Course Syllabus for English-Taught Majors

Special Topics for NMR Spectroscopy’Course Syllabus

 

Course Code09040012

Course Category专业选修课程 Major elective

MajorsChemistry, Chemical Engineering

SemesterFall

Total Hours36 Hours        

Credit

Lecture Hours36 Hours          Lab Hours        Practice Hours0

InstructorsXiaohong Li, Peter Rinaldi

TextbooksR. M. Silverstein et al., Spectrometric Identification of Organic Compounds, 8th Ed., Wiley, 2014.

References

   

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.

 

 

Teaching Aim

 

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

课时:1周,共2课时

Contents

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

课时:1周,共2课时

Contents

1.Magnet

2.Rf Components

3.Role of computer

 

Chapter Three       Proton NMR spectra

课时:2周,共4课时

Contents

1.Chemical Shift

2.Peak intensities

3.J Coupling

4. Relaxation (T1, T2)

 

Chapter Four Carbon 13 NMR spectra

课时:2周,共4课时

Contents

1.Chemical Shift

2. Peak intensities

3. J Coupling

4. Relaxation (T1, T2)

 

Chapter Five What should I do before I go to the NMR Lab

课时:1周,共2课时

Contents

1.Sample amount

2.Tubes

3.Solvents

4.Height

5.Look at sample ( undissolved, sample uniformity)

 

Chapter Six    Getting the best 1D-NMR spectrum Data Collection and Processing

课时:1周,共2课时

Contents

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

课时:1周,共2课时

Contents

1.Diffusion process

2.NMR with pulsed magnetic field gradients

3.Basic Gradient diffusion measurements (Stejskal/Tanner Equation)

4.Nucleus

5.Nature of sample (large/small molecule)

6.Gradient and diffusion delays

7.Convection

8.J Coupling artifacts

9.Spectral Window

 

Chapter Eight Intro to 2D-NMR

课时:1周,共2课时

Contents

1.Pulse sequence

2.Terminology

 

Chapter Nine  Methods for determining atomic connectivity

课时:1周,共2课时

Contents

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)

课时:1周,共2课时

Contents

1. Baseline correction

2. Weighting

3. Data extension

4. Dataset size/digital resolution

5. Undesired signal cancellation

 

Chapter Eleven      Presentation of 2D data (XL)

课时:1周,共2课时

Contents

1.Contours and spacing

2.Region selection

3.Labeling

 

Chapter Twelve      Quantitative NMR Data Collection

课时:1周,共2课时

Contents

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)

课时:1周,共2课时

Contents

1.How many points to transform

2.Weighting data

3.Digital resolution and integral accuracy

4.Baseline correction

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)

课时:1周,共2课时

Contents

1. T1 Inversion recovery

2. What can go wrong

3. T2 Carr Purcell Meiboon Gill echo experiment

 

Chapter Fifteen      Filtering interfering signals (ethics) (PLR)

课时:1周,共2课时

Contents

1.Gradients

2.Phase cycling

3.Decoupling

4. Multiple Quantum

5.Spectral addition/subtraction

 

Chapter Sixteen      Real samples detection experiments

课时:1周,共2课时

Contents

 

Students test the unknown samples by remote login the NMR instrument in groups.

 

 

Assessment Methods

Quiz

Homework Assignments

Real Sample Detection experiments

Final Exam

 

                                 Made by Xiaohong Li

                                 Date: 09/01/2016