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CONTENTS 1. CHROMATOGRAPHIC TECHNIQUES ............... 1 Chromatography for Analytical Analyses ............ 1 Gas Chromatography .......................... 1 General .................................. 1 Types of Gas Chromatography .................. 3 Liquid Chromatography ........................ 3 General .................................. 3 Types of Liquid Chromatography ................ 5 Type of Information Obtained ................... 6 Advantages ................................ 7 Disadvantages .............................. 7 Interferences ............................... 7 GPC/DRI ................................... 7 Gel Permeation Chromatography .................. 8 GPC/DRI/LALLS ............................ 10 GPC/DRI/VIS ............................... 11 GPC/DRI/UV ............................... 11 GPC/DRI/FTIR .............................. 15 Submitting Samples ......................... 15 2. THERMAL ANALYSIS .......................... 17 General Principles of Operation .................. 17 Thermal Analysis of Polymers ................... 19 Differential Scanning Calorimetry (DSC) .......... 20 Thermogravimetric Analysis (TGA) .............. 20 Thermomechanical Analysis (TMA) .............. 20 Dynamic Mechanical Thermal Analysis (DMTA) .... 23 ix X Contents 3. MICROSCOPY FOR POLYMER CHARACTERIZATION .......................... 25 General Information .......................... 25 Non-Routine Techniques ....................... 27 4. ELEMENTAL AND STRUCTURAL CHARACTERIZATION TESTS .................... 43 Atomic Absorption Spectroscopy ................. 43 Inductively Coupled Plasma Atomic Emission Spectroscopy .............................. 45 Ion Chromatography (IC) ...................... 48 Ion Selective Electrodes (ISE) ................... 52 Mass Spectrometry (MS and GC/MS) ............. 55 Nuclear Magnetic Resonance Spectrometer .......... 60 Sample Preparation ......................... 62 Established Methods by ‘H NMR ............... 63 Fourier Transform Infrared (FI’IR) ............... 64 Ultraviolet, Visible, and Infrared Spectrometry (UV, Vis, IR) .............................. 64 X-Ray Fluorescence Spectrometry ................ 73 Potentiometric Titrations ....................... 78 Neutron Activation Analysis ..................... 80 5. RHEOMETRY ................................. 83 Rheometrics System IV ........................ 83 Capillary Rheometry .......................... 85 Torque Rheometry ........................... 87 6. CHEMICAL ANALYSIS OF POLYMERS ............ 97 Comminution, Separation, and Identification ........ 97 Stabilizer Identification ....................... 100 Polymer Identification ........................ 102 APPENDIX A: ABBREVIATIONS OF POLYMERS . . . . . . . 105 APPENDIX B: GLOSSARY OF POLYMERS AND TESTING . . . . . . . . . . . . . . . , . . . . . . . . . . . . . . . . . . 107 APPENDIX C: PROFESSIONAL AND TESTING ORGANIZATIONS . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 117 American National Standards Institute (ANSI) . . . . . . 117 Contents xi American Society for Testing and Materials (ASTM) ......................... 117 Food and Drug Administration (FDA) ............ 118 National Bureau of Standards (NBS) ............. 119 National Electrical Manufacturers Association (NEMA) ........................ 119 National Fire Protection Association (NFPA) ....... 120 National Sanitation Foundation (NSF) ............ 120 Plastics Technical Evaluation Center (Plastec) ...... 121 Society of Plastics Engineers (SPE) ............... 122 Society of Plastics Industry (SPI) ................ 122 Underwriters Laboratories (UL) ................. 123 APPENDIX D: GLOSSARY OF ENGINEERING AND MATERIALS TERMS . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 125 INDEX . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 235
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