9780080427980

High-Resolution NMR Techniques in Organic Chemistry

by
  • ISBN13:

    9780080427980

  • ISBN10:

    0080427987

  • Format: Hardcover
  • Copyright: 1999-12-24
  • Publisher: Pergamon Pr
  • Purchase Benefits
  • Free Shipping Icon Free Shipping On Orders Over $35!
    Your order must be $35 or more to qualify for free economy shipping. Bulk sales, PO's, Marketplace items, eBooks and apparel do not qualify for this offer.
  • eCampus.com Logo Get Rewarded for Ordering Your Textbooks! Enroll Now
List Price: $58.95

Summary

Emphasis is on the more recently developed methods of solution-state NMR applicable to chemical research, which are chosen for their wide applicability and robustness. Softcover.

Table of Contents

Foreword v
Preface vii
Acknowledgements ix
Introduction
The development of high-resolution NMR
1(3)
Modern high-resolution NMR and this book
4(4)
What this book contains
5(2)
Pulse sequence nomenclature
7(1)
Applying modern NMR techniques
8(5)
References
12(1)
Introducing high-resolution NMR
Nuclear spin and resonance
13(3)
The vector model of NMR
16(8)
The rotating frame of reference
16(2)
Pulses
18(2)
Chemical shifts and couplings
20(1)
Spin-echoes
21(3)
Time and frequency domains
24(1)
Spin relaxation
25(10)
Longitudinal relaxation: establishing equilibrium
26(1)
Measuring T1 with the inversion-recovery sequence
27(3)
Transverse relaxation: loss of magnetisation in the x--y plane
30(1)
Measuring T2 with a spin-echo sequence
31(4)
Mechanisms for relaxation
35(10)
The path to relaxation
35(2)
Dipole--dipole relaxation
37(1)
Chemical shift anisotropy relaxation
38(1)
Spin-rotation relaxation
39(1)
Quadrupolar relaxation
40(3)
References
43(2)
Practical aspects of high-resolution NMR
An overview of the NMR spectrometer
45(3)
Data acquisition and processing
48(27)
Pulse excitation
48(3)
Signal detection
51(1)
Sampling the FID
52(7)
Quadrature detection
59(4)
Phase cycling
63(2)
Dynamic range and signal averaging
65(5)
Window functions
70(3)
Phase correction
73(2)
Preparing the sample
75(6)
Selecting the solvent
75(2)
Reference compounds
77(1)
Tubes and sample volumes
78(2)
Filtering and degassing
80(1)
Preparing the spectrometer
81(13)
The probe
82(1)
Tuning the probe
83(2)
The field-frequency lock
85(2)
Optimising the field homogeneity: shimming
87(7)
Spectrometer calibrations
94(11)
Radiofrequency pulses
94(5)
Pulsed field gradients
99(5)
Sample temperature
104(1)
Spectrometer performance tests
105(6)
Lineshape and resolution
106(1)
Sensitivity
107(2)
Solvent presaturation
109(1)
References
110(1)
One-dimensional techniques
The single-pulse experiment
111(5)
Optimising sensitivity
112(2)
Quantitative measurements and integration
114(2)
Spin decoupling methods
116(9)
The basis of spin decoupling
117(1)
Homonuclear decoupling
117(3)
Heteronuclear decoupling
120(5)
Spectrum editing with spin-echoes
125(4)
The J-modulated spin-echo
125(3)
APT
128(1)
Sensitivity enhancement and spectrum editing
129(14)
Polarisation transfer
130(2)
INEPT
132(7)
DEPT
139(3)
PENDANT
142(1)
Observing quadrupolar nuclei
143(5)
References
145(3)
Correlations through the chemical bond I: Homonuclear shift correlation
Introducing two-dimensional methods
148(5)
Generating a second dimension
149(4)
Correlation spectroscopy (COSY)
153(7)
Correlating coupled spins
155(1)
Interpreting COSY
156(3)
Peak fine structure
159(1)
Practical aspects of 2D NMR
160(14)
