Differential scanning calorimetry (DSC) was used, we believe for the first tlme, for compositional analyses of a compound semlconductor. The Cd-Te system electrosyntheslzed by a cathodlc route was used as a model to deflne the limits and power of thls analytical tool. Thus changes in the composltlon of the electrodeposited material were monltored as a function of deposition potential. Samples deposited at potentials 2-600 mV (vs SCE) contained excess Te in addition to CdTe and those synthesized at -696 and -698 mV contained both excess Cd and Te. The composition switched abruptly to a large excess of Cd near 700 mV. The excess Cd and Te were detected and quantitated by their characteristic DSC signals at 318 and 447 OC, respectively. Changes in compositional profiles as a function of solution hydrodynamics and TeO, concentration as well as chemical reactlons between the excess Cd and Te are described.