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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

Authors
Journal
Microchemical Journal
0026-265X
Publisher
Elsevier
Publication Date
Volume
94
Issue
1
Identifiers
DOI: 10.1016/j.microc.2009.08.001
Keywords
  • Biomorphic Zro2-Ceramics
  • Synthesis
  • Dissolution
  • Experimental Design
  • Icp-Ms
  • Faas
Disciplines
  • Biology
  • Design

Abstract

Abstract 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 (3 3) was used to find optimal conditions for the procedure through response surface study. Three variables (time, HNO 3 volume and HF volume) were regarded as factors and as response to the concentration of different metal ions in the optimization study.

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