Understanding the role of electronically nonadiabatic interactions during chemical reactions on metal surfaces in liquid media is of great importance for a variety of applications including catalysis, electrochemistry, and environmental science. Here, we report the design of an experimental apparatus for detection of the highly excited (hot) electrons created as a result of nonadiabatic energy transfer during the catalytic decomposition of hydrogen peroxide on thin-film metal-semiconductor nanodiodes. The apparatus enables the measurement of hot electron flows and related phenomena (e.g., surface chemiluminescence) as well as the corresponding reaction rates at different temperatures. The products of the chemical reaction can be characterized in the gaseous phase by means of gas chromatography. The combined measurement of hot electron flux, catalytic activity, and light emission can lead to a fundamental understanding of the elementary processes occurring during the heterogeneous catalytic reaction.