Preferred orientation has long been considered the primary source of systematic error involved in quantitative analysis by X-ray powder diffraction. Techniques of spherical agglomeration have been shown to eliminate preferred orientation provided that the agglomerate size is made sufficiently larger than the particle size. These techniques invariably employ the surface energy minimization of a liquid phase dispersed within a second fluid to create the spherical form desired. Spray drying has been the only method to date which has been successfully used to prepare spherical agglomerates suitable for X-ray diffraction. This study was undertaken to investigate possible deleterious effects of spray drying as a diffraction sample preparation technique.