Basic courses
General information
The theoretical course of NMR (prof. Nickolay M. Sergeyev)
Basic NMR practice
Optional courses
The theoretical course of NMR (Philip V. Toukach)
Extended NMR practice

General information

The NMR Center educational program was created as a part of the Higher Chemical College (Russ. Acad. Scis) educational program. It is also used by the students of Moscow State University, Department of Chemistry, and by any newcomers who are going to obtain the starting knowledge in NMR spectroscopy. The main purpose of the program is to give the students basics of NMR spectroscopy with modern methods emphasized. It is suggested that this allows them to formulate chemical problems and to solve them using NMR spectroscopy.

The NMR educational program for the Higher Chemical College includes lectures and seminars by Prof. N. Sergeyev and practice in the NMR Center. This proceeds usually the second term of the academic year (February-May). The Higher Chemical College students (course 4) are supplied with printed materials including manuals, problems to solve and supplementary data tables.

The basic course of NMR includes the following parts. 14 lectures (once a week), 10 seminars on solution of chemical problems using NMR, and the NMR practice.

The lectures are of increasing complexity and are substantially interlaced with seminars and practice. Seminars proceed usually in N.D. Zelinsky Institute of Organic Chemistry and include analyses of real NMR spectra, control tests and special software applications. At the end of the course each student should suggest a problem to solve that may be a 'live' problem of real research, a theoretical question or a problem from literature. Problems connected to students' own chemical activities are strongly recommended. The NMR practice includes 11 one-hour sessions using Bruker NMR instruments.

Any person wishing to join the classes should address to Prof. Nickolay Sergeyev (e-mail nickser@cacr.ioc.ac.ru) to arrange the access to the course.

The theoretical course of NMR (basic)      (C) Prof. N. Sergeyev.    NMR Laboratory, Department of Chemistry, Moscow State University

The program of the NMR course for Higher Chemical College (prof. N. Sergeyev) includes 14 lectures (28 h.) and 10 seminars (20 h.) and implies the 12 h. of practice in NMR center.

Lectures

1. What is NMR?

2. The NMR phenomenon, its classical and quantum descriptions.
3. Continuous wave NMR and Fourier NMR spectroscopy.
4. Chemical shift.
5. Coupling constants.
6. Organic compounds structure elucidation.

7. Relaxation and macroscopic magnetization vector evolutions.
8. Nuclear Overhauser Effect.
9. The special pulse methods.
10. Some peculiarities of experimental technique.
11. Two-dimensional Fourier spectroscopy.

12. Analysis of high resolution NMR spectra.
13. Computer-assisted analysis of NMR spectra.
14. Temperature and dynamic effects.

Seminars

1. Absolute and relative sensitivity. Sample preparation. Solutions, standarts, gas-phase measurement.
2. The analysis of the proton spectra with first-order multiplicity.
3. Structure elucidation using ¹H NMR spectra.
4. Structure elucidation using ¹³C NMR spectra.
5. Structure elucidation using both ¹H and ¹³C NMR spectra.
6. Structure elucidation using other methods (IR, UV, MASS) together with NMR.
7. Control test.
8. The analysis of NMR spectra using data of 2D NMR spectroscopy.
9. The analysis of NMR spectra using data of 2D NMR spectroscopy.
10. Chemical problems with application of dynamic NMR.

Basic practice       in the NMR Center    N.D. Zelinsky Institute of Organic Chemistry

The practical course of NMR spectroscopy is provided by the NMR center of  IOCh RAoS equiped with Bruker NMR instruments. It aims at giving students an ability to use modern NMR methods at high-resolution (200-300 MHz) NMR instruments.

The Higher Chemical College students are tought the basic practical course which implies teaching to perform routine proton NMR operations and includes a control test of obtaining a high-quality ¹H 1D NMR spectrum. More complex experiments are discussed briefly.

Students are divided into groups of 3-5 persons, each group provided with 10-12 hours of qualified teaching and assistance. The NMR instrument used is Bruker AC200.

