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Books > Science & Mathematics > Chemistry > Analytical chemistry > Qualitative analytical chemistry
Nuclear magnetic resonance (NMR) is an analytical tool used by chemists and physicists to study the structure and dynamics of molecules. In recent years, no other technique has grown to such importance as NMR spectroscopy. It is used in all branches of science where precise structural determination is required and where the nature of interactions and reactions in solution is being studied.
This book focuses on recently developed crystal growth techniques to grow large and high quality superconducting single crystals. The techniques applied are traveling solvent floating zone (TSFZ) with infrared image furnace, Bridgeman, solution/flux and top seeded solution growth (TSSG) methods. The materials range from cuprates, cobaltates to pnictides including La2CuO4-based (LCO), YBa2Cu3O7-d (YBCO), Bi2Sr2Can 1CunO2n+4+ (n=1,2,3) (BSCCO) to NaxCoO2. The modified Bridgman "cold finger" method is devoted to the pnictide system with the best quality (transition width DTc~0.5 K) with highest Tc~38.5 K of Ba0.68K0.32Fe2A2. The book presents various iron-based superconductors with different structures, such as 1111, 122, 111, 11 and 42622,10-3-8. Detailed single crystal growth methods (fluxes, Bridgman, floating zone), the associated procedures and their impact to crystal size and quality are presented. The book also describes the influence of doping on the structure and the electric, magnetic, and superconducting properties of these compounds in a comparative study of different growth methods. It describes particularly under-, optimal and over-doped with oxygen cuprates (LCO, YBCO and BSCCO) and hole/electron/isovalently doped parent compounds AFe2As2 (A = Ba, Sr, Ca) (122), chalcogenides AxFe2-ySe2(A = K, Rb, Cs) (122), and Fe1-dTe1-xSex (11). A review of the current growth technologies and future growth efforts handling volatile and poisonous components are also presented.
In this thesis, the ionization of atoms and small molecules in strong laser fields is experimentally studied using a reaction microscope. The population of autoionizing doubly excited states in the laser fields is proven and a possible connection to the well-known dielectronic recombination processes is discussed. The fundamental process of tunnel ionization in strong laser fields is subject of investigation in a pump-probe experiment with ultrashort laser pulses. A coherent superposition of electronic states in singly charged argon ions is created within the first, and subsequently tunnel-ionized with the second pulse. This gives access to state-selective information about the tunneling process and allows to test common models. Moreover, the ionization of krypton and argon at different wavelengths is studied, from the multiphoton to the tunneling regime. The wavelength-dependent investigations are furthermore extended to molecular hydrogen. In addition to ionization, this system might undergo different dissociative processes. Channel-selective electron momentum distributions are presented and compared to each other.
Proceedings of the 31st International Conference on the
Applications of the Mossbauer Effect (ICAME 2011) held in Kobe,
Japan, September 25-30, 2011 Reprint from Hyperfine Interactions"
This book explains concepts of transmission electron microscopy (TEM) and x-ray diffractometry (XRD) that are important for the characterization of materials. The fourth edition adds important new techniques of TEM such as electron tomography, nanobeam diffraction, and geometric phase analysis. A new chapter on neutron scattering completes the trio of x-ray, electron and neutron diffraction. All chapters were updated and revised for clarity. The book explains the fundamentals of how waves and wavefunctions interact with atoms in solids, and the similarities and differences of using x-rays, electrons, or neutrons for diffraction measurements. Diffraction effects of crystalline order, defects, and disorder in materials are explained in detail. Both practical and theoretical issues are covered. The book can be used in an introductory-level or advanced-level course, since sections are identified by difficulty. Each chapter includes a set of problems to illustrate principles, and the extensive Appendix includes laboratory exercises.
