Handbook of High Field Dynamic Nuclear Polarization

Description

Addresses Dynamic Nuclear Polarization (DNP) as a technique for sensitivity-enhancement in solid-state NMR spectroscopy 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. Have the content of this Handbook and the complete content of eMagRes at your fingertips! Visit: www.wileyonlinelibrary.com/ref/eMagRes Cover Title Page Copyright Editorial Board International Advisory Board Contents Contributors Series Preface Preface Acknowledgments Part A Concepts, Theory, & Instrumentation Chapter 1 The Discovery and Demonstration of Dynamic Nuclear Polarization – A Personal and Historical Account Introduction Graduate School Magnetic Resonance at Illinois Overhauser at Illinois Other Systems The Afterglow Acknowledgements References Chapter 2 DNP Mechanisms 2.1 Introduction 2.2 The Spin Systems 2.3 DNP Simulations of a Basic Spin System 2.4 Small Spin Systems as Model Systems for Macroscopic Samples 2.5 Large Spin Systems 2.6 The Spin Dynamics Leading to MAS-DNP Acknowledgments References Chapter 3 Pulsed Dynamic Nuclear Polarization 3.1 Introduction 3.2 Theory 3.3 Numerical Simulations 3.4 Instrumentation 3.5 Radicals for Pulsed DNP 3.6 Summary and Outlook Acknowledgments Related Article in Emagres References Chapter 4 MAS-DNP Enhancements: Hyperpolarization, Depolarization, and Absolute Sensitivity 4.1 Introduction 4.2 The Force of 𝜺on/off and its Dark Side 4.3 What Else Should We Consider? 4.4 Conclusions Acknowledgments Related Articles in Emagres References Chapter 5 Polarizing Agents: Evolution and Outlook in Free Radical Development for DNP 5.1 Introduction 5.2 Principle 5.3 Polarizing Agents (PAs) For MAS ssNMR/DNP 5.4 Outlook Acknowledgments Related Articles in Emagres References Chapter 6 Paramagnetic Metal Ions for Dynamic Nuclear Polarization 6.1 Introduction 6.2 EPR Properties of Paramagnetic Metal Ions 6.3 Nondegenerate Ground States: Anisotropic Zeeman Interaction 6.4 DNP Theory of High-Spin Systems 6.5 Practical Aspects of DNP With High-Spin Systems 6.6 Demonstrations of MAS DNP With Paramagnetic Metal Ions 6.7 Summary Acknowledgments Related Articles in Emagres References Chapter 7 Instrumentation for High-field Dynamic Nuclear Polarization NMR Spectroscopy 7.1 Introduction 7.2 Components of a DNP NMR System 7.3 Future Developments 7.4 Concluding Remarks Related Articles in Emagres References Chapter 8 Millimeter-wave Sources for DNP-NMR 8.1 Introduction 8.2 Solid-state Sources 8.3 Slow-wave Sources 8.4 Gyrotrons 8.5 Summary Related Articles in Emagres References Chapter 9 Cryogenic Platforms and Optimized DNP Sensitivity 9.1 Introduction 9.2 N2-Based MAS NMR Platform 9.3 He-Based MAS NMR Platforms 9.4 Cryogenically Optimized High-field DNP and Sensitivity 9.5 Summary and Outlook Related Articles in Emagres References Chapter 10 Versatile Dynamic Nuclear Polarization Hardware with Integrated Electron Paramagnetic Resonance Capabilities 10.1 Introduction 10.2 Hardware 10.3 Experimental Results 10.4 Conclusions Acknowledgments Related Articles in Emagres References Chapter 11 Dissolution Dynamic Nuclear Polarization Methodology and Instrumentation 11.1 Introduction 11.2 From Sample Preparation at Room Temperature to High Polarization at Low Temperatures 11.3 From Polarized Solids to the Liquid-state NMR or MRI Measurements 11.4 Commercial