Program:

• What does NMR spectrometer consist of?
• Supercon: construction
• Probeheads: selective, broad band, of different bore diameters
• Preamps: ¹H and ¹³C selective, broad band
• Computer, disks, display, keyboard, printer
• Air pumps: air lift, sample spinning, thermostabilizing
• Temperature control unit, thermosensor, heater
• Air lifting and sample spinner

• Spectrometer preparation for ¹H NMR spectra recording
• LOCK signal, its phase, power, gain, tuning and "locking". Deuterumn signal saturation.
• SCM panel, control of sample spinning and shimming coils. Resolution tune-up.

• Aspect 3000 and DISNMR.
• General information on commands and parameters. Multitasking in three independent jobs.
• Basic pulse sequence GO (ZG), which elementary steps it implies in the spectrometer
• Relaxation delay, pulse width, number of scans
• Receiver gain and its automatical adjustment
• Sample title and transferring the NMR data over the network

• Weight functions and corresponding parameters
• General information on spectrum processing. Knobs A-D and their functions.
• EP functions: phase adjustment, spectrum calibration, peak picking
• EP: integration subroutine
• Selecting and storing a part of spectrum to plot, plot parameters adjustment
• Spectra output and its automation

• Practical experience in routine NMR spectra recording (see also DISNMR command list)

• Demonstration of 2D H,H COSY, difference mode 1D NOE, DEPT

• Control test (one routine 1D ¹H NMR spectrum must be recorded for 15 min.)

The adapted detail description for all the experiments discussed in the practical course is availbale here: Ph. Toukach "The basic NMR experiments on Bruker WM/AM/AC"

The theoretical course of NMR (optional)      (C) Ph. Toukach, 1996 Mar 16.    N.D. Zelinsky Institute of Organic Chemistry RAoS, NMR Center

The program of optional NMR course (Ph. Toukach) includes from 8 to 10 seminars (2 h. each) with student groups of 1-3 persons, and may include practice in NMR center (additionally 16 h.).

Part 0

1. NMR spectoscopy in chemical research. The unique opportunities of this method. The price of NMR-spectroscopic investigation.

Part 1

1. Physical basics of continuous-wave NMR. The sample in magnetic field. Resonance transitions (briefly).
2. The idea of continuous reamer NMR. What is NMR spectrum?
3. Information provided by NMR spectrum: signals quantity, their position, form and square.
4. Nuclei screening by various chemical surround. The chemical shift and its ranges for different nuclei.
5. Proton chemical shifts, in correlation to the structure. Standarts, TMS.
6. The reasons of multiplicity. Pascal triangle etc.
7. Structural variations of spin-spin coupling constants (SSC), SSC in dependance on the number and type of bonds, torsion angle, heteroatoms and conugation.
8. Roof effect. NMR spectra of the first order and not.
9. Chemical exchange, signal of hydroxy- and amino-groups. Chemical shift temperature variations. NMR response time. Bond rotation and other dynamic effects.
10. The signal square. NMR spectrum integration.
11. Examples of proton spectra (substituted benzene, ethanol etc., considering roof effects and signals overlap).
12. The idea of additive ¹³C NMR spectra calculation.
13. Heteronuclear SSC. The ¹³C Gated experiment. The result of proton broadband decoupling. ¹³C satellites. The isotope shift (briefly).
14. Selected notes on double resonance and the result of this experiment. The Bloch-Zigert shift. The idea of difference mode experiments.

Part 2

1. The idea of pulse NMR. "Bell tuning" (by A. Derome).
2. NMR data in frequency and time domain. The Fourier transformation.
3. Relaxation (briefly). Exponential free induction decay. Lorenz line.
4. The data excerption rate required. The demands to ADC performance. What is the analog signal and its digital representation? Computer memory and precision required.
5. The principial spectrometer scheme and connection of its computer to I/O devices. The supercon and its principle.
6. Types and purposes of NMR probeheads.
7. Types and purposes of amplifiers and filters.
8. Controlling the computer (briefly): the operating system, software, the experiment acquisition and processing sequence: "shimming-acquisition-mathematical operations-output".
9. Digital resolution. The spectrum window. The number of data points.
10. What is the signal phase? Absorbtion and dispersion signals. Reflected signals and their phase.
11. What are resolution and sensitivity. Purpose and types of gradient shimms. The resolution adjustment using deuterium signal as a reference. FID square and outlook, depending on the resolution.
12. The deuterium stabilization (LOCK).
13. Factors affecting the resolution and sensitivity: NMR tube, sample volume, concentration and viscosity. How to select the solvent?
14. The signal/noise ratio. Why to accumulate data? The elementary experiment GO: "relaxation delay-pulse-delay-acquisition".
15. Basics of DISNMR, three jobs. Keyboard: the immediate parameters change or process start. SCM-panel: the gradual parameters change.
16. Pre-FT FID processing. Zero filing, cut-off and apodization.
17. Weight functions. Exponential multiplication and Gauss enhance.

