Investigation of the formation of new metastable phases in alloy thin films requires ways of quickly determining the crystalline structure of samples with different compositions. We report a novel technique for acquiring structural information from films intentionally grown with a composition gradient. For example, binary metal alloy films were deposited using a phase-spread sputtering method. In this way essentially the entire composition range could be grown in a single deposition. By using a narrow incident x-ray beam and a translating sample stage combined with a position sensitive x-ray detector technique, detailed information of the metastable phase diagram can be obtained rapidly. Compositional resolution of the order of ±0.2% can be achieved, and is limited by the brightness of the x-ray source. Initial results from studies of phase formation in Zr-Ta alloys will be presented. Extensions of the analysis technique to ternary systems will be discussed.