
Handbook of High Field Dynamic Nuclear Polarization
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This comprehensive handbook is a compendium of the current state-of-the art of high field Dynamic Nuclear Polarization--from long-proven, early developments, up to today's hot topics. It covers all the relevant subjects that have made a direct or indirect contribution toward advancing this field, and focuses on topics such as: the theory behind the effects seen within DNP; instrumentation required for carrying out DNP; and specific applications of DNP including protein monitoring, catalysis, nanoparticles, biological and clinical studies. Development and application of techniques that have indirectly contributed to advancing MAS DNP NMR, such as DNP experiments on static solids within microwave resonant structures, and high-field EPR, are also examined.
Handbook of High Field Dynamic Nuclear Polarization is presented in three sections--Theoretical Aspects, DNP Development (instrumentation / radical / sample), and DNP NMR Applications. The first section offers chapters on; solid and cross effect DNP; thermal mixing; Overhauser; and dissolution DNP. The second looks at: microwave technology, gyrotron, and IOE; homebuilt and commercial DNP spectrometers; and glassing vs. solvent-free DNP. The final section provides information on; amyloid, membrane, and nanocrystalline proteins; metals, and surface enhanced DNP; pharmaceuticals; nanoparticles; and much more.
* Covers one of the biggest developing fields in magnetic resonance
* Relevant to students, academics, and industry within the physical, materials, medical, and biochemical sciences
* An excellent starting point and point-of-reference for researchers in the field
* Edited by a widely respected team with contributions from key researchers in the NMR community
* Part of the eMagRes Handbook Series
Handbook of High Field Dynamic Nuclear Polarization is an ideal reference for all researchers and graduate students involved in this complex, interdisciplinary field.
About eMagRes Handbooks
eMagRes publishes a wide range of online articles on all aspects of magnetic resonance in physics, chemistry, biology and medicine. The existence of this large number of articles, written by experts in various fields, is enabling the publication of a series of eMagRes Handbooks on specific areas of NMR and MRI. The chapters of each of these handbooks will comprise a carefully chosen selection of eMagRes articles. In consultation with the eMagRes Editorial Board, the eMagRes Handbooks are coherently planned in advance by specially-selected Editors, and new articles are written to give appropriate complete coverage. The handbooks are intended to be of value and interest to research students, postdoctoral fellows and other researchers learning about the scientific area in question and undertaking relevant experiments, whether in academia or industry.
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Persons
Editors
Vladimir K. Michaelis is Assistant Professor in the Department of Chemistry at the University of Alberta.
Robert G. Griffin is Professor of Chemistry and Director of the Francis Bitter Magnet Laboratory at the Massachusetts Institute of Technology.
Björn Corzilius is Professor of Physical Chemistry in the Institute of Chemistry at the University of Rostock.
Shimon Vega is Professor in the Department of Chemical Physics at the Weizmann Institute of Science, Israel.
Content
Contributors xi
Series Preface xvii
Preface xix
Acknowledgments xxi
Part A: Concepts, Theory, & Instrumentation 1
1 The Discovery and Demonstration of Dynamic Nuclear Polarization-A Personal and Historical Account 3
Charles P. Slichter
2 DNP Mechanisms 15
Krishnendu Kundu, Frédéric Mentink-Vigier, Akiva Feintuch, and Shimon Vega
3 Pulsed Dynamic Nuclear Polarization 71
Kong Ooi Tan, Sudheer Jawla, Richard J. Temkin, and Robert G. Griffin
4 MAS-DNP Enhancements: Hyperpolarization, Depolarization, and Absolute Sensitivity 87