2D lineshapes and quadrature detection
161(6)
Axial peaks
167(1)
Instrumental artefacts
168(2)
2D data acquisition
170(2)
2D data processing
172(2)
Coherence and coherence transfer
174(4)
Coherence-transfer pathways
177(1)
Gradient-selected spectroscopy
178(9)
Signal selection with pulsed field gradients
179(4)
Phase-sensitive experiments
183(1)
PFGs in high-resolution NMR
184(2)
Practical implementation of PFGs
186(1)
Alternative COSY sequences
187(14)
Which COSY approach?
188(1)
Double-quantum filtered COSY (DQF-COSY)
189(8)
COSY-β
197(2)
Delayed-COSY: detecting small couplings
199(1)
Relayed-COSY
200(1)
Total correlation spectroscopy (TOCSY)
201(10)
The TOCSY sequence
202(3)
Using TOCSY
205(3)
Implementing TOCSY
208(3)
Correlating dilute spins: INADEQUATE
211(10)
2D INADEQUATE
212(1)
1D INADEQUATE
213(2)
Implementing INADEQUATE
215(1)
Variations on INADEQUATE
216(2)
References
218(3)
Correlations through the chemical bond II: Heteronuclear shift correlation
Introduction
221(1)
Sensitivity
222(2)
Heteronuclear single-bond correlation spectroscopy
224(20)
Heteronuclear multiple-quantum correlation (HMQC)
224(5)
Heteronuclear single-quantum correlation (HSQC)
229(1)
Practical implementations
230(8)
Hybrid experiments
238(6)
Heteronuclear multiple-bond correlation spectroscopy
244(7)
The HMBC sequence
245(3)
Applying HMBC
248(3)
Traditional X-detected correlation spectroscopy
251(8)
Single-bond correlations
252(2)
Multiple-bond correlations and small couplings
254(2)
References
256(3)
Separating shifts and couplings: J-resolved spectroscopy
Introduction
259(1)
Heteronuclear J-resolved spectroscopy
260(7)
Measuring long-range proton-carbon coupling constants
263(3)
Practical considerations
266(1)
Homonuclear J-resolved spectroscopy
267(6)
Tilting, projections and symmetrisation
268(2)
Applications
270(3)
Practical considerations
273(1)
`Indirect' homonuclear J-resolved spectroscopy
273(4)
References
274(3)
Correlations through space: The nuclear Overhauser effect
Introduction
277(2)
Definition of the NOE
279(1)
Steady-state NOEs
279(22)
NOEs in a two-spin system
279(9)
NOEs in a multispin system
288(6)
Summary
294(2)
Applications
296(5)
Transient NOEs
301(3)
NOE kinetics
302(1)
Measuring internuclear separations
303(1)
Rotating-frame NOEs
304(2)
Measuring steady-state NOEs: NOE difference
306(7)
Optimising difference experiments
307(6)
Measuring transient NOEs: Noesy
313(15)
The 2D NOESY sequence
314(6)
1D NOESY sequences
320(3)
Applications
323(3)
Measuring chemical exchange: Exsy
326(2)
Measuring rotating-frame NOEs: Roesy
328(7)
The 2D ROESY sequence
329(3)
1D ROESY sequences
332(1)
Applications
332(3)
Measuring heteronuclear NOEs
335(1)
Experimental considerations
336(5)
References
337(4)
Experimental methods
Composite pulses
341(5)
A myriad of pulses
344(1)
Inversion vs. refocusing
344(2)
Broadband decoupling and spin-locks
346(2)
Spin-locks
347(1)
Adiabatic pulses
348(1)
Selective excitation and shaped pulses
348(11)
Shaped soft pulses
350(4)
DANTE sequences
354(1)
Excitation sculpting
355(2)
Practical considerations
357(2)
Solvent suppression
359(7)
Presaturation
361(1)
Zero excitation
362(1)
Pulsed field gradients
363(3)
Recent methods
366(7)
Heterogeneous samples and MAS
366(2)
Diffusion-ordered spectroscopy
368(3)
References
371(2)
Appendix. Glossary of acronyms 373(2)
Index 375

Rewards Program

Reviews for High-Resolution NMR Techniques in Organic Chemistry (9780080427980)