A Practical Approach to Quantitative Metal Analysis of Organic Matrices
, by Brennan, Martin
- ISBN: 9780470031971 | 0470031972
- Cover: Hardcover
- Copyright: 10/20/2008
There has been significant expansion in the application of atomic spectrographic techniques in recent years, which has brought with it the need to provide more flexible methods to a wider range of samples, particularly non-aqueous samples. This book compares the traditional and improved methods in the analysis of non-aqueous samples for elemental analyses by atomic emission spectroscopic methods whilst describing procedures that will attempt to improve sample preparation methods.
Dr Martin Brennan is an analytical scientist of 30 years standing with considerable experience in atomic spectroscopy. He has a M.Sc. in analytical science from Queens University, Belfast and a Ph.D in atomic spectroscopy and electroanalytical techniques from University College Cork, Ireland. He has considerable experience in the analysis of a wide range of samples particularly organic type samples and is currently employed with Henkel Ireland Ltd., manufacturers of adhesives and other organic compounds. He holds the position of Hon. Sec. of the Republic of Ireland sub-region Analytical Division of the Royal Society of Chemistry.
| Preface | p. xiii |
| Biography | p. xv |
| Acknowledgements | p. xvii |
| A Practical Approach to Quantitative Metal Analysis of Organic Matrices Using ICP-OES | p. 1 |
| Introduction and Basic Overview | p. 1 |
| Schematic Representation of the Energies Generated by Atomic Spectroscopic Methods | p. 4 |
| Excitation Energy (Quantum Theory and Atomic Spectra) | p. 5 |
| Ionisation Energy and Number of Excited Atoms | p. 7 |
| Width of Atomic Lines | p. 9 |
| Natural Broadening | p. 9 |
| Doppler Broadening | p. 9 |
| Lorentzian Broadening or Pressure Broadening | p. 9 |
| Holtsmark Broadening or Resonance Broadening | p. 11 |
| Field Broadening or Stark Broadening | p. 11 |
| Self-Absorption and Self-Reversal Broadening | p. 11 |
| Brief Summary of Atomic Spectroscopic Techniques Used for Elemental Analysis | p. 12 |
| The Atomic Absorption Spectrophotometer | p. 12 |
| Atomic Fluorescence Spectroscopy | p. 13 |
| Direct Current Plasma Optical Emission Spectrometry (DCP-OES) | p. 13 |
| Microwave Induced Plasma (MIP) | p. 14 |
| Glow Discharge Optical Emission Spectrometry (GD-OES) | p. 15 |
| Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES) | p. 15 |
| Summary: Applications of Atomic Spectroscopy | p. 16 |
| References | p. 18 |
| Instrumentations Associated with Atomic Spectroscopy | p. 21 |
| Instrumentation | p. 21 |
| Types of Plasma Sources | p. 24 |
| Direct Current Plasma Atomic Emission Spectrograph | p. 25 |
| Microwave Induced Plasma | p. 25 |
| Optical Emission Spectroscopy | p. 26 |
| Sample Introduction Systems | p. 30 |
| Mechanical Transfer of Sample/Standards Using Peristaltic Pump, Pressure Valves, Motorised Syringes, etc. | p. 31 |
| Nebulisers | p. 31 |
| Brief Outline of Atomic Spectroscopy Hyphenated Systems | p. 39 |
| Spray Chambers | p. 43 |
| ICP-OES Torches | p. 45 |
| Optics | p. 49 |
| Grating Orders | p. 51 |
| Signal Detectors | p. 53 |
| Photomultiplier Tubes | p. 53 |
| Charge Coupled Devices | p. 55 |
| References | p. 58 |
| Methodologies of Metal Analysis of Organic Matrices Using ICP-OES | p. 59 |
