Characterization of Zircaloy-2 and Zircaloy-4 by X-Ray fluorescence

The analytical characterization of zircaloy-2 and zircaloy-4 is intimataly connected with the determination of Sn, Fe, Cr, Ni, O, N, H, and Hf. An analytical method developed in this laboratory is discribed for the determination of metallic elements like Sn, Fe, Cr and Ni using the technique of X-ray fluorescence. The samples are prepared in the form of double-layer pellets using boric acid as a binding agent. The zircaloy-4 is dissolved in hydrofluoric acid and the metallic elements are converted to fluorides. The standard samples used for calibration are prepared from synthetic materials. The elements are determined by measuring the characteristic first order K α lines. A Zircaloy-4 sample analysed yielded the following values: Sn=1.30+-0.03%, Fe=0.18+-0.01%, Cr=0.088+-0.004% and Ni=14+-3 ppm. The reproducibility, precision, as well as the theoretical limit of detection of the method are discussed. The determination of the elements O, N and H present as occluded gas in the zircaloy is nearing completion. These analyses are being carried out by a Mass Spectrometric technique where an aliquot of the released gas is analysed. (Author)