The short-range order in liquid binary Al-rich alloys (Al-Fe, Al-Ti) was studied by x-ray diffraction. The measurements were performed using a novel containerless technique which combines aerodynamic levitation with inductive heating. The average structure factors, S(Q), have been determined for various temperatures and compositions in the stable liquid state. From S(Q), the pair correlation functions, g(r), have been calculated. The first interatomic distance is nearly temperature-independent, whereas the first-shell coordination number decreases with increasing temperature for all the alloys investigated. For the Al-Fe alloys, room-temperature scanning electron microscropy (SEM) studies show the formation of a microstructure, namely the existence of Al(13)Fe(4) inclusions in the Al matrix.