| Sample Preparation Techniques and Methods of Analysis | p. 59 |
| Defining Goals | p. 60 |
| Steps in Chemical Analytical Protocol | p. 61 |
| Sampling and its Importance | p. 62 |
| Sample Preparation Methods | p. 63 |
| Direct Analysis of Organic Solutions | p. 64 |
| Sample Dissolution | p. 65 |
| Chemical Extraction of Metals from Organic Matrices | p. 65 |
| Dry Ashing without Retaining Aids | p. 66 |
| Dry Ashing with Retaining Aids | p. 69 |
| Acid Digestion Using Microwave Oven | p. 69 |
| Oxygen Bomb Flask Combustion (Low Pressure) | p. 71 |
| High Pressure Oxygen Combustion | p. 72 |
| Sample Preparation Using Fusion Methods | p. 73 |
| Analysis Using Slurry Solution Method | p. 74 |
| Sample Preparation Using Leaching Method | p. 75 |
| Sample Preparation Using a UV Digester | p. 75 |
| Non-Spectral Corrections Using ICP-OES | p. 76 |
| Effect of Solvents on ICP-OES | p. 76 |
| Effect of Viscosity on Signal Response | p. 77 |
| Comparison of Nebulisation Efficiency of Solvents Using ICP-OES | p. 78 |
| Choice of Carrier Liquid | p. 80 |
| Methodology of Measurement | p. 81 |
| Choice of Standard Materials | p. 82 |
| Quantitative Analysis Using Calibration Graph Method | p. 82 |
| Quantitative Analysis Using Standard Addition Method | p. 85 |
| Quantitative Analysis Using Internal Standard Method | p. 87 |
| Quantitative Analysis Using Matrix Matching Method | p. 88 |
| Quantitative Analysis Using Flow Injection Technique | p. 89 |
| Validation of an Analytical Method | p. 90 |
| Method Validation of Analysis of Organic Matrices | p. 91 |
| Control and Range Charts | p. 99 |
| Brief Outline of Measurement Uncertainty | p. 101 |
| References | p. 105 |
| Analysis of Plastics, Fibres and Textiles for Metals Content Using ICP-OES | p. 107 |
| A Brief History of Natural and Synthetic Plastic Materials | p. 107 |
| A Brief History of Chemistry of Plastics | p. 109 |
| Chemical Structure of Plastics | p. 110 |
| Polymerization Process of Plastics | p. 111 |
| Polymerisation by Addition Reactions | p. 112 |
| Polymerisation by Condensation Reactions | p. 112 |
| Additives in Plastics | p. 113 |
| Methods of Sample Preparation for Metal Content of Plastics, Fibres and Textiles | p. 115 |
| Sample Preparation Using Dissolution Method | p. 115 |
| Sample Preparation Using Dry Ashing Methods | p. 117 |
| Sample Preparation Using Microwave Acid Digestion Method | p. 119 |
| Sample Preparation Using Oxygen Bomb Combustion Method | p. 121 |
| Comparative Study of Methods of Analysis of Plastic Samples for Metals Content | p. 121 |
| Study of Leaching of Metals from Plastics | p. 123 |
| Study of Leaching of Metals from Children's Toys | p. 124 |
| Analysis for Toxic Metals in Plastics and Non-Electrical Additives Used in Electrical and Electronic Components as Required by RoHS | p. 125 |
| Method for Metal Analysis of Plastics and Non-Electrical Additives Used in Electrical and Electronic Products | p. 127 |
| Conclusion | p. 131 |
| References | p. 132 |
| Metal Analysis of Virgin and Crude Petroleum Products | p. 133 |
| Introduction | p. 133 |
| Brief Introduction to Refining Process in the Petroleum Industry | p. 134 |
| Metals in Crude Oils and Petroleum Products | p. 135 |
| Requirements for the Determination of Metal Content in Virgin and Crude Oils | p. 136 |
| Wear Metals and Metal Contaminants in Lubricating Oils | p. 138 |
