Chemistry 485f/585f

Topics in Physical Chemistry: Magnetic Resonance

Experimental Nuclear Magnetic Resonance Spectroscopy in Liquids and Solids

4 credit hours

Course Location: Science II, Room G-35, Monday/Wednesday, 6:00 to 7:30 PM

Instructor:        Dr. Mark D. Poliks                                           Office Phone:  757-1424

Email:              mpoliks@eitny.com                                                    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)

# 01                 Course overview, laboratory plan requirement, NMR and the Periodic Table,
Proton solution NMR, schedule training sessions with Dr. Jürgen Schulte

# 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

# 08                 Polarization transfer and spectral editing ( INEPT & DEPT   )

# 09                 Formalism in 1D methods

# 10                 Anisotropy of the chemical shift, dipolar and quadrupolar interactions in solids,
Magic-angle spinning and cross polarization dynamics

# 11                 Formalism in 2D methods, J-Resolved / Proton COSY

# 12                 Heteronuclear COSY (HETCOR  )

# 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

Laboratory Assignments:     Manual 1       Manual 2

            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:

Signal-to-noise ratio

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

Data Quality (HTML/ Powerpoint)

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.