Three different methods for pre-irradiation separation of the tantalum matrix combined with preconcentration of trace elements for NAA were developed. They involve selective extraction of tantalum with diantipyrylmethane, and anion- and cation-exchange from hydrofluoric acid medium. The role of the blank as the limiting factor for limits of detection and accuracy was one of the main aspects of this investigation. A conventional radiochemical NAA based on post-irradiation separation of the matrix radionuclides was also applied. The trace elements considered were Ag, Ba, Ce, Co, Cr, Cu, Eu, Hf, K, La, Mn, Mo, Na, Rb, Re, Sc, W, Y, Zn, Zr. The methods were used for the analysis of tantalum materials of different purity grades. The advantages and disadvantages of each technique are discussed and the achievable limits of detection are given.
A radiochemical neutron activation technique for the detemination of 19 elements in high purity tungsten has been developed. It is based on extraction with diantipyrylmethane (for tantalum and antimony), substoichiometric extraction of molybdophosphate (for phosphorus) and anion-exchange chromatography (other elements) in hydrofluoric acid medium. The results obtained and achievable limits of detection are given. The effects of self-shielding and nuclear interfering reactions are discussed.
Anion-exchange data have been obtained for the elements As, Hf, Mo, Nb, Pa, Re, Sb, Sn, Ta, Tc, W, and Zr in 0.1 to 10M H2SO4 and in HF–H2SO4 mixtures of combination extending from 0.1 to 10M HF and from 0.1 to 10M H2SO4. The distribution ratios for mixed solutions are presented in form of adsorption contour lines.
The sorption of niobium and tantalum on Dowex-1 and open-cell polyurethane foam polyether-type in HF–H2SO4 and HF–HCl medium has been investigated. The mechanism of the sorption as well as the composition of adsorbable complexes is discussed. A selective adsorption of tantalum was achieved from solutions, in which the concentration range of HF was 0.05–2M, of H2SO4
5M and of HCl4M. The most interesting separation possibilities have been tested under dynamic conditions.