Low cost and rapid analytical technique for determination of niobium and titanium in zirconium alloy

Abstract

A low cost and rapid analytical technique was developed for determination of major and minor constituents in zirconium alloys. Determination of niobium (Nb) and titanium (Ti) in the bulk matrix of Zr has been done by recording absorption spectra of their peroxy complexes. Samples were initially digested in an acid mixture of HF : H₂SO₄ : H₂O₂ (1 : 1 : 1 ratio). The interference from the bulk matrix of Zr and other major alloying elements such as Fe, Sn, Cr and Ni in addition to the interferences from trace elements such as Al, Cd, Co, Cu, Hf, Pb, Mn, W and V have been successfully avoided by forming peroxy complexes of Ti and Nb, using different concentrations of H₂O₂ and H₂SO₄. The spectrophotometric measurements were carried out at 310 nm and 410 nm for Nb and Ti, respectively. Determination of other major alloying (Fe, Sn, Cr and Ni) elements were also carried out by UV-Visible spectrophotometry, while detection of Cd, Co, Cu, Pb and Mn were carried out by Atomic Absorption Spectrometer (AAS). Inductively Coupled Plasma Optical Emission Spectroscopy (ICP-OES) was used for the determination of Al, Hf, W and V. The validation of the method used for determination of different elements was done by preparing samples using their respective standard solutions.