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John Hollerton joined the GSK spectroscopy department in 1980. Having spent time working with other spectroscopic techniques, he has been focused on NMR spectroscopy since 1982. He is now the manager with a staff of thirteen scientists working under his direction. John has also lectured internationally on the subject on many occasions.
Introduction | |
-Getting Started | |
The Technique | |
Instrumentation | |
CW Systems | |
FT Systems | |
Origin of the Chemical Shift | |
Origin of "Splitting" | |
Integration | |
-Preparing the Sample | |
How much sample do I need? | |
Solvent Selection | |
Deutero Chloroform (CDCl3) | |
Deutero Dimethyl Sulfoxide (DMSO) | |
Deutero Methanol (CD3OD) | |
Deutero water (D2O) | |
Deutero Benzene (C6D6) | |
Carbon Tetrachloride (CCl4) | |
Trifluoroacetic acid (CF3COOH) | |
Using Mixed Solvents | |
Spectrum Referencing | |
Sample Preparation | |
Filtration | |
-Spectrum Acquisition | |
Number of Transients | |
Number of Points | |
Spectral Width | |
Acquisition Time | |
Pulse Width | |
Relaxation Delay | |
Number of Increments | |
Shimming | |
Tuning and Matching | |
Frequency Lock | |
Run unlocked | |
Internal lock | |
External lock | |
To Spin or Not to Spin | |
-Processing | |
Introduction | |
Zero-Filling and Linear Prediction | |
Apodization | |
Fourier Transformation | |
Phase Correction | |
Baseline Correction | |
Integration | |
Referencing | |
Peak Picking | |
-Interpreting Your Spectrum | |
Common Solvents and Impurities | |
Group 1 - Exchangeables and Aldehydes | |
Group 2 - Aromatic and Heterocyclic Protons | |
Monosubstituted Benzene Rings | |
Multisubstituted Benzene Rings | |
Heterocyclic Ring Systems (Unsaturated) and polycyclic aromatic systems | |
Group 3 - Double and Triple Bonds | |
Group 4 - Alkyl Protons | |
-Delving Deeper | |
Chiral centres | |
Enantiotopic and Diastereotopic Protons | |
Molecular Anisotropy | |
Accidental Equivalence | |
Restricted Rotation | |
Heteronuclear Coupling | |
Coupling between protons and 13C | |
Coupling between protons and 19F | |
Coupling between protons and 31P | |
Coupling between 1H and other heteroatoms | |
Cyclic Compounds and the Karplus Curve | |
Salts, Free Bases and Zwitterions | |
-Further Elucidation Techniques - Part 1 | |
Chemical Techniques | |
Deuteration | |
Basification and Acidification | |
Changing Solvents | |
Trifluoroacetylation | |
Lanthanide Shift Reagents | |
Chiral Resolving Agents | |
-Further Elucidation Techniques - Part 2 | |
Instrumental Techniques | |
Spin-Decoupling (homonuclear, 1-D) | |
COSY (Correlated Spectroscopy) | |
TOCSY (Total Correlation Spectroscopy) 1&2-D | |
The Nuclear Overhauser Effect (NOE) and Associated Techniques | |
-Carbon-13 NMR Spectroscopy | |
General Principles and 1-D 13C | |
2-D Proton-Carbon (Single Bond) Correlated Spectroscopy | |
2-D Proton-Carbon (Multiple Bond) Correlated Spectroscopy | |
Piecing It All Together | |
Choosing the Right Tool | |
-Some of the Other Tools | |
HPLC-NMR | |
Flow NMR | |
Solvent Suppression | |
MAS (Magic Angle Spinning) NMR | |
Other 2-D Techniques | |
INADEQUATE | |
J-Resolved | |
DOSY | |
3-D Techniques | |
-Some of the Other Nuclei | |
-Quantification | |
Introduction | |
Relative Quantification | |
Absolute Quantification | |
Internal Standards | |
External Standards | |
Electronic Reference (ERETIC) | |
QUANTAS | |
Things to Watch Out For | |
Conclusion | |
-Safety | |
Magnetic Fields | |
Cryogens | |
Sample-Related Injuries | |
-Software | |
Acquisition Software | |
Processing Software | |
Prediction and Simulation Software | |
13C Prediction | |
1H Prediction | |
Incremental Approaches | |
HOSE Code Databases | |
Semi-empirical approaches | |
Ab initio approaches | |
Simulation | |
Structural Verification Software | |
Structural Elucidation Software | |
-Problems | |
Hints | |
Answers | |
Glossary | |
Index | |
Table of Contents provided by Publisher. All Rights Reserved. |
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