Powders of Al and Ti were blended and compacted, the compact then melted in an attempt to produce single phase Al3Ti. Optical microscopy of the cast and homogenized specimen revealed an almost single phase microstructure with minor amounts of a second phase. The composition of the matrix was measured using fully quantitative energy dispersive X-ray analysis. By use of X-ray diffractometry, the interplanar spacings and the associated integrated peak intensities were experimentally measured for the binary DO22 compound, Al3Ti. Using standard structure factor equations, the intensities were calculated for the various reflections. Good agreement was obtained between calculated and observed intensities.