‘Special Topics for NMR Spectroscopy’Course Syllabus
Course Category：专业选修课程 Major elective
Majors：Chemistry, Chemical Engineering
Total Hours：36 Hours
Lecture Hours：36 Hours Lab Hours：0 Practice Hours：0
Instructors：Xiaohong Li, Peter Rinaldi
Textbooks：R. M. Silverstein et al., Spectrometric Identification of Organic Compounds, 8th Ed., Wiley, 2014.
•R. M. Silverstein et al., Spectrometric Identification of Organic Compounds, 8th Ed., Wiley, 2014.
•M. H. Levitt, Spin Dynamics: Basics of Nuclear Magnetic Resonance, Wiley, 2005.
•J. Keeler, Understanding NMR, Wiley, 2005.
•S. Braun et al., 150 and More Basic NMR Experiments, 2nd Ed., Wiley, 1999.
This course will focus on the basic theory of how NMR spectroscopy works, fundamentals of Fourier transform spectroscopy, maximizing the available spectral information, data quality and reliability through optimization of data collection and processing parameters. It intended for advanced undergraduate and beginning graduate students who expect to collect and process their own data. There will be discussions and examples of how to recognize bad/unreliable data, the best way to present spectroscopic data, when an experiment should be repeated, and difference between acceptable and unethical data manipulation. Concepts will be illustrated with a generous number of figures from real spectral data of small molecules and polymers. Underlying themes throughout the course will also include the scientific method, ethics in science and spectroscopy, and environmental issues. These will be discussed by comparing and drawing parallels between spectroscopic data and digital photography. Generous use of striking digital images from international world heritage sites will be used for this purpose.
Chapter One Fundamental NMR
1. What causes nuclear spin
2. Interaction of nuclear spin with a magnetic field
3. Spin polarization, magnetic moment, Boltzmann distribution
4.Sensitivity compared to other spectroscopy
5.Detectable Nuclei Periodic Table
6.Detectability, magnetic moment, isotopic abundance, magnetic field strength
7.Commonly observed nuclei H,C,F,P
8.Rotating reference frame, interaction of spins with B0 and B1
9. Basic one pulse 1D-NMR experiment
Chapter Two NMR Instrument
3.Role of computer
Chapter Three Proton NMR spectra
4. Relaxation (T1, T2)
Chapter Four Carbon 13 NMR spectra
2. Peak intensities
3. J Coupling
4. Relaxation (T1, T2)
Chapter Five What should I do before I go to the NMR Lab
5.Look at sample ( undissolved, sample uniformity)
Chapter Six Getting the best 1D-NMR spectrum Data Collection and Processing
1.1D NMR optimization (pulse width/relaxation delay, acquisition time)
2.Optimimum instrument receiver gain
3.Signal averaging (nt vs. signal to noise level)
4.Processing for best S:N (zero filling, weighting data)
*How can I get a good spectrum in 1 hour instead of 16 hours without making more sample
*How do I get more of my overnight experiments to work. What should I do before I go home for the evening and let the instrument collect my data overnight.
*I collected this spectrum overnight and still don’t see my peaks can I please have one more hour to get better signal to noise? Why this is folly.
*Limits of detection
*How accurate are my chemical shifts?
*I don’t have any sample left and the spectrum I collected all weekend has no peaks!! (90% of the time signals can be recovered from these spectra with optimal data processing)
Chapter Seven Diffusion Measurement
2.NMR with pulsed magnetic field gradients
3.Basic Gradient diffusion measurements (Stejskal/Tanner Equation)
5.Nature of sample (large/small molecule)
6.Gradient and diffusion delays
8.J Coupling artifacts
Chapter Eight Intro to 2D-NMR
Chapter Nine Methods for determining atomic connectivity
1.Homonuclear 2D NMR
2.Heteronuclear 2D NMR
3. Structure information
4. SFORD, APT, INEPT, DEPT
5. Multiplicity edited 2D-NMR
6. Filtering interfering signals (ethics)
Chapter Ten 2D-Processing (XL)
1. Baseline correction
3. Data extension
4. Dataset size/digital resolution
5. Undesired signal cancellation
Chapter Eleven Presentation of 2D data (XL)
1.Contours and spacing
Chapter Twelve Quantitative NMR Data Collection
1.Role of relaxation and parameter optimization
2. T1 experiment
3. What can go wrong with T1 measurement and is the data still acceptable?
4. Uniform excitation (relation between pulse width and real excitation window)
5. Data Acquisition time
Chapter Thirteen Quantitative NMR Data Processing (XL)
1.How many points to transform
3.Digital resolution and integral accuracy
5.How should I break up integrals?
6.How wide are my lines and why do I need to know (The Lorenzian lineshape)
7.Limits of Quantitation (importance of good signal to noise level)
Chapter Fourteen Relaxation Measurement (PLR)
1. T1 Inversion recovery
2. What can go wrong
3. T2 Carr Purcell Meiboon Gill echo experiment
Chapter Fifteen Filtering interfering signals (ethics) (PLR)
4. Multiple Quantum
Chapter Sixteen Real samples detection experiments
Students test the unknown samples by remote login the NMR instrument in groups.
Real Sample Detection experiments
Made by ：Xiaohong Li