The problem of conventional, low-temperature superconductivity has been regarded as solved since the seminal work of Bardeen, Cooper, and Schrieffer (BCS) more than 50 years ago. However, the theory does not allow accurate predictions of some of the most fundamental properties of a superconductor, including the superconducting energy gap on the Fermi surface. This thesis describes the development and scientific implementation of a new experimental method that puts this old problem into an entirely new light. The nominee has made major contributions to the development and implementation of a new experimental method that enhances the resolution of spectroscopic experiments on dispersive lattice-vibrational excitations (the "glue" responsible for Cooper pairing of electrons in conventional superconductors) by more than two orders of magnitude. Using this method, he has discovered an unexpected relationship between the superconducting energy gap and the geometry of the Fermi surface in the normal state, both of which leave subtle imprints in the lattice vibrations that could not be resolved by conventional spectroscopic methods. He has confirmed this relationship on two elemental superconductors and on a series of metallic alloys. This indicates that a mechanism qualitatively beyond the standard BCS theory determines the magnitude and anisotropy of the superconducting gap.
This book demonstrates the usefulness of NMR spectroscopy for a wide variety of applications in environmental science and technology. The book contains a wealth of information relating to instrumentation, sample preparation, and data interpretation. It is divided into three sections discussing contaminant interaction, solution and condensed phase characterization, and nutrients and natural organic matter characterization. In addition to these in-depth chapters, an introductory overview provides the basic principles of solution and solid-state NMR spectroscopy. Each section also contains a discussion of advances in each area directly attributable to NMR spectroscopy. A final chapter suggests future directions for the deployment of this powerful technology in environmental science.
Nuclear Magnetic Resonance (NMR) is based on the fact that certain nuclei exhibit a magnetic moment, oriented by a magnetic field, and absorb characteristic frequencies in the radiofrequency part of the spectrum. The spectral lines of the nuclei are highly influenced by the chemical environment, i.e. the structure and interaction of the molecules. NMR is now the leading technique and a powerful tool for the investigation of the structure and interaction of molecules. The present Landolt-Bornstein volume III/35 "Nuclear Magnetic Resonance (NMR) Data" is therefore of major interest to all scientists and engineers who intend to use NMR to study the structure and the binding of molecules. Volume III/35 ''NMR-Data'' is divided into several subvolumes and parts. Subvolume III/35A contains the nuclei B-11 and P-31, subvolume III/35B contains the nuclei F-19 and N-15, subvolume III/35C contains the nucleus H-1, subvolume III/35D contains the nucleus C-13, subvolume III/35E contains the nucleus O-17, subvolume III/35F contains the nucleus Si-29, and subvolume III/35G contains the nucleus Se-77. More nuclei will be presented later.
This book provides a comprehensive summary of research to date in the field of stable iron isotope geochemistry. Since research began in this field 20 years ago, the field has grown to become one of the major research fields in "non-traditional" stable isotope geochemistry. This book reviews all aspects of the field, from low-temperature to high-temperature processes, biological processes, and cosmochemical processes. It provides a detailed history and state-of-the art summary about analytical methods to determine Fe-isotope ratios and discusses analytical and sample prospects.
This book discusses group theory investigations of zincblende and wurtzite semiconductors under symmetry-breaking conditions. The text presents the group theory elements required to develop a multitude of symmetry-breaking problems, giving scientists a fast track to bypass the need for recalculating electronic states. The text is not only a valuable resource for speeding up calculations but also illustrates the construction of effective Hamiltonians for a chosen set of electronic states in crystalline semiconductors. Since Hamiltonians have to be invariant under the transformations of the point group, the crystal symmetry determines the multiplet structure of these states in the presence of spin-orbit, crystal-field, or exchange interactions. Symmetry-breaking leads to additional coupling of the states, resulting in shifts and/or splittings of the multiplets. Such interactions may be intrinsic, as in the case of the quasi-particle dispersion, or extrinsic, induced by magnetic, electric, or strain fields. Using a power expansion of the perturbations these interaction terms can be determined in their parameterized form in a unique way. The hierarchic structure of this invariant development allows to estimate the importance of particular symmetry-breaking effects in the Hamiltonian. A number of selected experimental curves are included to illustrate the symmetry-based discussions, which are especially important in optical spectroscopy. This text is written for graduate students and researchers who want to understand and simulate experimental findings reflecting the fine structure of electronic or excitonic states in crystalline semiconductors.
