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Crash course in applied NMR

Practical aspects. Sample preparation:No solids!Balanced tubes, proper fillingChoice of solvents, deuterium lockingTube handling and cleaningTube labelingThere is an on-line manual for our NMR!. Instrument etiquette. Indicate when machine is in useReturn everything as you found itNo metals around NMRLeave door closed (and AC in control)Consider sample concentration, no endless runs during day time.

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Crash course in applied NMR

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    1. Crash course in applied NMR

    2. Practical aspects Sample preparation: No solids! Balanced tubes, proper filling Choice of solvents, deuterium locking Tube handling and cleaning Tube labeling There is an on-line manual for our NMR!

    3. Instrument etiquette Indicate when machine is in use Return everything as you found it No metals around NMR Leave door closed (and AC in control) Consider sample concentration, no endless runs during day time

    4. Basic considerations CV vs. FT principles Locking, shimming Definitions: pulse, pulse delay Signal to noise ratio Proton vs. carbon Sample spinning Spinning side bands TMS outdated – chloroform signal at 7.26

    5. A second look at interpretation Kinetic effects: DMF has two methyl peaks! Methylcyclohexane (below): same shift for axial/equ. methyl

    6. Exchangeable protons Types: amines, alcohols, carboxylic acids Pooling of different types Peak broadening, see below “Shaking out” with D2O Absence of spin splitting

    7. Second order considerations Conditions for 2nd order Leaning peaks, uninterpretable spectra

    8. Description of spin systems J values 1, 2, and 3 bond coupling Long range coupling Spin systems: A-B, A-X etc.

    9. Aromatic patterns: phenyl

    10. Aromatic patterns: disubstitution

    11. Ortho, multiple subst.

    12. Lanthanide shift reagents

    13. Suggested review McMurry, discussion of homotopic, heterotopic, enantiotopic, and diastereotopic relationships Hoffman Ch. 11

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