This book describes nuclear magnetic resonance (NMR) methods which are used to study translational dynamics of molecules in different complex systems including systems made of synthetic and natural polymers, tissues and the porous heterogeneous systems of different types, such as cement and wood. The results of proton spin-lattice and spin-spin relaxation, cross-relaxation, pulse field gradient (PFG) NMR in studying diffusion properties and dynamics of molecules in polymer systems of different complexity are reported. In addition to these methods, reports on the use of the double-quantum-filtered (DQF) NMR technique in a study of slow molecular dynamics and properties of systems with anisotropic properties, such as water in hardening cement pastes, are presented. The book also covers applications of one and two dimensional NMR techniques.This book is a useful reference for readers learning different NMR techniques and their applications in civil engineering and biochemistry.

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Rodin, Victor V.

United States, United States of America

Nov 02, 2018

lg2554088

producers:
mPDF 5.7

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CONTENTS 6
FOREWORD 9
FOREWORD 1
9
FOREWORD 2
10
FOREWORD 3
11
FOREWORD 4
12
PREFACE 13
CONFLICT OF INTEREST 15
ACKNOWLEDGEMENT 15
DEDICATION 16
Basic Principles of NMR and Experimental Techniques 17
INTRODUCTION TO NMR 17
SPIN-LATTICE AND SPIN-SPIN NMR RELAXATION 21
Spin-Lattice (Longitudinal) Relaxation 22
Spin-Spin (Transverse) Relaxation 24
EXPERIMENTAL MATERIALS AND METHODS 26
NMR Techniques for Studying T1,T2 and Cross-Relaxation 28
Pulsed Field Gradient (PFG) NMR in One- and Two-Dimensional Studies 31
Cross-Relaxation in PFG NMR Studies 32
Double-Quantum-Filtered (DQF) NMR Spectroscopy 34
CONCLUDING REMARKS 37
REFERENCES 37
Dynamic Properties of Bound Water in Natural Polymers as Studied by NMR Relaxation 42
NATURAL SILK BOMBYX MORI WITH LOW WATER CONTENT 42
NMR RELAXATION IN NONORIENTED AND ORIENTED COLLAGEN FIBERS 51
NMR Relaxation in ECSD (Randomly Oriented) Collagen Samples 51
NMR Relaxation in Oriented Collagen Fibers 57
CONCLUDING REMARKS 63
REFERENCES 64
NMR Diffusion Studies of Water in Natural Biopolymers 70
1H NMR STUDY OF THE SELF-DIFFUSION OF WATER IN CROSS-LINKED COLLAGENS 70
SELF-DIFFUSION OF WATER IN BOMBYX MORI SILK AS STUDIED BY NMR 75
CONCLUDING REMARKS 80
REFERENCES 80
Collagen Tissues with Different Degree of
Cross-Links and Natural Silk as Studied by
1H DQF NMR 84
1H DQF NMR SPECTROSCOPY IN STUDYING COLLAGENS WITH DIFFERENT DEGREE OF CROSS-LINKS 84
1H DQF NMR STUDY OF BOMBYX MORI SILK 93
CONCLUDING REMARKS 96
REFERENCES 96
NMR Relaxation and Restricted Self-Diffusion of Water in Wood 98
INTRODUCTION: WATER IN WOOD 98
STUDYING NMR RELAXATION IN WOOD: FROM WET TO DRIED WOOD 99
RESTRICTED DIFFUSION OF WATER IN WOOD: ONE-DIMENSIONAL PFG NMR STUDIES 103
CONCLUDING REMARKS 109
ACKNOWLEDGEMENTS 110
