Longitudinal recording media have shown remarkable longevity in the fast-paced computer hardware industry. While a variety of factors have contributed to the continued dominance of such magnetic hard disks, the role of atomic segregation to the grain boundaries has proven tantamount to their success [1]. Further decreasing grain size past the approximately 10 nm in current media would hasten the detrimental effects of thermal fluctuations. Therefore, the ability to shield neighboring grains by segregation of nonmagnetic species becomes of heightened interest. High resolution transmission electron microscopy (TEM) and nanoprobe x-ray energy dispersive spectroscopy (EDS) is clearly an important technique in characterizing these small-scale microstructures.