Amorphous Ti-Ni alloys may be prepared by a variety of techniques, including: liquid quenching, ion implantation, electron irradiation, and vapor synthesis. Each of these techniques involves fundamentally different atomic processes with concomitant different effective quench rates. Since quench rates affect the degree of structural order, it is conceivable that a variety of metastable configurational states may thus result. Radial distribution functions (RDF’s) from diffraction experiments are a generally accessible probe for statistical characterization of amorphous alloys, and hence, a useful tool to compare amorphous structures. However, not all of the amorphization methods are capable of producing sufficient quantities of material required for x-ray or neutron scattering. Therefore, the purpose of this paper is to report the preliminary results from a comparative structural investigation of Ti-Ni alloys by x-ray and electron diffraction.