Single-Sided NMR (eBook)

Currently an Assistant Editor for the journal Cell, Michaeleen Doucleff obtained her PhD in Chemistry from the University of California, Berkeley while working in the laboratory of David E. Wemmer. Doucleff then became a Nancy Nossal postdoctoral fellow at the National Institute's of Health in the laboratory of G. Marius Clore. Throughout her career, she has used NMR spectroscopy and X-ray crystallography to characterize the structure and dynamics of transcription factors and their interaction with DNA.Mary Hatcher-Skeers is a Professor of Chemistry in the Joint Science Department of Claremont McKenna, Pitzer and Scripps Colleges in Claremont CA.  She teaches General Chemistry, Biochemistry, Physical Chemistry and NMR Spectroscopy.  Hatcher-Skeers received her PhD in Chemistry from the University of Washington while working in the laboratory of Gary Drobny.  She was then a NIH Post-Doctoral Fellow in the labs of Judith Herzfeld at Brandeis University and Robert Griffin at MIT.  Professor Hatcher-Skeers’ research uses solid-state and solution NMR spectroscopy to investigate the role of DNA structure and dynamics in protein and drug binding.  She has trained over 70 undergraduates in her research lab, a number who have gone on to graduate programs in chemistry and biochemistry.Nicole Crane, Ph.D. is currently a Scientist at the Naval Medical Research Center in Silver Spring, MD where she is establishing the Regenerative Medicine Department’s Advanced Imaging Program.  Her research focuses on development and utilization of spectroscopic techniques to improve understanding of the wound healing process, particularly in traumatic acute wounds, as well as identifying and quantifying transplant-associated ischemia and reperfusion injury. Her experience as an applied spectroscopist includes applications in forensics, pharmaceuticals, and biomedicine. Dr. Crane has published over fifteen peer-reviewed publications and presented at numerous regional and national scientific meetings. She is also an inventor on two US patents. 

Preface 4
Contents 7
Contributors 11
1 Single-Sided NMR 12
Federico Casanova, Juan Perlo, and Bernhard Blümich 12
1.1 Development of Open NMR Sensors 13
1.1.1 Well-Logging Tools 13
1.1.2 Mobile Single-Sided Sensors 14
1.1.3 The NMR-MOUSE 15
1.2 Methods for Mobile NMR 17
References 18
2 NMR in Inhomogeneous Fields 22
Federico Casanova and Juan Perlo 22
2.1 Introduction 22
2.1.1 Evolution of the Magnetization During a Pulse Sequence 23
2.1.2 Separation of the Magnetization into Coherence Pathways 25
2.1.3 Numerical Calculation of the NMR Signal 31
2.2 Pulse Sequence Analysis 32
2.2.1 Single rf Pulse 32
2.2.2 The Generation of Hahn Echoes 34
2.2.3 The CPMG Sequence 39
2.2.4 Inversion and Saturation Recovery 46
2.2.5 Diffusion Measurements 53
2.3 The SNR in Inhomogeneous Fields 58
2.3.1 The Reciprocity Principle 59
2.3.2 Numerical Calculations of the SNR 60
2.3.3 An Analytical Solution for the SNR 66
References 66
3 Ex Situ Measurement of One- and Two-Dimensional Distribution Functions 68
Martin D. Hürlimann 68
3.1 Introduction 68
3.1.1 Relaxation 68
3.1.2 Diffusion 69
3.1.3 Diffusion--Relaxation Distribution Functions 69
3.2 Pulse Sequences and Spin Dynamics in Inhomogeneous Fields 70
3.2.1 Relaxation Measurement: Carr-Purcell-Meiboom-Gill Sequence 70
3.2.2 Diffusion Measurements with Static Gradients 73
3.2.3 T1 Measurements in Inhomogeneous Fields 75
3.3 One-Dimensional Distribution Functions 75
3.3.1 Data Inversion 76
3.3.2 Regularization 78
3.3.3 Systematic Errors 79
3.3.4 Uncertainties 79