This first book on load-pull systems is intended for readers with a broad knowledge of high frequency transistor device characterization, nonlinear and linear microwave measurements, RF power amplifiers and transmitters. Load-Pull Techniques with Applications to Power Amplifier Design fulfills the demands of users, designers, and researchers both from industry and academia who have felt the need of a book on this topic. It presents a comprehensive reference spanning different load-pull measurement systems, waveform measurement and engineering systems, and associated calibration procedures for accurate large signal characterization. Besides, this book also provides in-depth practical considerations required in the realization and usage of load-pull and waveform engineering systems. In addition, it also provides procedure to design application specific load-pull setup and includes several case studies where the user can customize architecture of load-pull setups to meet any specific measurement requirements. Furthermore, the materials covered in this book can be part of a full semester graduate course on microwave device characterization and power amplifier design.
As a spectroscopic method, Nuclear Magnetic Resonance (NMR) has seen spectacular growth over the past two decades, both as a technique and in its applications. Today the applications of NMR span a wide range of scientific disciplines, from physics to biology to medicine. Each volume of Nuclear Magnetic Resonance comprises a combination of annual and biennial reports which together provide comprehensive of the literature on this topic. This Specialist Periodical Report reflects the growing volume of published work involving NMR techniques and applications, in particular NMR of natural macromolecules which is covered in two reports: "NMR of Proteins and Acids" and "NMR of Carbohydrates, Lipids and Membranes." For those wanting to become rapidly acquainted with specific areas of NMR, this title provides unrivalled scope of coverage. Seasoned practitioners of NMR will find this an in valuable source of current methods and applications. Specialist Periodical Reports provide systematic and detailed review coverage in major areas of chemical research. Compiled by teams of leading authorities in the relevant subject areas, the series creates a unique service for the active research chemist, with regular, in-depth accounts of progress in particular fields of chemistry. Subject coverage within different volumes of a given title is similar and publication is on an annual or biennial basis.
This thesis describes a new approach for cell analysis by the rapid developing microfluidic technology. The nominee has made great contributions to develop a new analysis platform which combined microfluidic devices with mass spectrometry to determine the trace compounds secreted by cells. Based on this analysis platform, she studied the specific cell secreting behaviors under controlled microenvironment, of which the secretion compounds were qualified and semi-quantified by mass spectrometry. A novel cell sorting device integrated homogenous porous PDMS membrane was invented to classify cells from real samples based on the size difference. The nominee further studied the signal transmission between different cells, and the signal chemicals were qualitative and quantitative monitored by the analysis platform. This indicates the potential significant application of the new cell analysis platform in medicine screening and early diagnosis.
This book is devoted to the synthetic and physical chemistry of aromatic thiols and their closest derivatives, sulfides, sulfoxides, sulfones, including those substituted by various functional groups such as acyl and thioacyl, alkoxide, ester, hydroxyl and halogens. In some cases, for comparison, selenium and oxygen analogues are also detailed. The main focus of the book is on synthetic methods, both traditional and new, based on the use of transition metals as catalysts, as well as the reactivity of the compounds obtained. Its addition to the influence of conformational and electronic factors on spectral (NMR, IR, UV, NQR) and electrochemical characteristics of the compounds is presented. Finally, the book describes the application of aromatic thiols and their derivatives as drug precursors, high-tech materials, building blocks for organic synthesis, analytical reagents and additives for oils and fuels. It is a useful handbook for all those interested in organosulfur chemistry.
