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.