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E-book
Essential Practical NMR for Organic ChemistryISBN: 978-0-470-97722-4
E-book
216 pages
December 2010
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1. Getting Started.
1.1 The Technique.
1.2 Instrumentation.
1.3 CW Systems.
1.4 FT Systems.
2. Preparing the Sample.
2.1 How Much Sample Do I Need?
2.2 Solvent Selection.
2.3 Spectrum Referencing (Proton NMR).
2.4 Sample Preparation.
3. Spectrum Acquisition.
3.1 Number of Transients.
3.2 Number of Points.
3.3 Spectral Width.
3.4 Acquisition Time.
3.5 Pulse Width/Pulse Angle.
3.6 Relaxation Delay.
3.7 Number of Increments.
3.8 Shimming.
3.9 Tuning and Matching.
3.10 Frequency Lock.
3.11 To Spin or Not to Spin?
4. Processing.
4.1 Introduction.
4.2 Zero Filling and Linear Prediction.
4.3 Apodization.
4.4 Fourier Transformation.
4.5 Phase Correction.
4.6 Baseline Correction.
4.7 Integration.
4.8 Referencing.
4.9 Peak Picking.
5. Interpreting Your Spectrum.
5.1 Common Solvents and Impurities.
5.2 Group 1 – Exchangeables and Aldehydes.
5.3 Group 2 – Aromatic and Heterocyclic Protons.
5.4 Group 3 – Double and Triple Bonds.
5.5 Group 4 – Alkyl Protons.
6. Delving Deeper.
6.1 Chiral Centres.
6.2 Enantiotopic and Diastereotopic Protons.
6.3 Molecular Anistropy.
6.4 Accidental Equivalence.
6.5 Restricted Rotation.
6.6 Heteronuclear Coupling.
7. Further Elucidation Techniques – Part 1.
7.1 Chemical Techniques.
7.2 Deuteration.
7.3 Basification and Acidification.
7.4 Changing Solvents.
7.5 Trifluoroacetylation.
7.6 Lanthanide Shift Reagents.
7.7 Chiral Resolving Agents.
8. Further Elucidation Techniques – Part 2.
8.1 Instrumental Techniques.
8.2 Spin Decoupling (Homonuclear, 1-D).
8.3 Correlated Spectroscopy (2-D).
8.4 Total Correlation Spectroscopy (1- and 2-D).
8.5 The Nuclear Overhauser Effect and Associated Techniques.
9. Carbon-13 NMR Spectroscopy.
9.1 General Principles and 1-D 13C.
9.2 2-D Proton-Carbon (Single Bond) Correlated Spectroscopy.
9.3 2-D Proton-Carbon (Multiple Bond) Correlated Spectroscopy.
9.4 Piecing It All Together.
9.5 Choosing the Right Tool.
10. Some of the Other Tools.
10.1 Linking HPLC with NMR.
10.2 Flow NMR.
10.3 Solvent Suppression.
10.4 Magic Angle Spinning NMR.
10.5 Other 2-D Techniques.
10.6 3-D Techniques.
11. Some of the Other Nuclei.
11.1 Fluorine.
11.2 Phosphorus.
11.3 Nitrogen.
12. Quantification.
12.1 Introduction.
12.2 Relative Quantification.
12.3 Absolute Quantification.
12.4 Things to Watch Out For.
12.5 Conclusion.
13. Safety.
13.1 Magnetic Fields.
13.2 Cryogens.
13.3 Sample-Related Injuries.
14. Software.
14.1 Acquisition Software.
14.2 Processing Software.
14.3 Prediction and Simulation Software.
15. Problems.
15.1 Ten NMR Problems.
15.2 Hints.
15.3 Answers.
Glossary.
Index.
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