ABSTRACT:Perrhenate (ReO 4 − ), as a TcO 4 − analogue was incorporated into mixed-anion sodalites from binary solutions containing ReO 4 − and a competing anion X n− (Cl − , CO 3 2− , SO 4 2− , MnO 4 − , or WO 4 2− ). Our objective was to determine the extent of solid solutions formation and the dependence of competing ions selectivity on ion size. Using equivalent aqueous concentrations of the anions (ReO 4 − / X n− molar ratio = 1:1), mixed-anion sodalites were hydrothermally synthesized from zeolite and NaOH at 90°C for 96 hours. The resulting solids were characterized by bulk chemical analysis, X-ray diffraction, scanning electron microscopy, and X-ray absorption near edge structure (XANES) spectroscopy to determine the crystal structure, chemical composition, and morphology, and to confirm the rhenium (Re) oxidation state. Rhenium in the solid phase occurred predominately as [21]. The following parameters were allowed to vary: the background (8 parameters), unit cell, Na position, Re/anion occupancy, peak shape (5 parameters: