A method for Ca, Fe, Ga, Na, Si and Zn determination in alumina by inductively coupled plasma optical emission spectrometry after aluminum precipitation

In this present work a method for the determination of Ca, Fe, Ga, Na, Si and Zn in alumina (Al₂O₃) by inductively coupled plasma optical emission spectrometry (ICP OES) with axial viewing is presented. Preliminary studies revealed intense aluminum spectral interference over the majority of elements and reaction between aluminum and quartz to form aluminosilicate, reducing drastically the lifetime of the torch. To overcome these problems alumina samples (250 mg) were dissolved with 5 mL HCl + 1.5 mL H₂SO₄ + 1.5 mL H₂O in a microwave oven. After complete dissolution the volume was completed to 20 mL and aluminum was precipitated as Al(OH)₃ with NH₃ (by bubbling NH₃ into the solution up to a pH ~ 8, for 10 min). The use of internal standards (Fe/Be, Ga/Dy, Zn/In and Na/Sc) was essential to obtain precise and accurate results. The reliability of the proposed method was checked by analysis of alumina certified reference material (Alumina Reduction Grade-699, NIST). The found concentrations (0.037% w w⁻¹ CaO, 0.013% w w⁻¹ Fe₂O₃, 0.012% w w⁻¹ Ga₂O₃, 0.49% w w⁻¹ Na₂O, 0.014% w w⁻¹ SiO₂ and 0.013% w w⁻¹ ZnO) presented no statistical differences compared to the certified values at a 95% confidence level.