Methodology has been developed to separate nano-particles of amorphous material from Syncrude fine tailings. Both, separated finer solids and residual coarser solids, were characterized by elemental analysis, X-ray powder diffraction, XPS, SEM, infrared spectroscopy, solid-state NMR, density, and surface area measurements. Based on the results of infrared and X-ray diffraction, the amorphous minerals identified in finer solids included allophanes, halloysite, ferrihydrite, and amorphous silica. The finer fraction also contained some crystalline material consisting of muscovite and traces of quartz. The residual coarser solids consisted mostly of quartz, muscovite, and kaolinite.