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¡ï¡ï¡ï¡ï¡ï¡ïÔÌûʧЧhttp://muchong.com/bbs/viewthread.php?tid=1088616&fpage=1¡ï¡ï¡ï¡ï¡ï ÊéÃû A Practical Approach to Quantitative Metal Analysis of Organic Matrices ×÷ÕßBy Martin Brennan Publisher: Wiley Number Of Pages: Publication Date: 2008-11-03 ISBN-10 / ASIN: 0470031972 Binding: Hardcover Ŀ¼1 A Practical Approach to Quantitative Metal Analysis of Organic Matrices Using ICP-OES 1 1.1 Introduction and Basic Overview 1 1.2 Schematic Representation of the Energies Generated by Atomic Spectroscopic Methods 4 1.3 Excitation Energy (Quantum Theory and Atomic Spectra) 5 1.4 Ionisation Energy and Number of Excited Atoms 7 1.5 Width of Atomic Lines 9 1.5.1 Natural Broadening 9 1.5.2 Doppler Broadening 9 1.5.3 Lorentzian Broadening or Pressure Broadening 9 1.5.4 Holtsmark Broadening or Resonance Broadening 11 1.5.5 Field Broadening or Stark Broadening 11 1.5.6 Self-Absorption and Self-Reversal Broadening 11 1.6 Brief Summary of Atomic Spectroscopic Techniques Used for Elemental Analysis 12 1.6.1 The Atomic Absorption Spectrophotometer 12 1.6.2 Atomic Fluorescence Spectroscopy 13 1.6.3 Direct Current Plasma Optical Emission Spectrometry (DCP-OES) 13 1.6.4 Microwave Induced Plasma (MIP) 14 1.6.5 Glow Discharge Optical Emission Spectrometry (GD-OES) 15 1.6.6 Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES) 15 1.7 Summary: Applications of Atomic Spectroscopy 16 References 18 2 Instrumentations Associated with Atomic Spectroscopy 21 2.1 Instrumentation 21 2.2 Types of Plasma Sources 24 2.2.1 Direct Current Plasma Atomic Emission Spectrograph 25 2.2.2 Microwave Induced Plasma 25 2.2.3 Optical Emission Spectroscopy 26 2.3 Sample Introduction Systems 30 2.3.1 Mechanical Transfer of Sample/Standards Using Peristaltic Pump, Pressure Valves, Motorised Syringes, etc. 31 2.3.2 Nebulisers 31 2.3.3 Brief Outline of Atomic Spectroscopy Hyphenated Systems 39 2.4 Spray Chambers 43 2.5 ICP-OES Torches 45 2.6 Optics 49 2.6.1 Grating Orders 51 2.7 Signal Detectors 53 2.7.1 Photomultiplier Tubes 53 2.7.2 Charge Coupled Devices 55 References 58 3 Methodologies of Metal Analysis of Organic Matrices Using ICP-OES 59 3.1 Sample Preparation Techniques and Methods of Analysis 59 3.2 Defining Goals 60 3.3 Steps in Chemical Analytical Protocol 61 3.4 Sampling and its Importance 62 3.5 Sample Preparation Methods 63 3.5.1 Direct Analysis of Organic Solutions 64 3.5.2 Sample Dissolution 65 3.5.3 Chemical Extraction of Metals from Organic Matrices 65 3.5.4 Dry Ashing without Retaining Aids 66 3.5.5 Dry Ashing with Retaining Aids 69 3.5.6 Acid Digestion Using Microwave Oven 69 3.5.7 Oxygen Bomb Flask Combustion (Low Pressure) 71 3.5.8 High Pressure Oxygen Combustion 72 3.5.9 Sample Preparation Using Fusion Methods 73 3.5.10 Analysis Using Slurry Solution Method 74 3.5.11 Sample Preparation Using Leaching Method 75 3.5.12 Sample Preparation Using a UV Digester 75 3.6 Non-Spectral Corrections Using ICP-OES 76 3.6.1 Effect of Solvents on ICP-OES 76 3.6.2 Effect of Viscosity on Signal Response 77 3.6.3 Comparison of Nebulisation Efficiency of Solvents Using ICP-OES 78 3.6.4 Choice of Carrier Liquid 80 3.7 Methodology of Measurement 81 3.7.1 Choice of Standard Materials 82 viii Contents 3.7.2 Quantitative Analysis Using Calibration Graph Method 82 3.7.3 Quantitative Analysis Using Standard Addition Method 85 3.7.4 Quantitative Analysis Using Internal Standard Method 87 3.7.5 Quantitative Analysis Using Matrix Matching Method 88 3.7.6 Quantitative Analysis Using Flow Injection Technique 89 3.8 Validation of an Analytical Method 90 3.8.1 Method Validation of Analysis of Organic Matrices 91 3.9 Control and Range Charts 99 3.10 Brief Outline of Measurement Uncertainty 101 References 105 4 Analysis of Plastics, Fibres and Textiles for Metals Content Using ICP-OES 107 4.1 A Brief History of Natural and Synthetic Plastic Materials 107 4.2 A Brief History of Chemistry of Plastics 109 4.3 Chemical Structure of Plastics 110 4.4 Polymerization Process of Plastics 111 4.4.1 Polymerisation by Addition Reactions 112 4.4.2 Polymerisation by Condensation Reactions 112 4.5 Additives in Plastics 113 4.6 Methods of Sample Preparation for Metal Content of Plastics, Fibres and Textiles 115 4.6.1 Sample Preparation Using Dissolution Method 115 4.6.2 Sample Preparation Using Dry Ashing Methods 117 4.6.3 Sample Preparation Using Microwave Acid Digestion Method 119 4.6.4 Sample Preparation Using Oxygen Bomb Combustion Method 121 4.7 Comparative Study of Methods of Analysis of Plastic Samples for Metals Content 121 4.8 Study of Leaching of Metals from Plastics 123 4.8.1 Study of Leaching of Metals from Children¡¯s Toys 124 4.9 Analysis for Toxic Metals in Plastics and Non-Electrical Additives Used in Electrical and Electronic Components as Required by RoHS 125 4.9.1 Method for Metal Analysis of Plastics and Non-Electrical Additives Used in Electrical and Electronic Products 127 4.10 Conclusion 131 References 132 5 Metal Analysis of Virgin and Crude Petroleum Products 133 5.1 Introduction 133 5.2 Brief Introduction to Refining Process in the Petroleum Industry 134 5.3 Metals in Crude Oils and Petroleum Products 135 5.4 Requirements for the Determination of Metal Content in Virgin and Crude Oils 136 38RJQ}L4$XGKZ0[V373~4%H.jpg 20081207_8f737a07d571392cd32754sfutEjd3Qz.jpg |
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