Determination of Common Analytes at Trace Levels in Zr Matrix by ICP-AES Without Chemical/Physical Separation

摘要

Chemical (ICP-AES) or physical (d.c. arc carrier distillation technique) separation of the major matrix, followed by the determination of trace metallic impurities in the raffinate, is a well accepted protocol in the nuclear industries to avoid spectral interferences from emission- rich matrices such as U, Pu, Zr, Th, etc. With ICP-AES analysis, the RSD is better (less than 5%), separation is time-consuming, involves handling of the materi- als which increases the chances of contamination, while the pre- cision of the d.c. arc technique is 15-25%. Thus, there is a need to have an ICP-AES-based methodology where the analytes can be determined in a nuclear matrix at trace levels without requiring chemical separation. In this paper, an attempt was made to develop a method for the determination of trace constituents in a Zr matrix without separation by using the flexibility of a charge coupled device(CCD) detector for choosing additional interference-free analytical lines for Mn, Fe, Ga, In, Sr, K, Li, Eu, Co, Zn, Ni, Cu, Al, and Si. It was observed that the analytes can be determined up to 0.1 μg/mL in the presence of Zr The results were also compared with routinely used methods and found to be satisfactory. In addi- ion, an analytical method was developed for the determination of zirconium by ICP-AES, including the identification of suitable analytical lines (343.823 nm, 257.139 nm, and 272.262 nm) and studying the analytical performance such as sensitivity, detection limits, etc.