3.4 Two-Dimensional Diffusion--Relaxation Distribution Functions 80
3.4.1 Two-Dimensional Diffusion-Relaxation Measurements 80
3.4.2 Data Analysis 82
3.4.3 Interpretation of Distribution Functions 84
3.5 Applications of Two-Dimensional Distribution Functions 85
3.5.1 Two-Component Systems 86
3.5.2 Wettability 87
3.5.3 Complex Miscible Fluid 88
3.5.4 Structured Fluid 89
3.5.5 Pore Geometry of Porous Media 90
3.6 Conclusion 92
References 93
4 Magnets and Coils for Single-Sided NMR 97
Juan Perlo 97
4.1 Magnets 98
4.1.1 B0 Perpendicular to the Sensor Surface, the Bar Magnet Geometry 99
4.1.2 B0 Parallel to the Sensor Surface, the U-Shaped Geometry 103
4.1.3 Magnets for Depth Profiling 105
4.1.4 Sweet-Spot Magnets 109
4.2 RF Coils 112
4.2.1 Coils for Depth Profiling 113
4.2.2 Coils for Sweet-Spot Magnets 115
4.3 Gradient Coils 117
References 118
5 Single-Sided Tomography 121
Federico Casanova 121
5.1 Depth Resolution Using the Static Field Gradient 121
5.2 Spatial Encoding by Fourier Imaging 123
5.3 Multi-Echo Acquisition Schemes 127
5.3.1 RARE-Like Imaging Sequence 127
5.3.2 CPMG-CP for Quadrature Detection 131
5.4 Performance of the Multi-Echo Detection Scheme 135
5.4.1 Sensitivity Improvement 135
5.4.2 Relaxation and Diffusion Contrast 136
5.4.3 3D Imaging 138
5.5 Displacement Encoding 139
5.5.1 PFG Methods in Inhomogeneous Fields 140
5.5.2 Measurement of Velocity Distributions 145
5.6 Spatially Resolved Velocity Distributions 147
5.6.1 2D Velocity Maps 147
References 150
6 High-Resolution NMR in Inhomogeneous Fields 152
Vasiliki Demas, John M. Franck, Jeffrey A. Reimer, and Alexander Pines 152
6.1 Introduction 152
6.2 Approaches Based on Spin Interactions 153
6.3 Ex Situ NMR: Spatially Dependent ``z-Rotations'' 154
6.3.1 Ex Situ Matching: Compensating Static Field Inhomogeneities via Spatially Matched rf 156
6.3.2 Shim Pulses: Corrections Based on Gradient Modulations During an Adiabatic Double Passage 166
6.3.3 Adjusted Chirp Shim Pulses 169
6.4 Summary 171
References 171
7 High-Resolution Spectroscopy in Highly Homogeneous Stray Fields 174
Ernesto P. Danieli 174
7.1 Sensor Design 175
7.1.1 Main Unit 175
7.1.2 Shim Unit 176
7.2 Shimming Magnetic Fields with Movable Permanent Magnets 179
7.2.1 Generation of Linear Terms Along y 180
7.2.2 Generation of Linear Terms Along x and z 181
7.2.3 Generation of Quadratic Terms x2 and z2 181
7.3 Experimental Results 184
7.4 Shimming the Magnet to Higher Order 186
7.4.1 Improving Resolution and Working Volume Size 187
7.5 Temperature Compensation 190
7.6 Conclusions 194
References 194
8 Applications in Biology and Medicine 196
Bernhard Blümich 196
8.1 Skin 197
8.2 Tendon 201
8.3 Mummies and Bones 203
8.4 Unilateral Imaging of Biological Matter 205
8.5 Conclusions 207
References 208
9 Applications in Material Science and Cultural Heritage 212
Jürgen Kolz 212
9.1 Elastomers 213
9.1.1 Crosslink Density 213
9.1.2 Aging 215
9.1.3 Imaging 218
9.2 Hard Polymers 221
9.2.1 Ingress of Solvents 224
9.3 Cultural Heritage 226
References 228
10 Spectrometer Hardware 230
Jörg Felder 230
10.1 Single-Sided vs. Conventional: Systematic Differences 231
10.2 Frontend Design 232
10.2.1 Matching and Balancing 232
10.2.2 Transmit-Receive Switching 235
10.3 Transmitter Design 237
10.3.1 Conventional Power Amplifiers 238
10.3.2 Alternative Amplifier Designs 239
10.4 Receiver Design 242
10.4.1 Low-Noise Amplifier 243
10.4.2 Frequency Generation and Mixing 244
10.5 Digital Hardware 246
10.5.1 Frontend Signal Processor Selection 246
10.5.2 Digital Phase Sensitive Detector 248
References 248
Index 250