High-resolution High-frequency Dynamic Nuclear Polarization for Biomolecular Solid State NMR PDF Download
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Author: Alexander Benjamin Barnes
Publisher:
ISBN:
Category :
Languages : en
Pages : 252
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Book Description
Dynamic Nuclear Polarization (DNP) has exploded in popularity over the last few years, finally realizing its potential to overcome the detrimental lack of sensitivity that has plagued performing NMR experiments. Applied to magic angle spinning (MAS) experiments, this renaissance of DNP has been primarily driven by the development of instrumentation; namely gyrotron oscillators as high-power stable microwave power sources and the NMR probes and associated equipment required to spin samples routinely below 100 Kelvin. The first three chapters of this thesis provide an overview of the theory, instrumentation, and applications of DNP. Chapter 1 introduces the magnetic resonance Hamiltonian with a focus on interactions that are necessary to control in order to obtain high-resolution DNP spectra. Chapters 2 and 3 are published reviews of DNP. Whereas Chapter 2 targets magnetic resonance spectroscopists, Chapter 3 is intended for an electric engineering audience. Both reviews are included as the associated depth and coverage of the topics are complementary and lead to a better understanding of DNP. The later chapters describe in detail advancements in probe, cryogenics, and gyrotron technology required to perform DNP MAS experiments, as well as the gains in sensitivity and resolution such instrumentation has permitted. Of particular importance is the development of a cryogenic sample ejection system that resulted in exquisite resolution of spectra recorded 100 K, both of crystalline peptide and the active site of membrane proteins. Such developments in instrumentation and demonstrations of resolution go towards overturning a long-held stance in the field that DNP would always suffer from broadened, unresolved spectra. Such techniques also allow us to investigate site specific dynamics of a crystalline peptide, the high resolution SSNMR structure of which is discussed in Chapter 3. DNP and the developed instrumentation is also leveraged to measure inter-atomic distances in the active site of a membrane protein with sub-angstrom precision. Chapters 7 describes the calculation of the microwave field strength across the sample in a MAS DNP probe and introduces strategies to increase it. Finally Chapter 8 introduces a major advance in the microwave source technology associated with DNP experiments. Detailed designs of a novel 250 GHz gyrotron oscillator are shown and experiments demonstrate a continuous broad 3 GHz bandwidth with 10 W across the band, which results in substantially improved DNP performance.
Author: Alexander Benjamin Barnes
Publisher:
ISBN:
Category :
Languages : en
Pages : 252
Get Book Here
Book Description
Dynamic Nuclear Polarization (DNP) has exploded in popularity over the last few years, finally realizing its potential to overcome the detrimental lack of sensitivity that has plagued performing NMR experiments. Applied to magic angle spinning (MAS) experiments, this renaissance of DNP has been primarily driven by the development of instrumentation; namely gyrotron oscillators as high-power stable microwave power sources and the NMR probes and associated equipment required to spin samples routinely below 100 Kelvin. The first three chapters of this thesis provide an overview of the theory, instrumentation, and applications of DNP. Chapter 1 introduces the magnetic resonance Hamiltonian with a focus on interactions that are necessary to control in order to obtain high-resolution DNP spectra. Chapters 2 and 3 are published reviews of DNP. Whereas Chapter 2 targets magnetic resonance spectroscopists, Chapter 3 is intended for an electric engineering audience. Both reviews are included as the associated depth and coverage of the topics are complementary and lead to a better understanding of DNP. The later chapters describe in detail advancements in probe, cryogenics, and gyrotron technology required to perform DNP MAS experiments, as well as the gains in sensitivity and resolution such instrumentation has permitted. Of particular importance is the development of a cryogenic sample ejection system that resulted in exquisite resolution of spectra recorded 100 K, both of crystalline peptide and the active site of membrane proteins. Such developments in instrumentation and demonstrations of resolution go towards overturning a long-held stance in the field that DNP would always suffer from broadened, unresolved spectra. Such techniques also allow us to investigate site specific dynamics of a crystalline peptide, the high resolution SSNMR structure of which is discussed in Chapter 3. DNP and the developed instrumentation is also leveraged to measure inter-atomic distances in the active site of a membrane protein with sub-angstrom precision. Chapters 7 describes the calculation of the microwave field strength across the sample in a MAS DNP probe and introduces strategies to increase it. Finally Chapter 8 introduces a major advance in the microwave source technology associated with DNP experiments. Detailed designs of a novel 250 GHz gyrotron oscillator are shown and experiments demonstrate a continuous broad 3 GHz bandwidth with 10 W across the band, which results in substantially improved DNP performance.
