NMR-Spectroscopy - Data Acquisition

by ;
Edition: 1st
Format: Hardcover
Pub. Date: 2004-09-03
Publisher(s): Wiley-VCH
List Price: $315.00

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Summary

The key to correct structure analysis now in its second edition. There have been many important advances in the field since the first publication of this book. Consequently, this edition has been extended to incorporate a number of pulse sequence developments. Nevertheless, it still details the basic experiments on a step-by-step basis, such that students and newcomers may come to understand basic data acquisition procedures, modular pulse sequence units, and complete sequences in NMR spectroscopy. The author applies the numerous possibilities of Bruker's simulation program NMR-SIM to provide a guided introduction to the world of pulse sequences. The effectiveness of particular NMR experiments is demonstrated by the "Check Its" section and that of data processing by the accompanying CD-ROM containing the Bruker processing software 1D and 2D WIN-NMR. Major revisions include increased coverage of simulations of multiple offset selective pulse experiments as well as filter elements. One new chapter is a collection of some of the latest published ideas to improve existing sequences, together with spin-state selective experiments. The result is a volume encouraging beginners to use high resolution NMR, while prompting experts to evaluate new experiments using the easy-manageable simulation program. From the first edition: "... not only of interest for the NMR operators but also for interpreters of spectral data?. Many mistakes made with the application of modern NMR spectroscopy because of a lack of understanding of basic principles may be avoided. This volume covers all these aspects and explains them in an interactive way." AFS Advances in Food Science, 2002, Vol. 24

Author Biography

Christian Schorn is Principal Investigator for GlaxoSmithKline Research & Development Limited, Tonbridge, UK. He studied Chemistry at the UniversitSt zu K÷ln, Germany, and made his diploma thesis in Chemical Engineering in the central research department of the Bayer AG, Leverkusen. His PhD thesis at the UniversitSt zu K÷ln included preparative work and structural investigation using 19F NMR spectroscopy. For a post-doctoral stay he went to the UniversitSt Bern, Switzerland, where he worked on pulse program development and structural characterization in the NMR service lab of Peter Bigler. During his stay he started the first edition of the present compendium. The work was finished during his post-doctoral fellowship at the ETH Znrich, Switzerland, where he worked with Nobel Prize winner Kurt Wnthrich on mammalian prion protein structures. <br> <br> Brian Taylor is at the University of Sheffield where he holds the position of NMR Service manager. He was born in London and obtained both his degrees at the University of Bristol, his doctorate under the supervision of Robin Goodfellow. He was a post-doctoral fellow at University of Bristol, where he worked with Gordon Stone. He moved to the University of Sheffield in 1974 to take charge of the Department of Chemistry's first FT NMR spectrometer. He is interested in the application of NMR spectroscopy in undergraduate teaching and has been instrumental in pioneering the use of NMR automation in British Universities.

