NMR - from spectra to structures: an experimental approach
"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 assignments. The book is intended as a practical guide for students and laboratory personnel, so that t...
Gespeichert in:
| Hauptverfasser: | , |
|---|---|
| Format: | Buch |
| Sprache: | English |
| Veröffentlicht: |
Berlin [u.a.]
Springer
2007
|
| Ausgabe: | 2., rev. and exp. ed. |
| Schlagworte: | |
| Online-Zugang: | Inhaltsverzeichnis |
| Zusammenfassung: | "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 assignments. 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 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."--BOOK JACKET. |
| Beschreibung: | XIII, 207 S. graph. Darst. |
| ISBN: | 9783540721956 9783540406952 |
Internformat
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Datensatz im Suchindex
| _version_ | 1804137194878664704 |
|---|---|
| adam_text | Table of Contents
Introduction 1
Part 1: NMR Experiments 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 (CH2 Signal of 1) 11
1.1.4 The Proton Spectrum of 1 in D2O or H2O/D2O Mixtures 14
1.1.5 Integration: Relaxation, T,, 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 ID NOE Experiment (1D NOESY) and Selective ID
TOCSY Experiment 22
1.2 I3C 25
1.2.1 Natural Abundance BC Spectrum of Compound 1 25
1.2.2 Coupled Spectrum (Gated Decoupling) 28
1.2.3 Quantitative I3C 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 The INADEQUATE Experiment 34
1.3 P 37
1.3.1 Natural Abundance P 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 47
2.7 P,C Correlation 48
2.8 P,P Correlation 50
3 Quadrupolar Nucleus Experiments 51
3.1 General Principles: Quadrupole Moment, Relaxation, Linewidth .. 51
3 2 17O 51
3.2.1 17O Spectrum of 7: Chemical Shift (Reference), Coupling with P ... 52
3.2.2 P O Correlation 52
4 HPLC NMR Coupling 53
4.1 General Principles, NMR as a Highly Sensitive Analytical Tool
(ug to ng Amounts) 53
4.2 Example: Separation of 4 and 5, Two Acetals
of Formylphosphonic Ester 54
4.3 Chromatogram 54
4.4 On Flow Diagram (Chemical Shift vs. Time) 55
4.5 Stopped Flow Experiments 58
5 Other Spin Vi Nuclei .... 59
5 1 15N . 60
5.2 i9f 62
5.3 29Si .62
5.4 77Se 66
5.5 113Cd 67
5.6 117Sn,119Sn 67
5.7 195Pt ;; 69
5.8 207Pb 72
6 Solid State NMR 73
6.1 General Principles 73
6.2 Solid State lH 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
|
| adam_txt |
Table of Contents
Introduction 1
Part 1: NMR Experiments 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 (CH2 Signal of 1) 11
1.1.4 The Proton Spectrum of 1 in D2O or H2O/D2O Mixtures 14
1.1.5 Integration: Relaxation, T,, 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 ID NOE Experiment (1D NOESY) and Selective ID
TOCSY Experiment 22
1.2 I3C 25
1.2.1 Natural Abundance BC Spectrum of Compound 1 25
1.2.2 Coupled Spectrum (Gated Decoupling) 28
1.2.3 Quantitative I3C 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 The INADEQUATE Experiment 34
1.3 "P 37
1.3.1 Natural Abundance "P 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 47
2.7 P,C Correlation 48
2.8 P,P Correlation 50
3 Quadrupolar Nucleus Experiments 51
3.1 General Principles: Quadrupole Moment, Relaxation, Linewidth . 51
3 2 17O 51
3.2.1 17O Spectrum of 7: Chemical Shift (Reference), Coupling with P . 52
3.2.2 P O Correlation 52
4 HPLC NMR Coupling 53
4.1 General Principles, NMR as a Highly Sensitive Analytical Tool
(ug to ng Amounts) 53
4.2 Example: Separation of 4 and 5, Two Acetals
of Formylphosphonic Ester 54
4.3 Chromatogram 54
4.4 On Flow Diagram (Chemical Shift vs. Time) 55
4.5 Stopped Flow Experiments 58
5 Other Spin Vi Nuclei . 59
5 1 15N . 60
5.2 i9f 62
5.3 29Si .62
5.4 77Se 66
5.5 113Cd 67
5.6 117Sn,119Sn '" ' 67
5.7 195Pt ;; 69
5.8 207Pb 72
6 Solid State NMR 73
6.1 General Principles 73
6.2 Solid State lH 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 |
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| ctrlnum | (OCoLC)153582148 (DE-599)BVBBV022951297 |
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| dewey-hundreds | 500 - Natural sciences and mathematics |
| dewey-ones | 543 - Analytical chemistry |
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| dewey-sort | 3543 266 |
| dewey-tens | 540 - Chemistry and allied sciences |
| discipline | Chemie / Pharmazie Physik Chemie |
| discipline_str_mv | Chemie / Pharmazie Physik Chemie |
| edition | 2., rev. and exp. ed. |
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| id | DE-604.BV022951297 |
| illustrated | Illustrated |
