NMR Spectroscopy
of Polymers
by K. Hatada

This reference volume places emphasis on the practical use of NMR Spectroscopy in polymer chemistry rather than the theoretical treatments.

Based on the author's extensive experimental experience, topics covered include:

• Experimental problems such as preparatio of sample solution, selection of solvent, internal standard and tube, and contaminants in sample solution
• Accuracy and precision of NMR measurements required in the analysis of polymer structure such as tacticity, copolymer composition and chain end structures
• Volume magnetic susceptibility by NMR
• Stereochemistry of polymer chains, chemical composition and comonomer sequence distribution in copolymers, and end groups and irregular linkages
• On-line coupled size exclusion chromatography (SEC) and NMR spectroscopy (SEC/NMR) in which an NMR spectrometer is set in the SEC system as a detector.

Contents

1. Introduction to NMR Spectroscopy
   • Basic Principles of NMR
   • Spectrometers
   • Observable Nuclei
   • Sample Preparation
   • Outline of NMR Measurement

2. Measurement of Spectrum with High Qualtiy including Quantitative Analysis
   • Effects of Operating Conditions
   • Reliability of Chemical Shift and Signal Intensity
   • Determination of Absolute Signal Intensity
   • Microanalysis by NMR Spectroscopy
   • Determination of Volume Magnetic Susceptibility by NMR

3. Stereochemistry of Polymers
   • Definition of Tacticity
   • Methods of Stereochemical Peak Assignments
   • Quantitative Determination of Tacticity
   • Sequence Statistics and Propagation Mechanism

4. Copolymer
   • NMR Analysis of Composition and Sequence in Copolymers
   • Chemical Shift Calculation for Peak Assignment of Hydrocarbon Copolymer
   • Monomer Reactivity Ratios and Statistical Treatments
   • Analysis of Diene Polymers

5. NMR for the Study of Polymerization Reactions
   • Analysis of End Group and Structural Defects in Polymer Chains
   • Analysis of Polymerization Reaction
   • Chemical Shifts of Vinyl Monomer and Their Reactivities

6. Two-Dimensional NMR Spectroscopy
   • Principles of 2D NMR
   • ¹H COSY (2D Correlation Spectroscopy)
   • ¹³C-¹H COSY (¹³C-¹H HETCOR)
   • Heteronuclear Multiple-Band Correlation Spectroscopy
   • Two-dimensional Nuclear Overhauser Enhancement Spectroscopy
   • Conformation Analysis by 2D NMR
   • Incredible Natural Abundance Double Quantum Transfer Experiment
   • J-Resolved Spectroscopy

7. NMR Relaxation
   • Basic Principles of NMR Relaxation
   • Measurement of T₁ and NOE
   • Sample Preparation – Effect of Oxygen and Type of Sample Tube
   • Reliability of Spin–Lattice Relaxation Time and NOE
   • Effect of Frequency, Temperature, Solution Concentration and Solvent on the Measurement of T₁ and NOE
   • Tacticity Dependence of ¹H T₁ and ¹³C T₁ Values and NOE
   • Molecular Weight Dependence of ¹³C T₁

8. On-Line SEC/NMR Analysis of Polymers
   • SEC/NMR Instrumentation
   • Molecular Weight Determination of Polymers by SEC/NMR
   • Studies on Molecular Weight Dependence of Copolymer Composition and Tacticity
   • Simple and Accurate Analysis of Oligomers

Index

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