X-ray photoelectron spectroscopy (XPS) is one of the most powerful techniques for studying the chemistry at the surface of materials. However, it can only operate under vacuum conditions, far from the cycling pressures of hydrogen storage materials. Even ambient pressure XPS (often referred to as high-pressure XPS) cannot ever reach these sorts of pressures. Instead, we will adopt a novel method for moving a sample between the ultra-high vacuum XPS chamber and a reaction chamber where the materials can be subjected to the hydrogen pressures and temperatures required for hydrogen storage to undergo one or more cycles. The sample is then rapidly returned to the XPS chamber to perform core-level measurements to determine any chemical changes. In this way we can explore degradation mechanisms, the effects of impurities, and other irreversible reactions. Because the material never leaves the instrument, changes can be directly correlated to the cycling process.