions for the polyisoimide system using differential scanning calorimetry (DSC) were totally overlapped. Using dynamic FT-IR spectroscopy, the curing temperature ranges of the isomerization and crosslinking reactions were clearly separated. The isomerization reaction began at lower temperatures than the crosslinking reaction and was complete when only half of the crosslinking reaction had occurred. The temperature width, Delta T-1/2, was twice as great for the crosslinking reaction compared with the isomerization reaction. Activation energies from dynamic FT-IR spectroscopy can be obtained for the two separate reactions, however, for the reactions considered here, the activation energies were similar, 26 kcal/mol for the isomerization reaction and 23 kcal/mol for the crosslinking reaction.