REFERENCES 110
2D Diffusion-Diffusion Correlation NMR Spectroscopy in Study of Diffusion Anisotropy
in Wood 113
INTRODUCTION 113
THEORY AND MODELS IN DIFFUSION-DIFFUSION CORRELATION SPECTROSCOPY (DDCOSY) 114
DDCOSY WITH PARALLEL ORIENTED PAIRS OF GRADIENTS. SIMULATIONS AND EXPERIMENTS ON WOOD 117
2D DDCOSY WITH PERPENDICULAR PAIRS OF GRADIENTS. INVERSE LAPLACE TRANSFORM IN STUDYING DIFFUSION ANISOTROPY IN WOOD 118
CONCLUSION 122
ACKNOWLEDGEMENTS 123
REFERENCES 123
PFG NMR in Studying Solutions of Carboxylated Acrylic Polymers 126
INTRODUCTION: CARBOXYLATED ACRYLIC POLYMERS 127
SELF-DIFFUSION OF SOLVENT AND POLYMER IN SOLUTIONS OF RANDOM COPOLYMERS IN ISOPROPANOL 128
EFFECT OF POLYMER CONCENTRATION AND BMA/MAA MOLAR RATIO ON HYDROGEN BONDING IN NEUTRALIZED COPOLYMERS 131
SOLVENT AND POLYMER DIFFUSION STUDIES IN NEUTRALISED COPOLYMERS 135
Solvent Diffusion: Effect of mol% BMA in BMA-MAA Random Copolymers and Polymer Concentration at Neutralisation Level TEA:COOH = 1:1 135
Polymer Diffusion: Effect of BMA/MAA Molar Ratio at Neutralisation Level TEA:COOH=1:1 138
Polymer and Solvent Diffusion: Different Neutralisation Level (TEA:COOH = 1:1; 0.75:1 and 0.5:1) 139
CONCLUDING REMARKS 141
ACKNOWLEDGEMENTS 142
REFERENCES 142
Copolymer Films Swollen in Water: NMR Relaxation and PFG NMR techniques in Studying Polymer-Water Interactions 146
POLYMER FILMS AND WATER 146
DRIED AND WET POLYMER FILMS: 1H NMR SPECTRA AND T2 STUDIES OF WATER-POLYMER INTERACTIONS 148
Films in Experimental Conditions 148
Dried and Wet Polymer Films: NMR Spectra, FIDs and NMR relaxation Times 148
WATER SELF-DIFFUSION IN THE COPOLYMER FILMS 159
CONCLUDING REMARKS 161
ACKNOWLEDGEMENTS 162
REFERENCES 162
Magnetic Resonance Imaging in Characterisation of Polymer films 166
INTRODUCTION 166
POLYMER FILMS SWOLLEN IN WATER AS STUDIED BY FIDS, T2 AND MRI 167
NMR AND MRI IN STUDYING EVAPORATION OF WATER FROM THE FILMS 173
CONCLUDING REMARKS 176
ACKNOWLEDGEMENTS 176
REFERENCES 176
Self-Diffusion of Water in Cement Pastes as Studied by 1H PFG NMR and DDCOSY NMR 179
INTRODUCTION 179
METHODS AND MODELS 180
Methods of Spin Echo and Stimulated Echo in PFG Experiments 181
DDCOSY Experiments in Studying Anisotropy 184
COMPARISON OF PULSE SEQUENCES IN CEMENT STUDIES 186
SELF-DIFFUSION OF WATER IN CEMENT PASTE 187
Early Hydration of Cement Paste as Studied by 1-dimensional PFG NMR 187
DDCOSY in Studying Early Cement Hydration 189
Pore Size Distribution and Self-diffusion of Water in Mature Cement Paste 190
CONCLUDING REMARKS 192
ACKNOWLEDGEMENTS 192
REFERENCES 192
Characterisation of Hydrated Cement Pastes by 1H DQF NMR Spectroscopy 196
1D AND 2D 1H NMR RELAXATION 196
METHODS AND THEORY: MODEL STUDIES 204
DOUBLE-QUANTUM-FILTERED (DQF) SIGNALS: DEPENDENCE ON SAMPLE CURING AND ON CREATION TIME. PAKE DOUBLET 210
DQF LINE SHAPE 218
DQF AND DRYING THE SAMPLES: EXCHANGEABLE WATER 221
CONCLUDING REMARKS 225
ACKNOWLEDGEMENTS 226
REFERENCES 226
SUBJECT INDEX 230

2020-06-25