| Titre : | NMR, from spectra to structures : an experimental approach |
| Auteurs : | Terence N. Mitchell, Auteur ; Burkhard Costisella, Auteur |
| Type de document : | Monographie imprimée |
| Mention d'édition : | 2nd revised expanded edition |
| Editeur : | Berlin [Allemagne] : Springer, cop. 2007 |
| ISBN/ISSN/EAN : | 978-3-540-72195-6 |
| Format : | 1 vol. (XIII-207 p.) / ill., couv. ill. en coul. / 24 cm |
| Langues: | Anglais |
| Index. décimale : | 543.660 76 |
| Résumé : |
s Nuclear magnetic resonance spectroscopy is one of the most powerful analytical methods. This practice-oriented textbook aims at teaching how NMR experiments should be used to make structural asssignments. The book is intended as a practical guide for students and laboratory personnel, so that the emphasis is on practical rather than on theoretical aspects, which are treated only to the extent necessary to understand the basis of the experiments and to interpret the results. The second edition has been expanded to include several other heteronuclei (15N, 19F, 'Si, "Se, "'Cd, "'Snr"Sn,'"Pt, "'Pb) and a new chapter on solid state NMR. The problems section has been enlarged and now includes 50 problems. These are of different degrees of complexity and in all cases include two-dimensional (2D) methods as well as standard proton and carbon 1D spectra. |
| Sommaire : |
Introduction Part 1: NMR Experiments 1 3 1 ID Experiments 3 1.1 'H, D (2H): Natural Abundance, Sensitivity 3 1.1.1 Proton NMR Spectrum of the Model Compound 1 4 1.1.2 Field Dependence of the Spectrum of 1 10 1.1.3 FID Manipulation: FT, EM, SINE BELL (CH, Signal of 1) 11 1.1.4 The Proton Spectrum of 1 in D,0 or H20/D,0 Mixtures 14 1.1.5 Integration: Relaxation, TI, 90°-Pulse, Ernst Angle 16 1.1.6 The NOE: Through-Space Interactions between Protons 20 1.1.6.1 NOE Difference Spectroscopy 21 1.1.6.2 Selective 1D NOE Experiment (1D-NOESY) and Selective 1D TOCSY Experiment 22 1.2 13C 25 1.2.1 Natural Abundance 13 C Spectrum of Compound 1 25 1.2.2 Coupled Spectrum (Gated Decoupling) 28 1.2.3 Quantitative 13C Spectrum (Inverse Gated Decoupling) 29 1.2.4 Decoupled Spectrum: Proton Decoupling, Proton and Phosphorus Decoupling 31 1.2.5 APT, DEPT, INEPT 32 1.2.6 lhe INADÉQUATE Experiment 34 1.3 31P 37 1.3.1 Natural Abundance 31P Spectrum of Compound 6 37 1.3.2 Proton-Decoupled and Proton-Coupled Spectra 37 1.3.3 Coupled Spectrum (P-P Coupling) 38 2 2D Experiments 39 2.1 General Principles, Inverse Techniques, Gradients 39 2.2 H,H COSY 41 2.3 2D NOE 43 2.4 P,H COSY: with Varying Mixing Times for the Coupling 45 2.5 C,H Direct Correlation 46 2.6 C,H Long Range Correlation 2.7 P,C Correlation 2.8 P,P Correlation 3 Quadrupolar Nucleus Experiments 3.1 General Principles. Quadrupole Moment, Relaxation, Linewidth 51 3.2.1 170 Spectrum of 7 Chemical Shift (Reference), Coupling with P 52 3.2.2 P-0 Correlation 52 4 HPLC-NMR Coupling 53 4.1 General Principles, NMR as a Highly Sensitive Analytical Tool to ng Amounts) 53 4.2 Example: Separation of 4 and 5 Two Acetals of Formylphosphonic Ester 54 4.3 Ch rom atogram 54 4.4 On-Flow Diagram (Chemical Shift vs. Time) 55 5.2 19F 62 5.3 29Si 62 5.4 77Se 66 5.5 "3Cd 67 5.6 117n 119Sn S, 67 5.7 195pt 69 72 6 Solid State NMR 73 6.1 General Principles 73 6.2 Solid State 1H NMR 74 6.3 Solid State 13C NMR 75 6.4 Solid-State 31P NMR 77 6.5 Solid-State 29Si NMR 81 6.6 Solid State NMR 81 Appendix: Reference List 84 Part 2: Worked Example and Problems 85 2.1 Section 1 85 Solving the Structures of Organic Molecules 85 Elemental Analysis 86 Mass Spectrometry 86 2.2 Worked Example 88 H,H Correlation 89 C,H Correlation 89 2.3 Problems 93 2.4 Section 2 164 Introduction 164 Problems 166 |
Disponibilité (1)
| Cote | Support | Localisation | Statut |
|---|---|---|---|
| CH/241 | Livre | bibliothèque sciences exactes | Consultable |