Part 3 (based on A. Derome's book)

1. The direction of macroscopic magnetization (MM) vector and how it is formed.
2. The oscillating radio-frquency field representation as a pair of precessing vectors.
3. The rotating co-ordinate frame (RCF), examples.
4. Post-pulse MM evolution in RCF, examples. Types of pulses.
5. Detecting several frequencies at once, several MM vectors precessing in RCF.
6. The pulse phase and the idea of quadrature detection. Phase cycles (briefly).
7. Spin-lattice relaxation. What do FID oscilattions really represent?
8. Spin-spin relaxation.
9. The reasons of spin echo. It's use for SSC constants differenciation.

Part 4

1. The signal intensity, depending on the neighbouring spins irradiation. Nuclear Overhauser Effect observation experiments, the example of 2,4- and 3,4-dibromtoluene. NOEDIFF experiment.
2. The idea of two-dimentional NMR spectroscopy. Basics of H/H COSY experiment.
3. Homo- and heteronuclear COSY, HMQC, HMBC (briefly: the information provided by these experiments, examples).
4. COSY RCT, RCT2, TOCSY, DQF COSY (briefly: the information provided by these experiments).
5. NOESY and ROESY (briefly: the information provided by these experiments).
6. The possibilities of spectra edition, INEPT, DEPT, SPT and APT experiments.
7. The solvent signal suppresion in one- and two-dimentional spectroscopy. Decoupler.
8. Other experiments. What does the professionalism of NMR researcher assumes?

The optional literature is A.E. Derome "Modern NMR techniques for chemistry research", Pergamon Press. The russian edition is by Moscow "MIR", 1992.

Download the russian translation of "Selected notes on Fourier NMR spectroscopy and its application in carbohydrate research" by Ph. Toukach (strongly interlaces with the course)   (ZIPped RTF, 4 Mb)

Any person wishing to attend this course should address to Philip Toukach (e-mail tou@ioc.ac.ru).

Extended practice       in the NMR Center    N.D. Zelinsky Institute of Organic Chemistry

The extended practical course of NMR spectroscopy is provided by the NMR center of  IOCh RAoS equiped with Bruker NMR instruments. It aims at giving students an ability to use variety of modern NMR methods at high-resolution (200-300 MHz) NMR instruments. Each group of 1-3 students is provided with 12-20 hours of qualified teaching and assistance. The NMR instruments used are Bruker AC200, WM250 and AM300.

The detail description for all the experiments discussed in the practical course is available here:

Ph. Toukach "The basic NMR experiments on Bruker WM/AM/AC",
which includes all the nuances of the following:

• ¹H 1D NMR experiment without solvent suppression
• The special notes on solvent suppression (SSHD)
• ¹³C and other heteronuclei 1D NMR experiment special notes
• Cables connecting
• Special notes on homedecoupling (direct way, DIF, DIFSUP)
• Pulse length measurement
• Organizing the chain of NMR experiments
• H/H COSY experiment (COSY, COSY45)
• COSY RCT and RCT2 experiments special notes (COSYRCT, COSYRCT2)
• DQF COSY experiment special notes (COSYDQF)
• Special notes on solvent suppression in COSY-related experiments (COSYHG, COSYRCTG, COSRCT2G)
• 2D NOESY experiment special notes (NOESY)
• 2D ROESY experiment (ROESYW)
• {¹H-¹³C} correlation without J_CH suppression (BIRDPHPR)
• APT experiment (JMODXH)
• {¹³C-¹H} correlation (XCORRD)
• 1D NOE difference experiment (NOEDIFF)
• Multiple 1D NOE experiments (NOEMULT)
• DISNMR commands: basic, system, plot, for 2D-experiments, phase editor

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