This research involves an experimental investigation of the thermodynamics of nanophase materials. Mechanical attriting is the technique employed to process various nanophase metallic systems. Associated effects of environmental factors during attriting are determined. Both positive and negative heats of mixing are represented in the materials' systems proposed. Grain boundary segregation tendencies are noted and related to the potential for grain growth during low temperature annealing and consolidation. Several experimental characterization methods are proposed to examine the chemistry on a nanoscale, including calorimetry, electron energy loss spectrometry (EELS), Mossbauer spectrometry, and small angle X-ray scattering (SAXS). %%% Nanostructured materials are a class of new materials whose properties are expected to be markedly changed by the consequences of the fine structure. This research explores factors affecting the stability of such materials.