Many fundamental aspects of the methods used in mass spectrometry are presented here, with reference to recent developments. The principles and applications of electrospray, ion spray and MALDI ionization technique are included, together with optimised GC/MS interfacing systems and tools for quantitative analysis. There is also a comprehensive treatment of modern instrumentation for mass analysis and detection. The major part of the book deals with bioanalytical applications to peptides, proteins, oligonucleotides, polysaccharides, lipids and plant metabolites. Several contributions are devoted to the evaluation of adduct formation between DNA and carcinogens. Environmental applications are also included, with examples of some specific cases. Fundamentals and applications are treated with the same degree of depth, and the first two parts of the book therefore provide a basis for the understanding of the biomolecular-applications section. The book is intended for advanced graduate students of chemistry who have learned some basic mass spectrometry, and is also suitable for PhD students in chemistry, biology and medicine, as well as researchers in academic and industrial laboratories.
Topological insulators are insulating in the bulk, but process
metallic states present around its boundary owing to the
topological origin of the band structure. The metallic edge or
surface states are immune to weak disorder or impurities, and
robust against the deformation of the system geometry. This book,
the first of its kind on topological insulators, presents a unified
description of topological insulators from one to three dimensions
based on the modified Dirac equation. A series of solutions of the
bound states near the boundary are derived, and the existing
conditions of these solutions are described. Topological invariants
and their applications to a variety of systems from one-dimensional
polyacetalene, to two-dimensional quantum spin Hall effect and
p-wave superconductors, and three-dimensional topological
insulators and superconductors or superfluids are introduced,
helping readers to better understand this fascinating new
field.
This book is the first comprehensive work to be published on far-ultraviolet (FUV) and deep-ultraviolet (DUV) spectroscopy, subjects of keen interest because new areas of spectroscopy have been born in the FUV and DUV regions. For example, FUV spectroscopy in condensed matter has become possible due to the development of attenuated total reflection/FUV spectroscopy. As other examples, DUV surface-enhanced Raman scattering and DUV tip-enhanced Raman scattering have received great attention. Imaging by DUV spectroscopy has also become an area of interest. More recently, FUV and DUV spectroscopy have shown potential for applications in several fields including industry. All these topics are described in this book. Doctoral students and researchers in universities and national research institutes as well as researchers in various industries will find this volume highly useful.
This book compares and offers a comprehensive overview of nine analytical techniques important in material science and many other branches of science. All these methods are already well adapted to applications in diverse fields such as medical, environmental studies, archaeology, and materials science. This clearly presented reference describes and compares the principles of the methods and the various source and detector types.
Simulation of materials at the atomistic level is an important tool in studying microscopic structures and processes. The atomic interactions necessary for the simulations are correctly described by Quantum Mechanics, but the size of systems and the length of processes that can be modelled are still limited. The framework of Gaussian Approximation Potentials that is developed in this thesis allows us to generate interatomic potentials automatically, based on quantum mechanical data. The resulting potentials offer several orders of magnitude faster computations, while maintaining quantum mechanical accuracy. The method has already been successfully applied for semiconductors and metals.
This thesis provides the first successful study of jump diffusion processes in glasses on the atomic scale, utilizing a novel coherent technique. This new method, called atomic-scale X-ray Photon Correlation Spectroscopy or aXPCS, has only recently been proven to be able to capture diffusion processes with atomic resolution in crystal systems. With this new toolkit for studying atomic diffusion in amorphous systems, new insight into basic processes in a wide range of technically relevant materials, like fast ionic conductors, can be obtained.
The behavior of nanoscale materials can change rapidly with time either because the environment changes rapidly or because the influence of the environment propagates quickly across the intrinsically small dimensions of nanoscale materials. Extremely fast time resolution studies using X-rays, electrons and neutrons are of very high interest to many researchers and is a fast-evolving and interesting field for the study of dynamic processes. Therefore, in situ structural characterization and measurements of structure-property relationships covering several decades of length and time scales (from atoms to millimeters and femtoseconds to hours) with high spatial and temporal resolutions are crucially important to understand the synthesis and behavior of multidimensional materials. The techniques described in this book will permit access to the real-time dynamics of materials, surface processes and chemical and biological reactions at various time scales. This book provides an interdisciplinary reference for research using in situ techniques to capture the real-time structural and property responses of materials to surrounding fields using electron, optical and x-ray microscopies (e.g. scanning, transmission and low-energy electron microscopy and scanning probe microscopy) or in the scattering realm with x-ray, neutron and electron diffraction.
