Experimental design in the optimization of a microwave acid digestion procedure for the determination of metals in biomorphic ceramic samples by inductively coupled plasma mass spectrometry and atomic absorption spectrometry

In the present paper, we have synthesized a biomorphic ceramic material from oak wood as biological template structure and infiltration with zirconia-sol. After the material characterization, we have optimized the sample dissolution by acid attack in an oven under microwave irradiation. Experimental designs were used as a multivariate strategy for the effect's evaluation of varying several variables. This article describes the development by response surface methodology (RSM) of a procedure for zirconium determination, and other ions, such as copper and nickel by inductively coupled plasma mass spectrometry (ICP-MS) and others, such as iron, calcium and magnesium determination by flame atomic absorption spectrometry (FAAS) in the synthesized sample after digestion. A full factorial design (33) was used to find optimal conditions for the procedure through response surface study. Three variables (time, HNO3 volume and HF volume) were regarded as factors and as response to the concentration of different metal ions in the optimization study.