A sensitive new measurement technology is described which combines calorimetry. gravimetry, and rheology applied to chemical reactions in thin films: quartz crystal microbalance/heat conduction calorimetry (QCM/HCC). The quartz crystal microbalance/heat conduction calorimeters constructed so far simultaneously measure heat generation, mass uptake or release, and viscoelastic property changes in the same, sub-milligram solid film sample when gases interact with the film in an isothermal surrounding. It is Possible to Measure the energetics of formation of a single layer of adsorbed molecules on a gold surface with this technique. The principles of operation of both the mass and the heat flow sensor are described, and one implementation of the combined sensor and apparatus and its electronics is presented. Methods for calibration and the preparation of thin sample films are summarized. As an illustrative example. the determination of the sorption enthalpy of hydrogen in a 25 degrees C palladium film of 140 nrn thickness is discussed in detail. Other examples of the operation of the QCM/HCC are tabulated. (c) 2005 Elsevier B.V. All rights reserved.