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As new alloys are being developed for additive manufacturing (AM) applications, questions related to the temperature-dependent structural and compositional stability of these alloys remain. In this work, the benefits and limitations of a unique method for testing this stability are presented. This system employs the use of polychromatic synchrotron light to perform energy-dispersive x-ray diffraction (ED-XRD) on an electrostatically levitated sample at high temperatures. In comparison with a traditional angular-dispersive setup, the container-less electrostatic levitation method has unique advantages, including quicker acquisition times, simultaneous compositional information through fluorescence emissions, a reduction in background noise, and, importantly, concurrent/subsequent measurement of thermophysical properties. This combined method is ideal for phase transition studies by holding the levitated sample at a stable position and temperature through controlled heating and temperature management. To illustrate these capabilities, we show ED-XRD data of the well-known martensitic phase transition (hcp to bcc) in Ti–6Al–4V. In addition, results from the novel alloy Ni51Cu44Cr5 are presented. This alloy is shown to maintain an fcc structure upon heating. However, the concentration of Cu is reduced at high temperatures, resulting in a decrease in the lattice constant. As concurrent thermophysical properties are probed, these preliminary structure and composition experiments demonstrate the capabilities of this technique to determine the composition–processing–structure–properties of metal alloys for AM.