Author: Vladimir K. Michaelis
Publisher: John Wiley & Sons
ISBN: 1119441668
Category : Science
Languages : en
Pages : 920
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Book 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
Author: Gareth R. Eaton
Publisher: Springer Science & Business Media
ISBN: 3211929487
Category : Science
Languages : en
Pages : 192
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Book Description
There is a growing need in both industrial and academic research to obtain accurate quantitative results from continuous wave (CW) electron paramagnetic resonance (EPR) experiments. This book describes various sample-related, instrument-related and software-related aspects of obtaining quantitative results from EPR expe- ments. Some speci?c items to be discussed include: selection of a reference standard, resonator considerations (Q, B ,B ), power saturation, sample position- 1 m ing, and ?nally, the blending of all the factors together to provide a calculation model for obtaining an accurate spin concentration of a sample. This book might, at ?rst glance, appear to be a step back from some of the more advanced pulsed methods discussed in recent EPR texts, but actually quantitative “routine CW EPR” is a challenging technique, and requires a thorough understa- ing of the spectrometer and the spin system. Quantitation of CW EPR can be subdivided into two main categories: (1) intensity and (2) magnetic ?eld/mic- wave frequency measurement. Intensity is important for spin counting. Both re- tive intensity quantitation of EPR samples and their absolute spin concentration of samples are often of interest. This information is important for kinetics, mechanism elucidation, and commercial applications where EPR serves as a detection system for free radicals produced in an industrial process. It is also important for the study of magnetic properties. Magnetic ?eld/microwave frequency is important for g and nuclear hyper?ne coupling measurements that re?ect the electronic structure of the radicals or metal ions.
Author: Souheil James Inati
Publisher:
ISBN:
Category :
Languages : en
Pages : 161
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Book Description
Author: M. Mehring
Publisher: Springer Science & Business Media
ISBN: 3642687563
Category : Science
Languages : en
Pages : 352
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Book Description
The field of Nuclear Magnetic Resonance (NMR) has developed at a fascinating pace during the last decade. It always has been an extremely valuable tool to the organic chemist by supplying molecular "finger print" spectra at the atomic level. Unfortunately the high resolution achievable in liquid solutions could not be obtained in solids and physicists and physical chemists had to live with unresolved lines open to a wealth of curve fitting procedures and a vast amount of speculations. High resolution NMR in solids seemed to be a paradoxon. Broad structure less lines are usually encountered when dealing with NMR in solids. Only with the recent advent of mUltiple pulse, magic angle, cross-polarization, two-dimen sional and multiple-quantum spectroscopy and other techniques during the last decade it became possible to resolve finer details of nuclear spin interactions in solids. I have felt that graduate students, researchers and others beginning to get involved with these techniques needed a book which treats the principles, theo retical foundations and applications of these rather sophisticated experimental techniques. Therefore I wrote a monograph on the subject in 1976. Very soon new ideas led to the developement of "two-dimensional spectroscopy" and "multiple-quantum spectroscopy", topics which were not covered in the first edition of my book. Moreover an exponential growth of literature appeared in this area of research leaving the beginner in an awkward situation of tracing back from a current article to the roots of the experiment.
