Chapter 2

Overview of Microwave Assisted

Sample Preparation

Peter J. Walter, Stuart Chalk, H. M. 'Skip' Kingston

Department of Chemistry and Biochemistry

Duquesne University

Pittsburgh, PA 15282-1503

1. HISTORICAL PERSPECTIVES ON THE DEVELOPMENT OF MICROWAVE SAMPLE PREPARATION

1.1 Reaction Control and Transferring of Microwave Methods

2. DOCUMENTATION OF MICROWAVE METHODS

3. CURRENTLY APPROVED INTERNATIONAL STANDARD MICROWAVE METHODS

4. ROBOTIC AUTOMATION OF MICROWAVE PROCEDURES

5. RESOURCES FOR METHOD DEVELOPMENT

5.1 General guide to literature tables

5.2 Review papers

5.3 Microwave drying

5.4 Microwave Ashing

5.5 Microwave dissolution

5.5.1 General information

5.5.2 Matrix

5.5.3 Analytes

5.5.4 Reagents and microwave conditions

5.5.5 Microwave cavity and reaction vessel descriptions

5.5.6 Detection

5.6 Dissolution Reagents

5.6.1 Nitric Acid (HNO3)

5.6.2 Hydrochloric Acid (HCl)

5.6.3 Hydrofluoric Acid (HF)

5.6.4 Sulfuric Acid (H2SO4)

5.6.5 Perchloric Acid (HClO4)

5.6.6 Hydrogen Peroxide(H2O2)

5.6.7 Physical Properties of the Common Dissolution Reagents

5.6.8 Guidelines for using the chemical reactivity tables and figures

5.6.9 Volatility of an Elemental Specie

5.6.10 Reactions of the Elements with a Reagent

5.6.11 Solubility of the Element

5.6.12 Stability (complexation or precipitation)

5.6.13 Catalytic Effects

6. BIBLIOGRAPHY

7. APPENDICES

1 Biological Reference Materials

1.1 Animal Tissue and Fluid

1.2 Botanical

1.3 Marine

References


2 Geological and Metallurgical Reference Materials

2.1 Rocks and Minerals

2.2 Steels and Alloys

2.3 Soils and Sediments

References


3 Other Reference Materials