1 Types and Properties of Polymers Production of Synthetic Resins Polycondensation Reactions Polymerisation Reactions...

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1 Contents 1 Types and Properties of Polymers Production of Synthetic Resins Polycondensation Reactions Polymerisation Reactions Determination of Elements Non-metallic Elements Halogens Combustion Methods Oxygen Flask Combustion Alkali Fusion Methods Physical Methods for Determining Halogen Sulfur Combustion Methods Sodium Peroxide Fusion Oxygen Flask Combustion Phosphorus Acid Digestion Nitrogen Combustion Methods Physical Method for Determination of Total Nitrogen Silicon Boron Total Organic Carbon Total Sulfur/Total Halogen Nitrogen, Carbon, and Sulfur Carbon, Hydrogen, and Nitrogen iii

2 Introduction to Polymer Analysis Oxygen Flask Combustion: Ion Chromatography XRFS Thermogravimetric Analysis Metals Destructive Techniques Atomic Absorption Spectrometry (AAS) GFAAS Atom Trapping Technique Vapour Generation Atomic Absorption Spectrometry (VGAAS) Zeeman AAS ICP-AES Hybrid Inductively Coupled Plasma Systems Chromatography ICP Flow Injection with ICP Inductively Coupled Plasma with Atomic Fluorescence Spectrometry (ICP-AFS) Inductively Coupled Plasma Optical Emission Spectrometry Mass Spectrometry (ICP-MS) Pre-concentration AAS Techniques Applications of Techniques Detailed So Far Elemental Analysis of Polymers Trace Metals in Polymers Pressure Dissolution Technique Visible and UV Spectroscopy Polarography and Voltammetry Ion Chromatography Non-destructive Methods XRFS NAA Functional Groups Hydroxy Groups Chemical Methods iv

3 Contents Acetylation and Phthalation Procedures Spectrophotometric methods Direct Injection Enthalpimetry IR Spectroscopy Determination of Hydroxy Groups in Dinitropropyl Acrylate Prepolymer NMR Carboxyl Groups NMR Titration Procedures IR Spectroscopy Ester Groups Saponification Hydriodic Acid Reduction Gas Chromatography IR Spectroscopy Determination of Free and Combined Vinyl Acetate Groups in Vinyl Chloride-Vinyl Acetate Copolymers Determination of Bound Vinyl Acetate in Ethylene-Vinyl Acetate Copolymers NMR Pyrolysis Gas Chromatography Carbonyl Groups IR Spectroscopy Derivatisation Methods Spectrophotometric methods Ether Groups Cleavage Gas Chromatography Alkoxy Groups IR Spectroscopy NMR Spectroscopy Pyrolysis-Based Method Alkoxy Groups in Ethylene Oxide-Propylene... Oxide Condensates Miscellaneous Methods v

4 Introduction to Polymer Analysis 3.7 Oxyalkylene Groups Cleavage Gas Chromatography Pyrolysis Gas Chromatography IR Spectroscopy NMR Spectroscopy Anhydride Groups Total Unsaturation Hydrogenation Methods Halogenation Methods Iodine Monochloride Procedure IR Spectroscopy NMR Spectroscopy Pyrolysis Gas Chromatography Derivitivisation Gas Chromatography Radiochemical Methods Determination of unsaturation in butyl rubber Alkyl and Aryl Groups Alkali Fusion Reaction Gas Chromatography Oxirane Rings Amino Groups Amino and Imido Groups Alkali Fusion Gas Chromatography Nitrile Groups Silicon Functions Determination of Monomer Ratios in Copolymers IR Spectroscopy Ethylene Propylene Copolymers Ethylene Vinyl Acetate Styrene-based Copolymers Styrene Acrylic Acid Styrene acrylate and styrene methylacrylate copolymers Vinyl Chloride Vinyl Acetate Copolymers vi

