A method for quantitative measurements of gas and liquid distributions is demonstrated using simultaneous x-ray fluorescence and radiography of both phases in an atomizing coaxial spray. Synchrotron radiation at 10.1 keV from the Advanced Photon Source at Argonne National Laboratory is used for x-ray fluorescence of argon gas and two tracer elements seeded into the liquid stream. Simultaneous time-resolved x-ray radiography combined with timeaveraged dual-tracer fluorescence measurements enabled corrections for reabsorption of x-ray fluorescence photons for accurate, line-of-sight averaged measurements of the distribution of the gas and liquid phases originating from the atomizing nozzle.