Table of Contents

Preface to 2nd Edition ix
Acknowledgements xi
Introduction
1(18)
Scope and Audience
1(3)
Simulation Environment
2(1)
Book Content
3(1)
Software
4(7)
Installation
4(3)
The User Interfaces of NMR-SIM, ID and 2D WIN-NMR
7(2)
Data Organization
9(2)
The Check Its
11(5)
Book Layout
16(1)
References
17(2)
Background on Simulation
19(44)
Description of Real Samples - Spin systems and Processes on Spin Systems
20(2)
Spin System Parameters
20(1)
Coherence Transfer Processes
21(1)
Description of Pulse Sequences
22(10)
Density Matrix Formalism
22(2)
Product Operator Formalism
24(4)
Coherence Level Scheme
28(3)
Energy Level Scheme
31(1)
Signal Detection
32(28)
Quadrature Detection
32(9)
Decoupling Methods
41(2)
Coherence Selection - Phase Cycling and Gradients
43(17)
References
60(3)
Acquisition and Processing
63(48)
Excitation of Nuclear Spins and Their Response Detection
63(1)
One Dimensional Experiments
64(26)
Recording a Free Induction Decay
65(3)
Simulation of a Free Induction Decay
68(2)
Processing and Analysis of ID NMR Data
70(2)
Time Domain Processing of raw NMR Data
72(5)
Fourier Transformation
77(2)
Frequency Domain Processing of NMR Data
79(5)
Analysis, Display and Output Tools in ID WIN-NMR
84(6)
Two Dimensional Experiments
90(19)
Recording and Simulation of 2D Experiments
91(6)
Processing of 2D NMR Data
97(12)
NMR-SIM Options
109(1)
References
110(1)
Experiment Setup in NMR-SIM
111(66)
Spin Systems and Pulse Programs
112(33)
Editing a Spin System
113(1)
Defining a Spin System
114(3)
Spin Systems with Variable Arguments
117(2)
Editing a Partial Spin System - The Molecule Bromomethylcrotonate
119(4)
Pulse Programming
123(1)
Modifying an Existing Pulse Program or Creating a New One
124(1)
The Syntax for Using Pulses, Delays, Gradients and Decoupling
125(5)
Acquisition Loops and Data Storage
130(1)
Non-Standard Bruker Pulse Program Commands
131(2)
Editing Pulse Programs - From One Pulse to the DEPT Experiment
133(8)
Gradients and the Second Dimension - The gs-13C, 1H HMQC Experiment
141(4)
Experiment and Processing Parameters
145(17)
Editing Experiment Parameters
145(1)
Manual Parameter Selection
145(6)
Using Configuration Files
151(2)
Using Job Files
153(1)
NMR-Wizard for Homonuclear Experiments
154(3)
Parameter Optimization
157(3)
Editing Processing Parameters
160(2)
Using the Bloch Simulator
162(13)
A Classical and Pictorial Approach
162(3)
General Experiment Setup
165(4)
Analysing Shaped Pulses
169(3)
Analysing Pulse Sequence Fragments
172(3)
References
175(2)
Complete Sequences, Elements and Building Blocks
177(188)
The Philosophy of Pulse Sequences
178(5)
Pulse Sequences as Combination of Building Blocks
178(2)
Two Different Approaches to Pulse Sequence Classification
180(2)
Pulse Sequence Nomenclature
182(1)
Single Pulse and Simple Multi-Pulse Experiments
183(80)
One-pulse 1H and nX Experiments
184(13)
Single Line or Multiplet Excitation Experiment
197(6)
Single Line or Multiplet Suppression Experiment
203(11)
Single Line Perturbation Experiment
214(7)
2D Shift and Coupling Resolved Experiments (JRES, SERF, SELRESOLV)
221(13)
Multiplicity Edited Experiments (APT, SEMUT, DEPT, POMMIE, INEPT and PENDANT)
234(26)
Relaxation Time Measurement Experiments
260(3)
Building Blocks and Elements - Part One
263(21)
Pulse Types and Pulse Properties
263(15)
Composite Pulses
278(3)
Dante Pulses - A Different Way for Selective Excitation
281(2)
Spin Echo - The First Step to Sequences
283(1)
Homonuclear Correlation Experiments
284(28)
Homonuclear COSY Experiments
285(1)
2D COSY Experiments
285(8)
Selective 1D COSY Experiments
293(5)
Relayed COSY Experiments
298(5)
TOCSY Experiments
303(5)
Inadequate Experiment
308(4)
Building Blocks and Elements - Part Two
312(9)
Coherence Transfer Problems
313(2)
Delay Incrementation - Constant Time and Accord-Principle
315(6)
Heteronuclear Correlation Experiments I nX Detected Experiments
321(7)
1H, nX HETCOR Experiment
321(4)
1H, nX COLOC Experiment
325(3)
Heteronuclear Correlation Experiments II 1H Detected Experiments
328(11)
nX, 1H HMQC Experiment
329(4)
nX, 1H HSQC Experiment
333(3)
nX, 1H HMBC Experiment
336(3)
Building Blocks and Elements - Part Three
339(10)
Bird, Tango and Bango as Members of the Same Family
339(5)
Filter Elements: z-Filter, Multi-Quantum Filter and Low-Pass Filter
344(2)
Chemical Shift Filter
346(3)
Latest Developments in NMR
349(8)
Olympic Spirit in NMR Spectroscopy
349(3)
Spin-State Selective Experiments
352(5)
References
357(8)
Glossary 365(1)
Index 366

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