Zeolites are microporous aluminosilicate materials with a wide range of applications including catalysis, water purification, agriculture, and laundry detergents. In the petrochemical industry, zeolites are used as catalysts in a process for the production of gasoline from crude oil, and more recently they have been explored as active catalyst material for the emerging biomass-derived fuels and chemicals production processes. In other words, these catalyst materials significantly impact the energy needs of our Nation. The catalytic performance of zeolites is determined by the number and nature of the acid sites, which are governed by the siting and zoning of aluminum within the zeolite framework. This location and distribution will furthermore affect the diffusion pathways of the reactants and products. This proposal therefore aims to determine the location and distribution of the Al atoms in a prototypical zeolite ZSM-5 material, using a combination of 3-D and in-situ methods unique to EMSL facilities and staff.