Anomalous small-angle scattering (ASAXS) spectra from Al–Zn and Al–Zn–Ag alloys have been recorded at the Stanford Synchrotron Radiation Laboratory (SSRL). The data were obtained at different energies close to the Zn absorption edge. For the binary alloy, the ASAXS intensities follow quantitatively the variation in the atomic scattering factor of zinc. For the ternary alloys, the anomalous effect decreases when the Zn content decreases. Although only weighted sums of the partial structure functions could be determined, it is shown that the results are consistent with the `two-phase' unmixing model and the direction of tie lines of the metastable miscibility gap has been determined. A new method for analyzing ASAXS data for two absorption edges is proposed.