| Brief Outline of the Determination of Metals in Organic Materials Using Atomic Spectroscopy Methods | p. 139 |
| Application of Atomic Spectroscopic Techniques in the Analysis of Virgin and Wear Oils for Metals Content | p. 140 |
| Choice of Solvents Suitable for Metal Analysis of Crude and Lubricating Oils Using ICP-OES | p. 141 |
| Selection of Representative Samples in the Study of Metal Analysis of High Viscosity and Low Viscosity Oil Blends | p. 141 |
| Physical Properties of Selected Solvents for Dissolving High Viscosity and Low Viscosity Oils for Metal Analysis | p. 142 |
| Methods of Sample Preparation for Metal Analysis of High Viscosity and Low Viscosity Oil Blends | p. 142 |
| Long-Term Study of Metal Analysis Using Kerosene, Teralin and Decalin Solvents Using ICP-OES | p. 143 |
| Comparative Study of Non-Destructive Methods of Analysis of Metals 'Spiked' in High Viscosity and Low Viscosity Oil Blends Using ICP-OES | p. 144 |
| Analysis of Type C and D Fractions for Metal Content Using Dry Ashing Method | p. 149 |
| Analysis of 'Metal Spiked' Oil Blends Using Microwave Acid Digestion for Metals Content | p. 150 |
| Analysis of 'Metal Spiked' Oil Blends Using High Pressure Oxygen Combustion for Metals Content | p. 152 |
| Comparative Study of Analysis of Trace Levels of Toxic Metals Using Microwave Acid Digestion and Oxygen Bomb Combustion | p. 153 |
| Conclusion to Trace Analysis of Toxic Metals in Oil Products | p. 155 |
| Extraction Method for the Determination of Metals of High Viscosity and Low Viscosity Oil Blends | p. 155 |
| Analysis of Old Lubricating Oil for Total Metal Content Using a Slurry Method with Internal Standard | p. 156 |
| Conclusion | p. 158 |
| References | p. 160 |
| Metal Analysis of Structural Adhesives | p. 161 |
| Introduction | p. 161 |
| Setting and Curing of Adhesives | p. 162 |
| Introduction to Modern Synthetic Adhesives | p. 162 |
| Cyanoacrylate Adhesives | p. 162 |
| Anaerobic and Acrylic Adhesives | p. 163 |
| Epoxy Structural Adhesives | p. 165 |
| Phenolic Adhesives | p. 167 |
| Polyurethane Adhesives | p. 167 |
| Metal Salts and Concomitant Metals in Adhesives | p. 168 |
| Metals Associated with Cyanoacrylate Adhesives | p. 169 |
| Non-Destructive Methods of Analysis for Metals Content in Cyanoacrylate Adhesives | p. 170 |
| General Method | p. 170 |
| Standard Addition Method | p. 171 |
| Internal Standard Method | p. 171 |
| Destructive Methods of Analysis for Metals Content in Cyanoacrylate Adhesives | p. 172 |
| Sample Preparation Using Ashing Method | p. 173 |
| Sample Preparation Using Microwave Acid Digestion | p. 174 |
| Sample Preparation Using Oxygen Bomb Combustion | p. 174 |
| Conclusion to Analysis of Cyanoacrylate Products | p. 175 |
| Metals Associated with Anaerobic Adhesives | p. 176 |
| Destructive Methods of Sample Preparation for Metals Content in Anaerobic Adhesives | p. 177 |
| Ashing Method of Type A and Type B Anaerobic Adhesives | p. 177 |
| Sample Preparation of Anaerobic Adhesives Using Microwave Acid Digestion | p. 178 |
| Sample Preparation of Anaerobic Adhesive Using Oxygen Bomb Combustion | p. 180 |
| Conclusion to Analysis of Anaerobic Adhesives | p. 180 |
| Metal Analysis of Chemical Raw Materials Used to Manufacture Anaerobic Adhesives | p. 181 |
| Column Extraction of Metal from Liquid Monomers | p. 181 |
| Analysis of Metal Salt Content Dissolved in Aerosol Solvent(s) | p. 182 |
