The purpose of this research is to examine local atomic order in several metallic alloy systems that display a metastable transitional state. Early stages of homogeneous precipitation is examined in aluminum-copper-magnesium, iron-beryllium and nickel-beryllium alloys. Precipitation from nickel-aluminum alloys is studied to better understand formation of ordered precipitates. The structure of ferrous martensites immediately following the quench is being determined; structural changes from tempering is also pursued. Local atomic order in mercury- cadmium-telluride is being determined using synchrotron anomalous dispersion techniques. Advanced X-ray diffraction methods are the primary experimental tool used to characterize the alloy systems. Advanced diffuse X-ray scattering techniques from atomic displacements and the associated analysis are part of the research.