Sabine Hediger, Daniel Lee, Frédéric Mentink-Vigier, and Gaël De Paëpe
5 Polarizing Agents: Evolution and Outlook in Free Radical Development for DNP 103
Gilles Casano, Hakim Karoui, and Olivier Ouari
6 Paramagnetic Metal Ions for Dynamic Nuclear Polarization 121
Björn Corzilius
7 Instrumentation for High-field Dynamic Nuclear Polarization NMR Spectroscopy 143
Guy M. Bernard and Vladimir K. Michaelis
8 Millimeter-wave Sources for DNP-NMR 155
Monica Blank and Kevin L. Felch
9 Cryogenic Platforms and Optimized DNP Sensitivity 169
Yoh Matsuki and Toshimichi Fujiwara
10 Versatile Dynamic Nuclear Polarization Hardware with Integrated Electron Paramagnetic Resonance Capabilities 189
Alisa Leavesley, Ilia Kaminker, and Songi Han
11 Dissolution Dynamic Nuclear Polarization Methodology and Instrumentation 219
Dennis Kurzbach and Sami Jannin
12 Introduction to Dissolution DNP: Overview, Instrumentation, and Human Applications 239
Jan H. Ardenkjaer-Larsen
13 Liquid-state Overhauser DNP at High Magnetic Fields 261
Vasyl P. Denysenkov and Thomas F. Prisner
14 Overhauser DNP in Liquids on 13C Nuclei 279
Marina Bennati and Tomas Orlando
Part B: Applications 289
15 DNP and Cellular Solid-state NMR 291
Alessandra Lucini Paioni, Marie A.M. Renault, and Marc Baldus
16 Cryo-trapped Intermediates of Retinal Proteins Studied by DNP-enhanced MAS NMR Spectroscopy 305
Johanna Becker-Baldus and Clemens Glaubitz
17 DNP Solid-state NMR of Biological Membranes 323
Burkhard Bechinger
18 DNP in Materials Science: Touching the Surface 337
Pierrick Berruyer, Lyndon Emsley, and Anne Lesage
19 Growing Signals from the Noise: Challenging Nuclei in Materials DNP 353
Frédéric A. Perras, Takeshi Kobayashi, and Marek Pruski
20 DNP-enhanced Solid-state NMR Spectroscopy of Active Pharmaceutical Ingredients 373
Li Zhao, Arthur C. Pinon, Lyndon Emsley, and Aaron J. Rossini
21 In Vivo Hyperpolarized 13C MRS and MRI Applications 405
Irene Marco-Rius and Arnaud Comment
22 Dissolution Dynamic Nuclear Polarization 421
Walter Köckenberger
Index 435
Contributors
Jan H. Ardenkjaer-Larsen Technical University of Denmark, Lyngby, Denmark; GE Healthcare, BrØndby, Denmark Chapter 12: Introduction to Dissolution DNP: Overview, Instrumentation, and Human Applications Marc Baldus Utrecht University, Utrecht, The Netherlands Chapter 15: DNP and Cellular Solid-state NMR Burkhard Bechinger Institut de Chimie, Université de Strasbourg/CNRS, UMR7177, Strasbourg, France Chapter 17: DNP Solid-state NMR of Biological Membranes Johanna Becker-Baldus Biophysical Chemistry & Centre for Biomolecular Magnetic Resonance, Goethe University Frankfurt, Frankfurt, Germany Chapter 16: Cryo-trapped Intermediates of Retinal Proteins Studied by DNP-enhanced MAS NMR Spectroscopy Marina Bennati Max Planck Institute for Biophysical Chemistry, Göttingen, Germany; University of Göttingen, Göttingen, Germany Chapter 14: Overhauser DNP in Liquids on 13C Nuclei Guy M. Bernard Gunning-Lemieux Chemistry Centre, University of Alberta, Edmonton, Canada Chapter 7: Instrumentation for High-field Dynamic Nuclear Polarization NMR Spectroscopy Pierrick Berruyer Institut des Sciences Analytiques, UMR 5280, University of Lyon, CNRS, Université Claude Bernard Lyon 1, ENS Lyon, Villeurbanne, France Chapter 18: DNP in Materials Science: Touching the Surface Monica Blank Communications and Power Industries (CPI), Palo Alto, CA, USA Chapter 8: Millimeter-wave Sources for DNP-NMR Gilles Casano CNRS, ICR, Aix Marseille University, Marseille, France Chapter 5: Polarizing Agents: Evolution and Outlook in Free Radical Development for DNP Arnaud Comment General Electric Healthcare, Chalfont St Giles, UK Chapter 21: In Vivo Hyperpolarized 13C MRS and MRI Applications Björn Corzilius Goethe University, Frankfurt, Germany Chapter 6: Paramagnetic Metal Ions for Dynamic Nuclear Polarization Vasyl P. Denysenkov Goethe University, Frankfurt-am-Main, Germany Chapter 13: Liquid-state Overhauser DNP at High Magnetic Fields Lyndon Emsley Institut des Sciences et Ingénierie Chimiques, Ecole