Comparison of various digestion procedures in chemical analysis of spent hydrodesulfurization catalyst

Four digestion procedures have been tested to verify their applicability to the determination of major and trace elements (Al, Ba, Cd, Co, Cr, Cu, Fe, Mn, Mo, Ni, Pb, Sr, Ti, V, Zn) in a spent catalyst by inductively coupled plasma optical emission spectrometry (ICP-OES). Two digestion procedures have been carried out in a closed microwave system using: (1) HCl + HNO3 + H2O2; (2) HNO3 + HF, whereas the remaining two in an open system using: (1) aqua regia + NH4F, HNO3, H2SO4; (2) HF + HClO4, H3BO3, HCl. Among these four procedures the microwave digestion system (1) gave the best recovery results. The quality of the analytical results has been evaluated by the analysis of the CTA-FFA-1 Fine Fly Ash Certified Reference Material. A good agreement between the measured and reference values was found for almost all elements. The precision was assessed from the replicate analyses of microwave digestion (1) system and was found to be less than 5% of the relative standard deviation (R.S.D.).