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AE Tonelli

NMR Spectroscopy and Polymer Microstructure – The Conformational Connection

Name: NMR Spectroscopy and Polymer Microstructure – The Conformational Connection
Author: AE Tonelli

The Conformational Connection

Gebonden Engels 1989 9780471187486

310,38

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Samenvatting

The various techniques used to analyze the microstructures of polymers are presented in this book. High resolution and solid state techniques are described, and applications to both synthetic and biological polymers are discussed in detail.

Particular emphasis is placed on the determination of polymer microstructure by NMR spectroscopy. Here attention is drawn to the connection between the microstructures and NMR spectra of polymers, and it is demonstrated that the local polymer conformation provides this link. The numerous examples illustrating this connection are a special feature of the book.

Specificaties

ISBN13:9780471187486

Taal:Engels

Bindwijze:gebonden

Aantal pagina's:264

Uitgever:John Wiley & Sons

Serie:Methods in Stereochemical Analysis

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Inhoudsopgave

Preface
 
 1. The Microstructure of Polymer Chains
 
 1.1 Introduction
 
 1.2 Polymers Are Macromolecules
 
 1.3 Polymer Microstructures from Polymerization of Monomers
 
 1.3.1 Directional Isomerism
 
 1.3.2 Stereochemical Isomerism
 
 1.3.3 Geometrical Isomerism
 
 1.3.4 Truly Asymmetric Polymers
 
 1.3.5 Copolymer Sequences
 
 1.4 Organization of Polymer Chains
 
 1.5 Polymer Properties and Their Relation to Microstructure
 
 2. Nuclear Magnetic Resonance
 
 2.1 Introduction
 
 2.2 The NMR Phenomenon
 
 2.2.1 Resonance
 
 2.2.2 Interactions and Relaxations of Nuclear Spins
 
 2.2.3 Chemical Shift
 
 2.2.4 Spin–Spin Coupling
 
 2.3 Experimental Observation of NMR
 
 3. High–Resolution NMR of Polymers
 
 3.1 Introduction
 
 3.2 ¯1H NMR
 
 3.3 ¯13C NMR
 
 3.4 High–Resolution ¯13C NMR in the Solid State
 
 3.4.1 Dipolar Broadening
 
 3.4.2 Chemical–Shift Anisotropy
 
 3.4.3 Cross–Polarization
 
 3.5 Two–Dimensional NMR
 
 3.6 Other Nuclei–¯15N, ¯19F, ¯29Si, and ¯31p
 
 4. ¯13C NMR of Polymers
 
 4.1 Introduction
 
 4.2 ¯13C Chemical Shifts and Their Dependence on Microstructure
 
 4.2.1 ¯13C Nuclear Shielding
 
 4.2.2 Substituent Effects on ¯13C Chemical Shifts
 
 4.2.3 The –Substituent Effect in ¯13C NMR
 
 4.2.4 –gauche Effects in ¯13C NMR
 
 5. –gauche Effect Method of Predicting ¯13C NMR Chemical Shifts
 
 5.1 Introduction
 
 5.2 Polymer Conformations
 
 5.2.1 Rotational Isomeric–State Model of Polymers
 
 5.2.2 Average Bond Conformations
 
 5.3 –gauche Effect Calculation of ¯13C NMR Chemical Shifts
 
 5.3.1 Small–Molecule Example
 
 5.3.2 Macromolecular Example
 
 6. Determination of Stereosequences in Vinyl Polymers
 
 6.1 Introduction
 
 6.2 Traditional Methods
 
 6.2.1 Stereoregular Polymers
 
 6.2.2 Epimerization of Stereoregular Polymers
 
 6.2.3 Model Compounds
 
 6.2.4 Assumed Polymerization Mechanism
 
 6.3 2D NMR Determination of Vinyl Polymer Stereosequence
 
 6.4 Application of –gauche Effect Method
 
 6.5 Establishing Vinyl Polymerization Mechanisms from Stereosequence Analysis
 
 7. Microstructural Defects in Polymers
 
 7.1 Introduction
 
 7.2 Determining the Regiosequence of PVF—2
 
 7.2.1 ¯13C NMR
 
 7.2.2 ¯19F NMR
 
 7.2.3 2D ¯19F NMR
 
 7.3 Regiosequence Defects in PPO
 
 8. Copolymer Microstructure
 
 8.1 Introduction
 
 8.2 Comonomer Sequences
 
 8.3 Copolymer Stereosequences
 
 8.4 Copolymer Conformations
 
 8.5 Copolymerization Mechanisms
 
 9. Chemically Modified Polymers
 
 9.1 Introduction
 
 9.2 Transformation of PVC to Ethylene–Vinyl Chloride Copolymers
 
 9.2.1 Tri–n–butyltin Hydride Reduction of PVC
 
 9.2.2 Microstructures of E–V Copolymers
 
 9.2.3 (n–Bu)—3SnH Reduction of PVC Model Compounds
 
 9.2.4 Computer Simulation of TCH and PVC Reduction
 
 9.3 Modification of 1,4–Poly(butadienes) with Dihalocarbenes
 
 9.3.1 Possible Microstructures in the Dihalocarbene Adducts of PBD
 
 9.3.2 NMR of Dihalocarbene Adducts of PBD
 
 10. Biopolymers
 
 10.1 Introduction
 
 10.2 Polypeptides
 
 10.2.1 2D NMR Assignment of ¯1H Resonances
 
 10.2.2 Determination of Polypeptide Conformation by 2D NMR
 
 10.3 Polynucleotides
 
 10.4 Polysaccharides
 
 11. Solid Polymers
 
 11.1 Introduction
 
 11.2 Solid–State Polymer Conformation
 
 11.3 Interchain Packing in Solid Polymers
 
 11.4 Molecular Motion in Solid Polymers
 
 11.5 Application of CPMAS/DD ¯13C NMR to Solid Polymers
 
 11.5.1 Morphology and Motion in Polymer Crystals
 
 11.5.2 Solid–Solid Polymer Phase Transitions
 
 11.6 Other Nuclei Observed In Solid–State Polymer Spectra
 
 11.6.1 CPMAS/DD ¯29Si NMR
 
 11.6.2 MAS/DD ¯31p NMR
 
 11.6.3 CPMAS/DD ¯15N NMR
 
 11.7 Concluding Remarks

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