Compositional characterization of hafnium recovered from zirconium purification process using total reflection X-ray fluorescence

Hafnium is a very valuable metal having many applications which require it to be free from impurities. It does not exist freely in the earth crust and is found to be associated with zirconium ores. The raffinate of Zr purification process is one of the sources for obtaining Hf. Accurate analysis of Hf in presence of Zr is essential for such recovery processes. A Total reflection X-ray Fluorescence (TXRF) method for chemical characterization of Hf containing solution samples, obtained during the various steps of recovery process of hafnium nitrate from the Zr purification process, was developed. The finally obtained solid HfO2 samples were also characterised by TXRF directly without any dissolution. The TXRF results obtained were compared with Inductively Coupled PlasmaOptical Emission Spectrometry (ICP-OES) results for solution samples and were found to be in good agreement. The TXRF method developed has an added advantage that it can analyse the solid samples directly without any dissolution, in addition to requirement of small amount of samples (ng level), economical, fast and no requirement of matrix matched standards.

Automated summary

Hafnium, a valuable metal found in association with zirconium ores, requires accurate analysis for recovery processes. A TXRF method was developed for chemical characterization of Hf containing solution samples, with the advantage of analyzing solid samples directly without dissolution, requiring small amounts of samples, and being economical and fast. The TXRF results were compared with ICP-OES results and found to be in good agreement.