- Shopping Bag ( 0 items )
A discussion is then presented on carbon-13 NMR, detailing its pros and cons and showing how it can be used in conjunction with proton NMR via the pivotal 2-D techniques (HSQC and HMBC) to yield vital structural information. Some of the more specialist techniques available are then discussed, i.e. flow NMR, solvent suppression, Magic Angle Spinning, etc. Other important nuclei are then discussed and useful data supplied. This is followed by a discussion of the neglected use of NMR as a tool for quantification and new techniques for this explained. The book then considers the safety aspects of NMR spectroscopy, reviewing NMR software for spectral prediction and data handling and concludes with a set of worked Q&As.
1 Getting Started.
Origin of the Chemical Shift.
Origin of "Splitting".
2 Preparing the Sample.
How much sample do I need?
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 (Proton NMR).
3 Spectrum Acquisition.
Number of Transients.
Number of Points.
Number of Increments.
Tuning and Matching.
To Spin or Not to Spin.
Zero-Filling and Linear Prediction.
5 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.
6 Delving Deeper.
Enantiotopic and Diastereotopic Protons.
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.
7 Further Elucidation Techniques – Part 1.
Basification and Acidification.
Lanthanide Shift Reagents.
Chiral Resolving Agents.
8 Further Elucidation Techniques – Part 2.
Spin-Decoupling (homonuclear, 1-D).
COSY (Correlated Spectroscopy).
TOCSY (Total Correlation Spectroscopy) 1&2-D.
The Nuclear Overhauser Effect (NOE) and Associated Techniques.
9 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.
10 Some of the Other Tools.
MAS (Magic Angle Spinning) NMR.
Other 2-D Techniques.
11 Some of the Other Nuclei.
Electronic Reference (ERETIC).
Things to Watch Out For.
Prediction and Simulation Software.
HOSE Code Databases.
Ab initio approaches.
Structural Verification Software.
Structural Elucidation Software.