| Sample Preparation and Analysis of Metals in Aerosol | p. 183 |
| A Study of the Effects of Anaerobic Adhesives on Metallic Substrates | p. 183 |
| Metals Associated with Epoxy Adhesives | p. 186 |
| Composition of Epoxy Adhesives | p. 187 |
| Preparation of Epoxy Adhesive 'Spiked' with Ge(AcAc)BF[subscript 4] | p. 187 |
| Determination of the Concentration of Ge(AcAc)BF[subscript 4] in Epoxy Adhesives Using Non-Destructive Methods | p. 188 |
| Determination of the Concentration of Ge(AcAc)BF[subscript 4] in Epoxy Adhesives Using Destructive Methods | p. 190 |
| Conclusion of Metal Analysis of Epoxy Adhesives | p. 192 |
| Metals Associated with Phenolic Adhesives | p. 193 |
| Preparation of Typical Phenolic Adhesives Containing Calcium and Copper Sulphonate Salts | p. 193 |
| Non-Destructive Methods of Analysis of Phenolic Adhesives | p. 194 |
| Metals Associated with Polyurethane Adhesives | p. 194 |
| Preparation and Analysis of Polyurethane Adhesives Containing Organometallic Catalysts | p. 195 |
| Conclusion to Metal Analysis of Phenolic and Polyurethane Adhesives | p. 197 |
| References | p. 198 |
| Hyphenated and Miscellaneous Techniques Used with ICP-OES | p. 199 |
| Introduction | p. 199 |
| Coupling of Flow Injection Analysis with ICP-OES | p. 200 |
| Theory of Flow Injection | p. 201 |
| Configuration of ICP-OES/FIA System | p. 202 |
| Signal Acquisition and Data Management | p. 203 |
| Reproducibility of Measurements Using ICP-OES/FIA | p. 204 |
| Dispersion and Diffusion of 'Sample Plug' in a Carrier Stream | p. 205 |
| Metal Analysis of Organic Compounds Using ICP-OES-FIA | p. 206 |
| Effect of Loop Size on Signal Response | p. 207 |
| Comparative Measurements of Peak Height and Peak Area | p. 208 |
| Effect of Viscosity Using ICP-OES/FIA | p. 209 |
| A Study of Solvent Effects Using ICP-OES/FIA | p. 210 |
| Determination of Limit of Detection and Quantification | p. 210 |
| Conclusions of Analysis Using ICP-OES-FIA | p. 211 |
| Use of Internal Standard(s) with ICP-OES | p. 213 |
| Conclusion to Internal Standard(s) Study | p. 217 |
| Coupling of Ion Chromatography with ICP-OES | p. 218 |
| Preconcentration of Metals Using Ion Chromatography | p. 220 |
| Analysis of Lanthanide and Transition Metals with ICP-OES/IC | p. 221 |
| Coupling of Gas Chromatography with ICP-OES or Atomic Emission Detector | p. 222 |
| Metal Analysis Using ICP-OES Coupled with Electro-Thermal Vaporisation | p. 224 |
| Surface Analysis Using Laser Ablation with ICP-OES | p. 226 |
| Determination of Thickener Content of Paints, Pharmaceutical Products and Adhesives Using ICP-OES | p. 227 |
| Metal Analysis of Metallo-Pharmaceutical Products | p. 230 |
| Metallic Type Antibiotic Drugs | p. 233 |
| Platinum and Palladium Drugs for Cancer Treatments | p. 234 |
| Metal Analysis of Infusion and Dialysis and Bio-Monitoring Solutions | p. 235 |
| Organometallic Compounds | p. 236 |
| Metals and Metalloid Analysis in Support of Forensic Science | p. 237 |
| Non-Prescription Nutritional Dietary Supplements | p. 239 |
| Trace Metal Analysis of Foods | p. 244 |
| General Methods of Metal Analysis of Foods | p. 244 |
| Conclusion to Food Analysis | p. 246 |
| References | p. 246 |
| Index | p. 249 |
| Table of Contents provided by Ingram. All Rights Reserved. |
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