An on-line matrix separation and preconcentration procedure for ICP OES determination of Cd, Co, Cu, Mn and Pb traces in Zr and Zr–Nb alloys using a cation-exchange resin microcolumn

Abstract

Determination of traces of Cd, Co, Cu, Mn and Pb elements in zirconium and its alloys by inductively coupled plasma optical emission spectrometry (ICP OES) suffers from severe spectral interferences from the matrix elements. Here we developed an interference-free analytical procedure for ICP OES determination of these elements in zirconium and zirconium–niobium alloys based on a simple and inexpensive on-line matrix separation method using a small amount of a strong cation exchange resin (∼0.4 g) in a microcolumn, which also serves to preconcentrate the elements. The conditions of adsorption and desorption of the above mentioned elements were optimized. The desorption of the elements was performed using a dilute aqueous solution (1%) of diethylenetriaminepentaacetic acid (DTPA). The developed method is free from spectral interferences caused by zirconium and niobium in the determination of the aforementioned elements by ICP OES. The results of the proposed method were compared with those of Japanese Industrial Standards (JIS) as reference methods, and by recovery tests performed by spiking standard reference solutions of the desired elements to the solution of the dissolved zirconium–niobium alloy samples.