This thesis addresses the development of a new force spectroscopy tool, correlation force spectroscopy (CFS) for the measurement of the properties of very small volumes of material (molecular to m3) at kHz-MHz frequency range. CFS measures the simultaneous thermal fluctuations of two closely-spaced atomic force microscopy (AFM) cantilevers. CFS then calculates the cross-correlation in the thermal fluctuations that gives the mechanical properties of the matter that spans the gap of the two cantilevers. The book also discusses development of CFS, its advantages over AFM, and its application in single molecule force spectroscopy and micro-rheology.
Specialist Periodical Reports provide systematic and detailed review coverage of progress in the major areas of chemical research. Written by experts in their specialist fields the series creates a unique service for the active research chemist, supplying regular critical in-depth accounts of progress in particular areas of chemistry. For over 80 years the Royal Society of Chemistry and its predecessor, the Chemical Society, have been publishing reports charting developments in chemistry, which originally took the form of Annual Reports. However, by 1967 the whole spectrum of chemistry could no longer be contained within one volume and the series Specialist Periodical Reports was born. The Annual Reports themselves still existed but were divided into two, and subsequently three, volumes covering Inorganic, Organic and Physical Chemistry. For more general coverage of the highlights in chemistry they remain a 'must'. Since that time the SPR series has altered according to the fluctuating degree of activity in various fields of chemistry. Some titles have remained unchanged, while others have altered their emphasis along with their titles; some have been combined under a new name whereas others have had to be discontinued. The current list of Specialist Periodical Reports can be seen on the inside flap of this volume.
The work presented in this thesis established the existence of wobbling at low spin and low deformation in the Z~60, N~76 nuclear region. This opens the region to further searches for wobbling and shows that wobbling is not confined to a particular quasiparticle orbital, spin or deformation. While deformed nuclei usually have axial shape, triaxial shapes have been predicted at low to moderate spins in certain regions of the nuclear chart (e.g. Z~60, N~76 and Z~46, N~66). Observation of one of the fingerprints of triaxiality, chirality and wobbling, guarantees that the nucleus is axially asymmetric. While chirality has been observed in numerous nuclei from many regions of the nuclear chart, wobbling, prior to this work, had only been observed at high spins in super deformed bands in five nuclei confined to the Z~70, N~90 region. Additionally, this dissertation establishes a new interpretation for the wobbling phenomenon. It shows for the first time that the nucleon aligns to the short axis, which explains the decrease in wobbling energies with angular momentum seen on this and all previous wobbling nuclei while still explaining the observed B(E2out)B(E2in) ratios. This is a new phenomenon, which is in contrast to the increase of the wobbling energies predicted by Bohr and Mottelson.
This thesis examines various aspects of excess excitation energy dissipation via dynamic changes in molecular structure, vibrational modes and solvation. The computational work is carefully described and the results are compared to experimental data obtained using femtosecond spectroscopy and x-ray scattering. The level of agreement between theory and experiment is impressive and provides both a convincing validation of the method and significant new insights into the chemical dynamics and molecular determinants of the experimental data. Hence, the method presented in the thesis has the potential to become a very important contribution to the rapidly growing field of femtosecond x-ray science, a trend reflected in the several free-electron x-ray lasers (XFELs) currently being built around the world. Light-induced chemical processes are accompanied by molecular motion of electrons and nuclei on the femtosecond time scale. Uncovering these dynamics is central to our understanding of the chemical reaction on a fundamental level. Asmus O. Dohn has implemented a highly efficient QM/MM Direct Dynamics method for predicting the solvation dynamics of transition metal complexes in solution. |
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