The combination technique of thermal analysis—flame ionization detection (TAFID) offers attractive new possibilities for the precise measurement of the volatilization patterns of a wide variety of organic materials. Advantages over other methods are due chiefly to the sensitivity, specificity, and small sample requirement of the flame detector. Essential features of apparatus design are a close coupling of the detector to the sample furnace and provision for operating the detector at high temperatures in order to avoid condensation and thus allow quantitative measurements. Advances that have been made in instrumentation of the system provide speed and convenience. Recent improvements in techniques and apparatus will be discussed. The wide applicability of this approach to thermal analysis will be illustrated by a number of methods developed for specific purposes, including the characterization of various polymers, oils, bitumens, rubber compositions, and other organic materials.