Designs and Instrumentational Aspects 11.5 Future Perspectives and Concluding Remarks Acknowledgments References Chapter 12 Introduction to Dissolution DNP: Overview, Instrumentation, and Human Applications 12.1 Introduction 12.2 Dynamic Nuclear Polarization 12.3 Electron Paramagnetic Agent (EPA) 12.4 Imaging Agents 12.5 DNP Sample Preparation 12.6 Dissolution and Relaxation in the Liquid State 12.7 dDNP Instrumentation 12.8 Imaging 12.9 Kinetic Modeling 12.10 Applications 12.11 Outlook Acknowledgement Related Articles in Emagres References Chapter 13 Liquid-state Overhauser DNP at High Magnetic Fields 13.1 Introduction 13.2 Theory of Overhauser DNP 13.3 Experimental Results 13.4 Summary and Outlook Conflicts of Interest Acknowledgments Related Articles in Emagres References Chapter 14 Overhauser DNP in Liquids on 13C Nuclei 14.1 Introduction 14.2 General Theory of Overhauser DNP in Liquids 14.3 Field Dependence of Coupling Factors for Mixed Dipolar and Scalar Relaxation 14.4 Experimental Results on Organic Molecules 14.5 Mechanistic Analysis 14.6 Perspectives Related Articles in Emagres References Part B Applications Chapter 15 DNP and Cellular Solid-state NMR 15.1 Introduction 15.2 Methodological Aspects of DNP-Supported Cellular ssNMR 15.3 Applications 15.4 Conclusions Acknowledgments Related Articles in Emagres References Chapter 16 Cryo-trapped Intermediates of Retinal Proteins Studied by DNP-enhanced MAS NMR Spectroscopy 16.1 Introduction 16.2 Cryo-trapping of Intermediate States 16.3 DNP-enhanced MAS NMR of Membrane Proteins 16.4 Retinal Proteins 16.5 Outlook Acknowledgments Related Articles in Emagres References Chapter 17 DNP Solid-state NMR of Biological Membranes 17.1 Introduction 17.2 Solid-state NMR of Membranes 17.3 Applications 17.4 Perspectives Acknowledgments Related Articles in Emagres References Chapter 18 DNP in Materials Science: Touching the Surface 18.1 Introduction 18.2 Principles of DNP Surface Enhanced NMR Spectroscopy 18.3 DNP Formulation for Surfaces 18.4 DNP Sens on Porous Materials 18.5 DNP Sens on Low Surface Area Materials 18.6 DNP Sens for the observation of Insensitive Surface Nuclei 18.7 Highly Reactive and Sensitive Materials 18.8 Conclusions References Chapter 19 Growing Signals from the Noise: Challenging Nuclei in Materials DNP 19.1 Introduction 19.2 Detection of Challenging Nuclei 19.3 Correlation Spectroscopy Involving Unreceptive and/or Rare Nuclei 19.4 Concluding Remarks Acknowledgments Related Articles in Emagres References Chapter 20 DNP-enhanced Solid-state NMR Spectroscopy of Active Pharmaceutical Ingredients 20.1 Introduction 20.2 Preparing Samples for DNP NMR Experiments 20.3 Modeling 1H Spin Diffusion in Relayed DNP Experiments 20.4 Applications of DNP-enhanced Solid-state NMR Spectroscopy to Pharmaceuticals 20.5 Conclusions and Future Perspectives Acknowledgments References Chapter 21 In Vivo Hyperpolarized 13C MRS and MRI Applications 21.1 Introduction 21.2 Early Results in Humans 21.3 Problems and Challenges 21.4 New Approaches 21.5 Preclinical and Cellwork as a Testbed for DNP Innovations 21.6 Conclusions Acknowledgments Related Articles in Emagres References Chapter 22 Dissolution Dynamic Nuclear Polarization 22.1 Introduction 22.2 Principle 22.3 Hardware 22.4 Strategies and Variants 22.5 Application 22.6 Outlook Related Articles in Emagres References Index EULA