Topics in Physical Chemistry: Magnetic Resonance
Experimental Nuclear Magnetic Resonance Spectroscopy in Liquids and Solids
4 credit hours
Instructor: Dr. Mark D. Poliks Office Phone: 757-1424
Email: firstname.lastname@example.org Fax: 757-1156
Office hours: After class in Sc II 245 or by appointment.
Course Goal: To provide a structured environment to acquire basic NMR theory and laboratory techniques for organic, physical and materials chemists.
Course requirements: Attend lectures, outside reading, laboratory work (1/3) assisted by Dr. Schulte, midterm (1/3) and final report/presentation (1/3).
Midterm examination will cover NMR fundamentals covered in lectures and readings.
Students may choose a family of compounds to characterize from their research for laboratory assignments.
Solid-State NMR methods will be included in lectures and laboratory.
Textbooks: "Nuclear Magnetic Resonance", P. J. Hore, Oxford Science Publications, 1998.
"Modern NMR Spectroscopy - A Guide for Chemists", J. K. M. Sanders and B. K. Hunter, 2nd edition, Oxford, 1993.
Supplemental textbooks: "Basic One- and Two- Dimensional NMR Spectroscopy", Horst Friebolin, VCH Publishers, 1998.
"150 and More Basic NMR Experiments -- A Practical Course", S. Braun, H.-O. Kalinowski and S. Berger, VCH Publishers, 1998.
Week # Tentative Lecture &Lab Topic (with links to lecture notes and animations)
# 02 Principles of NMR, Experimental NMR in isotropic liquids, Course Project requirement, Pulse width calibration
# 03 Density matrix formalism and coherence, Common "rare" Nuclei solution NMR
# 04 Spin tickling and decoupling methods, laboratory project topic due
# 05 NMR Relaxation, spin echoes and spin/spin relaxation
# 06 Molecular dynamics and spin/lattice relaxation
# 07 Nuclear Overhauser effect and internuclear distances
# 09 Formalism in 1D methods
Anisotropy of the chemical shift, dipolar and quadrupolar interactions in solids,
Magic-angle spinning and cross polarization dynamics
# 13 Proton NOESY
# 14 NMR Imaging, complete laboratory project , schedule lab quiz with Dr. Schulte
# 15+16 Last week of classes, make-up lecture/discussion, prepare project presentation
0 NMR Lab Training
1 Comprehensive 1H NMR and Indirect 13C Observation
2 Pulse Width Calibration and B1
3 Rare spin NMR
4 Decoupling 1H from 13C and B2
5 Spin Echo and Spin/Spin Relaxation, T2
6 Spin/Lattice Relaxation, T1
7 Nuclear OverHauser Effect
8 Polarization Transfer and DEPT
9 13C CP/MAS in Solids
10 HETCOR (1H/13C COSY)
11 1H COSY / NOESY (optional)
In all assignments you are expected to report on the following information:
Chemical shifts and method of reference in relation to structure
J coupling (homo and heteronuclear) in relation to structure
Peak intensity and area in relation to concentration and structure/dynamics/relaxation
Effect of B0 / lab magnetic field strength, Larmor frequency and gyromagnetic ratio
Effect of B0 inhomogeneity
Pulse width and tip angle
Magnitude of B1 and B2 fields / rf field strengths used
Effect of B1 and B2 inhomogeneity
Effects of O1 and O2 / frequency offsets
Effects of sample spinning and location of spinning sidebands
Method of decoupling if used as well as effectiveness
Solvent and temperature used
Pulse sequence and instrument control programming
All critical instrument or data processing parameters
Vector and spin diagrams, as needed.
Note any experimental or instrumental anomalies
All data taken using the department's NMR spectrometers must have the highest possible quality that can be obtained. Dr. Schulte must approve of your data before leaving the lab. Problems that cannot be resolved must be documented in your lab report. Data will only be provided if there are major equipment problems. Incomplete reports with poor data will not be accepted and the laboratory work will have to be repeated.