The properties of nanostructured films can be tailored by many factors such as composition, structure, preferred orientation, microstructure, interphase interface and grain boundaries. Compositional control of magnetic properties of recording media depends on the miscibility of constituent elements. However, for nanostructured materials with a large surfaceto-volume ratio of atoms, the miscibility at the nanoscale may not necessarily follow the prediction of conventional phase diagram that does not consider the effects of surface and interface. This limitation further complicates the prediction of phase separation at grain boundaries and interphase interface. Using anomalous x-ray scattering, the alloying and composition of a specific long range order of textured nanostructured films has been investigated. Such information may not be readily available from conventional characterization techniques.