| index_date | 2024-07-02T19:02:25Z |
| indexdate | 2024-07-09T21:08:25Z |
| institution | BVB |
| isbn | 9783540721956 9783540406952 |
| language | English |
| oai_aleph_id | oai:aleph.bib-bvb.de:BVB01-016155761 |
| oclc_num | 153582148 |
| open_access_boolean | |
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| owner_facet | DE-19 DE-BY-UBM DE-91G DE-BY-TUM DE-634 DE-11 DE-384 |
| physical | XIII, 207 S. graph. Darst. |
| publishDate | 2007 |
| publishDateSearch | 2007 |
| publishDateSort | 2007 |
| publisher | Springer |
| record_format | marc |
| spelling | Mitchell, Terence Nigel Verfasser aut NMR - from spectra to structures an experimental approach Terence N. Mitchell ; Burkhard Costisella 2., rev. and exp. ed. Berlin [u.a.] Springer 2007 XIII, 207 S. graph. Darst. txt rdacontent n rdamedia nc rdacarrier "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 assignments. 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 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."--BOOK JACKET. Espectroscopia de ressonância magnética nuclear larpcal Spectroscopie de la résonance magnétique nucléaire Nuclear magnetic resonance spectroscopy Chemische Struktur (DE-588)4009857-6 gnd rswk-swf NMR-Spektroskopie (DE-588)4075421-2 gnd rswk-swf Organische Verbindungen (DE-588)4043816-8 gnd rswk-swf Chemische Analyse (DE-588)4009840-0 gnd rswk-swf NMR-Spektrum (DE-588)4171956-6 gnd rswk-swf Strukturaufklärung (DE-588)4183788-5 gnd rswk-swf Organische Verbindungen (DE-588)4043816-8 s Chemische Analyse (DE-588)4009840-0 s Chemische Struktur (DE-588)4009857-6 s NMR-Spektroskopie (DE-588)4075421-2 s DE-604 Strukturaufklärung (DE-588)4183788-5 s 1\p DE-604 NMR-Spektrum (DE-588)4171956-6 s 2\p DE-604 Costisella, Burkhard Verfasser aut HBZ Datenaustausch application/pdf http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=016155761&sequence=000002&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA Inhaltsverzeichnis 1\p cgwrk 20201028 DE-101 https://d-nb.info/provenance/plan#cgwrk 2\p cgwrk 20201028 DE-101 https://d-nb.info/provenance/plan#cgwrk |
| spellingShingle | Mitchell, Terence Nigel Costisella, Burkhard NMR - from spectra to structures an experimental approach Espectroscopia de ressonância magnética nuclear larpcal Spectroscopie de la résonance magnétique nucléaire Nuclear magnetic resonance spectroscopy Chemische Struktur (DE-588)4009857-6 gnd NMR-Spektroskopie (DE-588)4075421-2 gnd Organische Verbindungen (DE-588)4043816-8 gnd Chemische Analyse (DE-588)4009840-0 gnd NMR-Spektrum (DE-588)4171956-6 gnd Strukturaufklärung (DE-588)4183788-5 gnd |
| subject_GND | (DE-588)4009857-6 (DE-588)4075421-2 (DE-588)4043816-8 (DE-588)4009840-0 (DE-588)4171956-6 (DE-588)4183788-5 |
| title | NMR - from spectra to structures an experimental approach |
| title_auth | NMR - from spectra to structures an experimental approach |
| title_exact_search | NMR - from spectra to structures an experimental approach |
| title_exact_search_txtP | NMR - from spectra to structures an experimental approach |
| title_full | NMR - from spectra to structures an experimental approach Terence N. Mitchell ; Burkhard Costisella |
| title_fullStr | NMR - from spectra to structures an experimental approach Terence N. Mitchell ; Burkhard Costisella |
| title_full_unstemmed | NMR - from spectra to structures an experimental approach Terence N. Mitchell ; Burkhard Costisella |
| title_short | NMR - from spectra to structures |
| title_sort | nmr from spectra to structures an experimental approach |
| title_sub | an experimental approach |
| topic | Espectroscopia de ressonância magnética nuclear larpcal Spectroscopie de la résonance magnétique nucléaire Nuclear magnetic resonance spectroscopy Chemische Struktur (DE-588)4009857-6 gnd NMR-Spektroskopie (DE-588)4075421-2 gnd Organische Verbindungen (DE-588)4043816-8 gnd Chemische Analyse (DE-588)4009840-0 gnd NMR-Spektrum (DE-588)4171956-6 gnd Strukturaufklärung (DE-588)4183788-5 gnd |
| topic_facet | Espectroscopia de ressonância magnética nuclear Spectroscopie de la résonance magnétique nucléaire Nuclear magnetic resonance spectroscopy Chemische Struktur NMR-Spektroskopie Organische Verbindungen Chemische Analyse NMR-Spektrum Strukturaufklärung |
| url | http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=016155761&sequence=000002&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA |
| work_keys_str_mv | AT mitchellterencenigel nmrfromspectratostructuresanexperimentalapproach AT costisellaburkhard nmrfromspectratostructuresanexperimentalapproach |