2 nd n nmr - ubi.pt
TRANSCRIPT
NMR - from theory to practice - 10th - 14th February 2014
10th-14th
FEB
2014
FUNDAMENTALS OF LIQUID STATE NMRSTRUCTURAL ANALYSIS OF SMALL MOLECULESHANDS ON ACQUISITION AND PROCESSING
TUTORS: EURICO CABRITA MARTA CORVO FILIPA MARCELO ANGELO FIGUEIREDO CARLA CRUZ
NMRFROM THEORY TO PRACTICE
2ND ED
ITION
Course ObjectivesBasic formation in the theory and practice (acquisition and processing) of Nuclear Magnetic Resonance in the liquid state.
One day “hands-on” classes on NMR based Structural Analysis of small molecules.
The basic theoretical principles of NMR will be reviewed. Standard homonuclear and heteronuclear 1D and 2D techniques employed in structural analysis will be approached with special emphasis to acquisition and processing theory and routines.
With "hands on” practice on acquisition and processing (Bruker Avance III 400 and 600 MHz spectrometers).
Schedule
Monday Tuesday Wednesday Thursday Friday
9:00-10:30
10:30-11:00
11:00-12:30
12:30-14:00
14:00-16:00
16:00-16:30
16:30-18:30
Basic 1D NMR
theory
Basic 2D NMR theory
Structural Analysis
Strategies
CaseStudies
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General NMR Theory
Basic 1D NMR
theory
Basic 2D NMR theory
Structural Analysis
Strategies
CaseStudies
Lunch Lunch Lunch Lunch Lunch
General Aspects Practical
NMR
1H, 13C Acquisition/Processing
2DAcquisition/Processing
Spectrainterpretation
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Spectrometer Calibration
1H, 13C Acquisition/Processing
2DAcquisition/Processing
Spectrainterpretation
NMR - from theory to practice - 10th - 14th February 2014
Detailed Program
DAY 1 - Monday 10th February 2014
Morning Session 11:00 - 12:30
Introduction and General Concepts- Spin, angular momentum, magnetic moment- Interaction with magnetic fields, Precession, Larmor frequency- Relaxation, interaction with radiofrequencies, magnetic coherence, laboratory and rotating-frame
referencials- Saturation
Theoretical aspects for spectral acquisition- Radiofrequency pulses- NMR signal (FID) and Fourier Transformation- Signal intensity and S/N ratio- Sampling, digitalization and detection- Digital and real resolution and acquisition time- Phase- Processing parameters and apodization functions
Afternoon Session14:00 - 16:00
Presentation of the NMR spectrometer and its principal componentsSample preparation
16:30 - 18:30
Preparing the NMR for data acquisition (lock, shimming, tuning, etc)Pulse calibration
NMR - from theory to practice - 10th - 14th February 2014
DAY 2 - Tuesday 11th February 2014
Morning Session 9:00 - 12:30
Simple pulse experiments - 1H and 13C - Pulse calibration- Proton decoupling and the nuclear Overhauser effect in 13C NMR
Multiple pulse experiments- Determination of T1 - the inversion recovery experiments- Spin echoes - determination of T2 and J coupling modulation
- The Attached Proton Test (APT)
Afternoon Session14:00 - 18:30
The 1H NMR experiment - acquisition and processing- resolution, S/N ratio, apodization functions, etc
The 13C NMR experiment - acquisition and processing- resolution, S/N ratio, apodization functions, etc
Introduction to multiple pulse experiments (T1 determination, APT, water suppression)
DAY 3 - Wednesday 12th February 2014
Morning Session 9:00 - 12:30
Introduction to 2D NMR techniques - The second dimension- Correlation spectroscopy (COSY)- Other homonuclear techniques (TOCSY, NOESY)- Introduction to heteronuclear correlation (HETCOR, HMQC, HSQC, HMBC)
Practical aspects for the acquisition and processing of 2D NMR
Afternoon Session14:00 - 18:30
Acquisition and processing of 2D experiments (COSY, HSQC, HMBC)
NMR - from theory to practice - 10th - 14th February 2014
DAY 4 - Thursday 13th February 2014
Morning Session 9:00 - 12:30
Chemical shift and J coupling in structural and conformational analysis
Strategies for the structural elucidation of unknowns
Afternoon Session14:00 - 18:30
From spectra to structures - exercises
DAY 5 - Friday 14th February 2014
Morning Session 9:00 - 12:30
Case Studies
NMR - from theory to practice - 10th - 14th February 2014
Tutors
NAME CONTACT INSTITUTION
Eurico J. Cabrita [email protected] FCT-UNL
Angelo Figueiredo [email protected] FCT-UNL
Filipa Marcelo [email protected] FCT-UNL
Marta C. Corvo [email protected] FCT-UNL
Carla Cruz [email protected] UBI
NMR - from theory to practice - 10th - 14th February 2014