5 Contents 4.2 NMR Spectroscopy Ethylene Propylene Copolymers Ethylene hexane Styrene-Based Copolymers Styrene Methacrylate Styrene methyl acrylate Styrene acrylic acid Benenyl Acrylate Vinyl Acetate [27] Vinyl Acetate Methylacrylate Hexafluoropropylene Vinylidene Fluoride Copolymer F-NMR Pyrolysis Gas Chromatography Acrylamide Methacryloyl Oxy-ammonium Chloride Pyrolysis Gas Chromatography Ethylene-Based Copolymers Ethylene butene Ethylene - butadiene Vinylidene Chloride Vinyl Chloride Copolymers Acrylonitrile-cis (or trans) Penta 1,3 diene Pyrolysis IR Spectroscopy Olefin Copolymers Sequencing of Monomer Unit in Polymers Sequencing in Homopolymers NMR Spectroscopy Pyrolysis Gas Chromatography (Py-GC) Polyolefins Polyisoprene Polyvinyl Chloride (PVC) SIMS Polystyrene Ozonisation Technique Polybutadiene Polyisoprene Sequencing in Copolymers vii

6 Introduction to Polymer Analysis IR Spectroscopy Styrene methacrylonitrile NMR Spectroscopy Styrene acrylate and styrene acrylic acid Propylene-1-butene Vinylidene chloride methacrylonitrile and vinylidene cyanovinyl acetate copolymers Acrylonitrile butyl acrylate copolymer Py-GC Ethylene propylene diene Hydrogenated acrylonitrile butadiene copolymers (NBR) Butadiene acrylonitrile methacrylic acid terpolymer Styrene-n-butyl acrylate Ethylene oxide condensates SIMS Polydimethyl siloxane urethane Ozonolysis Techniques Butadiene propylene Styrene butadiene copolymers Stereoisomerism and Tacticity Tacticity of Polypropylene Tacticity of Syndiotactic Polystyrene (sps) Tacticity of Polyvinyl Chloride (PVC) Tacticity of Poly(n-butyl methacrylate) Identification of Diastereoisomeric Tetramers in the Pyrograms of polymethyl methacrylate Tacticity of Poly(1-chloro-fluoroethylene) Regioisomerism Polypropylene Propylene-1-Ethylene Copolymer Polybutadiene-1-ethylene viii

7 Contents 7.4 Poly-2,3-dimethyl Butadiene Polybutadiene Polyisoprene Polypropylene Glycol Polyepichlorohydrin Other Polymers Determination of End Groups Polypropylene Oxide Polyvinyl chloride (PVC) Polystyrene (PS) NMR Spectroscopy Pyrolysis Gas Chromatogarphy (Py-GC) Dye Partition Methods Polyethylene (PE) Polyethylene Terephthalate Polyisobutylene (PIB) Tert-chlorine Terminated PIB Olefin-terminated PIB Anisotropic Effect Hydroxy-terminated PIB Polymethylmethacrylate Py GC MALDI-ToF-MS Dye Partition Methods Terminal Epoxides IR spectroscopy Poly(2,6-dimethyl 1,4, phenylene oxide) NMR spectroscopy Miscellaneous End Groups Types of Unsaturation Unsaturation in Homopolymers Polybutadiene Unsaturation ix

8 Introduction to Polymer Analysis Infrared spectrometry Nuclear Magnetic Resonance (NMR) Spectroscopy Polyisoprene Unsaturation IR Spectroscopy Nuclear Magnetic Resonance (NMR) spectroscopy Polyethylene Unsaturation Polypropylene Unsaturation Unsaturation in Copolymers Styrene divinyl benzene IR Spectroscopy Poly(trimethylolpropane trimethacrylate) (TRIM) Miscellaneous Copolymers Ozonolysis Techniques Polymer Branching IR Spectroscopy Methyl Branching in Polyethylene NMR Spectroscopy Ethyl and Higher Alkyl Groups Branching in Polyethylene Branching in Ethylene propylene Copolymers Branching Ethylene Higher Olefin Copolymers Polystyrene Polyvinyl Chloride Polyvinyl Fluoride Vacuum Radiolysis Ethylene Copolymer Pyrolysis-based Techniques Elucidation of Short Chain Branching in Polyethylene Short Chain Branching in Ethylene Higher Olefin Copolymers Branching in Ethylene propylene Copolymers Microstructure of Ethylene-Propylene Copolymers x

9 Contents Branching in PVC Size-Exclusion Chromatography (SEC) Polyethylene Other Polymers Block Copolymers 395 Abbreviations 401 Index 407 xi

10 Introduction to Polymer Analysis xii