A simple method for determining Hf in Zr and Zr alloys by ICP-AES

Abstract

This paper describes a rapid, accurate and precise method for determination of trace hafnium (Hf) in zirconium and zirconium alloys by inductively coupled plasma atomic emission spectrometry (ICP-AES). It was found that using a mixture of sulfuric acid (H2SO4) and ammonium sulfate (NH4)2SO4, the total sample dissolution time was 15 min. Experimental works revealed that a high Zr concentration would result in a significant decrease in the peak height of the analyte lines, which was corrected by standard addition method. The performance of the developed method was evaluated by calculating the recovery percent and using standard reference material analysis. The recoveries were in the range of 97.6%–99.5% and the relative standard deviations were within 0.8%–3.0%. The detection limit (3σ) of Hf was found to be 0.01 μg·g-1, respectively. The proposed technique, with high precision and accuracy, was applied to the analysis of trace Hf in zirconium-niobium ingots and tubes for the first time in Iran.