Polytechnique Fédérale de Lausanne (EPFL), Lausanne, Switzerland Chapter 18: DNP in Materials Science: Touching the Surface Chapter 20: DNP-enhanced Solid-state NMR Spectroscopy of Active Pharmaceutical Ingredients Akiva Feintuch Chemical and Biological Physics Department, Weizmann Institute of Science, Rehovot, Israel Chapter 2: DNP Mechanisms Kevin L. Felch Communications and Power Industries (CPI), Palo Alto, CA, USA Chapter 8: Millimeter-wave Sources for DNP-NMR Toshimichi Fujiwara Institute for Protein Research, Osaka University, Suita, Osaka, Japan Chapter 9: Cryogenic Platforms and Optimized DNP Sensitivity Clemens Glaubitz Biophysical Chemistry & Centre for Biomolecular Magnetic Resonance, Goethe University Frankfurt, Frankfurt, Germany Chapter 16: Cryo-trapped Intermediates of Retinal Proteins Studied by DNP-enhanced MAS NMR Spectroscopy Robert G. Griffin Department of Chemistry, Francis Bitter Magnet Laboratory, Massachusetts Institute of Technology, Cambridge, MA, USA Chapter 3: Pulsed Dynamic Nuclear Polarization Songi Han Department of Chemistry and Biochemistry, University of California Santa Barbara, Santa Barbara, CA, USA; Department of Chemical Engineering, University of California Santa Barbara, Santa Barbara, CA, USA Chapter 10: Versatile Dynamic Nuclear Polarization Hardware with Integrated Electron Paramagnetic Resonance Capabilities Sabine Hediger Univ. Grenoble Alpes, CEA, CNRS, INAC-MEM, Grenoble, France Chapter 4: MAS-DNP Enhancements: Hyperpolarization, Depolarization, and Absolute Sensitivity Sami Jannin Université de Lyon, CNRS, Université Claude Bernard Lyon 1, ENS de Lyon, Institut des Sciences Analytiques, UMR 5280, Villeurbanne, France Chapter 11: Dissolution Dynamic Nuclear Polarization Methodology and Instrumentation Sudheer Jawla Plasma Science and Fusion Center, Massachusetts Institute of Technology, Cambridge, MA, USA Chapter 3: Pulsed Dynamic Nuclear Polarization Ilia Kaminker Department of Chemistry and Biochemistry, University of California Santa Barbara, Santa Barbara, CA, USA Chapter 10: Versatile Dynamic Nuclear Polarization Hardware with Integrated Electron Paramagnetic Resonance Capabilities Hakim Karoui CNRS, ICR, Aix Marseille University, Marseille, France Chapter 5: Polarizing Agents: Evolution and Outlook in Free Radical Development for DNP Takeshi Kobayashi U.S. DOE Ames Laboratory, Ames, IA, USA Chapter 19: Growing Signals from the Noise: Challenging Nuclei in Materials DNP Walter Köckenberger University of Nottingham, Nottingham, UK Chapter 22: Dissolution Dynamic Nuclear Polarization Krishnendu Kundu Chemical and Biological Physics Department, Weizmann Institute of Science, Rehovot, Israel Chapter 2: DNP Mechanisms Dennis Kurzbach Laboratoire des biomolécules, LBM, Département de chimie, école normale supérieure, PSL University, Sorbonne Université, CNRS, Paris, France Chapter 11: Dissolution Dynamic Nuclear Polarization Methodology and Instrumentation Alisa Leavesley Department of Chemistry and Biochemistry, University of California Santa Barbara, Santa Barbara, CA, USA Chapter 10: Versatile Dynamic Nuclear Polarization Hardware with Integrated Electron Paramagnetic Resonance Capabilities Daniel Lee Univ. Grenoble Alpes, CEA, CNRS, INAC-MEM, Grenoble, France Chapter 4: MAS-DNP Enhancements: Hyperpolarization, Depolarization, and Absolute Sensitivity Anne Lesage Institut des Sciences Analytiques, UMR 5280, University of Lyon, CNRS, Université Claude Bernard Lyon 1, ENS Lyon, Villeurbanne, France Chapter 18: DNP in Materials Science: Touching the Surface Alessandra Lucini Paioni Utrecht University, Utrecht, The Netherlands Chapter 15: DNP and Cellular Solid-state NMR Irene Marco-Rius Cancer Research UK Cambridge Institute, University of Cambridge, Cambridge, UK Chapter 21: In Vivo Hyperpolarized 13C MRS and MRI Applications Yoh Matsuki Institute for Protein Research, Osaka University, Suita, Osaka, Japan Chapter 9: Cryogenic Platforms...
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