TA-MS is also used for the characterization of solid state reactions taking place in high temperature materials. For this purpose high temperature coupling systems are preferred. Starting from a historical survey of the evolved gas analysis the technical prerequisites are described more in detail (requirements to the coupling systems and current trends in methodology). Applications in the high temperature range (carbothermal reduction of TiO2, outgassing and sintering of hard metals) demonstrate the advantages and limitations of such techniques.