A combination of advanced characterization techniques: synchrotron X-ray micro- and nanotomography, micro-X-ray fluorescence, and micro-XRD have been used to characterize a commercial spent equilibrium fluid catalytic cracking catalyst (ECAT) at both the ensemble and individual particle level. At the ensemble level, X-ray microtomography was used to determine the average size, shape, and respective distributions of over 1200 individual catalyst particles. This information is important to determine performance in commercial operation. It is shown that a large fraction of the particles contained large internal voids (5–80 μm diameter), and these voids likely aid the accessibility for large hydrocarbon molecules. At the individual particle level, by using X-ray nanotomography, these voids were visualized at a much smaller scale (≈100 nm–12 μm in diameter). In addition, the individual phases that are present in the particle, for example, TiO2 and clay, are readily visualized in 3 D. Micro-X-ray fluorescence (XRF) was used to map, and semiquantitatively determine, both the contaminant (Ni, V, Fe) and inherent (La) catalyst elemental distributions. The distribution of zeolite Y in the ECAT particle was inferred from the La XRF map. Micro-XRD determined the lattice constant of the zeolite Y at the individual catalyst particle level. This in-depth characterization study at the ensemble and individual ECAT particle level presents a robust methodology that provides an understanding of the ECAT at both the micro- and nanometer scales.