Author: Frances Separovic
Publisher: Royal Society of Chemistry
ISBN: 1849739102
Category : Science
Languages : en
Pages : 632
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Book Description
Advances in Biological NMR brings the reader up to date with chapters from international leaders of this growing field, covering the most recent developments in the methodology and applications of solid state NMR to studies of membrane interactions and molecular motions
Author: Chukun Gao
Publisher:
ISBN:
Category :
Languages : en
Pages : 119
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Book Description
Author: Roderick E. Wasylishen
Publisher: John Wiley & Sons
ISBN: 1118588843
Category : Science
Languages : en
Pages : 564
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Book Description
NMR OF QUADRUPOLAR NUCLEI IN SOLID MATERIALS Over the past 20 years technical developments in superconducting magnet technology and instrumentation have increased the potential of NMR spectroscopy so that it is now possible to study a wide range of solid materials. In addition, one can probe the nuclear environments of many other additional atoms that possess the property of spin. In particular, it is possible to carry out NMR experiments on isotopes that have nuclear spin greater that 1⁄2 (i.e. quadrupolar nuclei). Since more that two-thirds of all NMR active isotopes are quadrupolar nuclei, applications of NMR spectroscopy with quadrupolar nuclei are increasing rapidly. The purpose of this handbook is to provide under a single cover the fundamental principles, techniques and applications of quadrupolar NMR as it pertains to solid materials. Each chapter has been prepared by an expert who has made significant contributions to out understanding and appreciation of the importance of NMR studies of quadrupolar nuclei in solids. The text is divided into three sections: The first provides the reader with the background necessary to appreciate the challenges in acquiring and interpreting NMR spectra of quadrupolar neclei in solids. The second presents cutting-edge techniques and methodology for employing these techniques to investigate quadrupolar nuclei in solids. The final section explores applications of solid-state NMR studies of solids ranging from investigations of dynamics, characterizations of biological samples, organic and inorganic materials, porous materials, glasses, catalysts, semiconductors and high-temperature superconductors. About EMR Handbooks The Encyclopedia of Magnetic Resonance (EMR) 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 EMR Handbooks on specific areas of NMR and MRI. The chapters of each of these handbooks will comprise a carefully chosen selection of Encyclopedia articles. In consultation with the EMR Editorial Board, the EMR Handbooks are coherently planned in advance by specially-selected Editors, and new articles, are written (together with updates of some already existing articles) 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 the Encyclopedia of Magnetic Resonance at your fingertips! Visit: www.wileyonlinelibrary.com/ref/emr
Author: The Nuclear Magnetic Resonance Society of Japan
Publisher: Springer
ISBN: 9811059667
Category : Science
Languages : en
Pages : 634
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Book Description
This book describes the advanced developments in methodology and applications of NMR spectroscopy to life science and materials science. Experts who are leaders in the development of new methods and applications of life and material sciences have contributed an exciting range of topics that cover recent advances in structural determination of biological and material molecules, dynamic aspects of biological and material molecules, and development of novel NMR techniques, including resolution and sensitivity enhancement. First, this book particularly emphasizes the experimental details for new researchers to use NMR spectroscopy and pick up the potentials of NMR spectroscopy. Second, the book is designed for those who are involved in either developing the technique or expanding the NMR application fields by applying them to specific samples. Third, the Nuclear Magnetic Resonance Society of Japan has organized this book not only for NMR members of Japan but also for readers worldwide who are interested in using NMR spectroscopy extensively.
Author: Gregory S. Nusinovich
Publisher: JHU Press
ISBN: 1421429411
Category : Science
Languages : en
Pages : 352
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Book Description
As unique sources of coherent high-power, microwave, and millimeter-wave radiation, gyrotrons are an essential part of the hunt for controlled fusion. Presently, gyrotrons are actively used for electron cyclotron resonance plasma heating and current drive in various controlled fusion reactors. These sources have been under development in many countries for more than forty years. In spite of their widespread use, however, there is as yet no single book to introduce non-specialists to this vital field. Now Gregory S. Nusinovich, an early pioneer of the gyrotron and widely regarded today as the world's leading authority on the subject, explains the fundamental physical principles upon which gyrotrons and related devices operate. Nusinovich first sets forth some "rules of thumb" that allow readers to understand gyrotron operation in simple terms. He then explores the fundamentals of the general theory of gyrotrons and offers an overview of the various types of gyro-devices, including gyromonotrons, gyroklystrons, gyro-traveling-wave tubes, and gyrotwystrons. He explains not only the theory, linear and nonlinear, but also the practical challenges that users of such devices face. This book will be of interest to undergraduate and graduate students as well as to those who develop gyrotrons or who use them in various applications. It should also appeal to plasma physicists interested in charged-particle dynamics, as well as to applied physicists needing to know more about micro- and millimeter-wave technologies.
