Conventional microanalytical tools, particularly analytical electron microscopy (AEM), electron probe microanalysis (EPMA), and powder x-ray diffraction (XRD), have been traditionally used in the development of new engineering alloys to determine the identity of phases in new materials, their composition, phase equilibria, and the subsequent effect on properties. Recently, there has been a growing effort in industry to reduce the cycle time (and lower the cost) associated with new material development. This is particularly true for the advanced alloys needed for high-temperature components in power generation and aerospace application. This has led first to the development of more rapid screening methodologies, such as combinatorial approaches, where a large number of compositions can be evaluated in parallel, or the diffusion multiple method, where multi-component phase space is investigated in a single experiment. These new approaches require new analysis tools that can rapidly assess crystal structure and composition in automated fashion.