The composition of molybdate-based conversion coatings on zinc-nickel alloy electrodeposits was examined by extended X-ray absorption. ne structure (EXAFS). The absorption spectra from appropriate standards showed distinct differences between the Mo(IV) and Mo(VI) oxidation states. A pre-edge peak was apparent for the various molybdate species and molybdenum trioxide, with the energy and intensity dependent on the coordination of the molybdenum. A shift in the molybdenum K-edge spectra was also evident between Mo(IV) and Mo(VI) compounds. A qualitative analysis revealed that both Mo(IV) and Mo(VI) species were present within the molybdate-based conversion coating, with a significant prevalence of hexavalent molybdenum.