Alternative dissolution of zircon samples and simultaneous analysis of major and trace components drying unit
SJ Lötter, W Purcelll, JT Nel, E Snyders

Analysis of the major and minor components of raw zircon as well as plasma-dissociated zircon was undertaken using inductively coupled plasma optical emission spectroscopy (ICP-OES). Microwave-assisted acid extraction as well as flux fusion using lithium tetraborate were investigated as digestion methods. Microwave-assisted acid extraction samples were analysed with matrix-matched standards. The most successful microwave-assisted acid extractions yielded 44.3(1), 49.75(7), 78.3(3) and 90.0(7) per cent recovery for Zr, Hf, Al, and Fe respectively using sulphuric acid. In no instance was acid extraction capable of complete digestion of the sample matrix. A standard addition method was applied to the flux-fusion samples due to the high complexity of the sample matrix. Method validation for the flux fusion procedure was performed using the SARM 62 certified reference material (CRM) with acceptable recovery ranges being based on the 95 per cent confidence intervals of the CRM. Successful analyses were achieved for Zr, Hf, and Ti with apparent content of 66(6), 1.7(1) and 0.15(1) per cent respectively.
Keywords: zircon, zirconium, ICP-OES, analysis, quantification, nuclear grade.