Versatile semi-batch apparatus for manometric measurement of gas-solid reaction rates

We describe the design, construction, operation, and performance of a simple and versatile semi-batch reactor that is especially useful for measurement of gas/solid reaction rates at pressures in the range of 1 mTorr to 1500 Torr. The reactor operates by repeatedly imposing small AC modulations of reactant gas pressure on top of a much larger DC pressure background. Based on the rate of pressure relaxation following each AC pulse, the reaction rate is determined. Our design is characterized by modular construction from off-the-shelf, ultra-high-vacuum-compatible components, which facilitate easy retrofitting and adaptation to a range of experimental conditions. Automated experiment control and data acquisition is accomplished via a custom National Instruments^© LabView virtual instrument. Data analysis is automated using a custom series of Mathworks^© Matlab scripts. We demonstrate reactor performance through measurements of hydrogenation kinetics for a composite H₂ getter material consisting of 1,4-bis(phenylethynyl)benzene mixed with a palladium/carbon catalyst.