"“Operando” studies of catalyst surfaces under reaction conditions have emerged recently as a very valuable tool for improving catalysts for energy applications and exhaust purification. In particular, synchrotron-based near-ambient-pressure photoelectron spectroscopy (NAP-XPS) enables detailed studies of oxidation behaviour and other changes of the catalyst material under the influence of the reactants. This new method will be available at a new beamline of Diamond Light Source, which is the first purpose-built instrument for operando studies in the UK with strong participation of UoR. . The aim of the project is to synthesise a range of new bi-metallic heterogeneous catalysts for hydrogen fuel and syn-gas production from natural gas and to systematically apply NAP-XPS (using the beamline at Diamond). The application of synchrotron techniques allows a more detailed understanding of the chemistry of the active system than is possible with other techniques and will provide unique information about the chemical nature of the nanoparticle surface region and correlate the catalyst activity/selectivity with surface state and characterise surface intermediates.