The detection of unstable intermediates in chemical, photochemical, and radiation-chemical reactions can be greatly facilitated by the use of thermoanalytical methods. Special advantages are offered by differential thermal analysis (DTA), since it permits fast, easy investigation, from about -150 " C upward in some cases, over a wide temperature range. In this way processes that under normal conditions follow one another with immeasurable rapidity can be separated on the basis of their different temperature dependences. The great sensitivity of the method also allows the use of very dilute solutions, so that the studies can be confined to unimolecular processes.The value of the method for the determination of energetic and kinetic data is illustrated by its application to the photochemically obtainable, unstable, ozonide-like epidioxydihydrofurans.