Determination of impurities in zirconium disilicide and zirconium diboride by inductively coupled plasma atomic emission spectrometry

Abstract

A sensitive method is described for the determination of impurities (Al, Ca, Co, Cr, Fe, Hf, Mg, Mn, Ni, Sr, Ti, V, W, and Y) in zirconium disilicide (ZrSi₂) and zirconium diboride (ZrB₂) by inductively coupled plasma atomic emission spectrometry after acid decomposition under pressure. A zirconium disilicide powder sample was decomposed with sulfuric acid in a poly(tetrafluoroethylene)(PTFE) pressure vessel after hydrofluoric acid and sulfuric acid treatment. A zirconium diboride powder sample was also decomposed with sulfuric acid, nitric acid, and hydrofluoric acid in a PTFE pressure vessel after predecomposition with the sulfuric and nitric acids. The matrix effects on the background levels and the emission intensities of the elements were compensated by using matrix-matched standard solutions for calibration. Fourteen elements in commercial ZrSi₂ and ZrB₂ powder samples were determined with good precision and the results obtained by the proposed methods were found to be in good agreement with those obtained by a fusion method with sodium carbonate.