1. Introduction to Nuclear Magnetic Resonance---NMR Principle of NMR

2. without Magnetic Field In the Magnetic Field B0B0 Magnetic Nuclei In the absence of the field B0, the Magnetic nuclei in the sample are oriented randomly.In the magnetic field, they must adopt either the aligned orientation(of lower energy) or the opposed orientation(of higher energy).

3. without Magnetic Field In the Magnetic Field B0B0 EE Energy Level Magnetic Nuclei In the absence of B0 the magnetic nuclei all have the same energy. When B0 is applied,the aligned and opposed orientations correspond to different energies,the energy difference,  E, having the dimension hv. hv

4. without Magnetic Field In the Magnetic Field B0B0 EE Magnetic Nuclei When the nuclei(in the magnetic field) are irradiated with radio- frequency(RF) energy of the appropriate frequency, some of them undergo transitions from the aligned to the opposed orientations and vice versa. （ Resonance!!!) Resonance condition : W(2 兀 f )= r B0 f=RF, r = Gamma ratio,  E=h

5. Energy Level  E E 300MHz 7.0T 500MHz 11.4T 800MHz 18.8T Field-frequency relationship

6. Magnetic moment(1) 1 If both the mass number(A) and the atomic number(Z) are even, I = 0 (No NMR signal) 12 C, 16 O 2 If (A) is odd and (Z) is odd or even, I will have half- integral values. I =1/2, 3/2, 5/2 etc 1 H, 19 F, 29 Si, 11 B(3/2), 17 O(5/2) 3 If (A) is even and (Z) is odd, I will have integral value 1,2,3 etc. 14N, 6Li,

7. Magnetic moment(2) 2H nucleus 1 proton 1 neutron magnetic 1H nucleus 1 proton magnetic 4He nucleus 2 protons 2 neutrons Non-magnetic 12C nucleus 6 proton 6 neutrons Non-magnetic 13C nucleus 6 protons 7 neutrons magnetic

8. Typical Magnetic Isotopes Resonance condition: W(2 兀 f )= r B0 1H : 2x3.14 x400(25.12) = 26.75 x 9.39(25.118) 13C: 2x3.14x100.533(63.13)= 6.73x9.39(63.19)

9. Sensitivity Table relative to 13C

10. Block diagram of NMR instrument RF Oscillator RF Gate Pulse Programmer RF Power Amplifier Pre- amplifier Phase Sensitive detector AD Converter Computer Display Printer Probe SCM

11. ECA 500 NMR JEOL LTD Composition of NMR instrument

12. The NMR information 1) Chemical Shift 2) Spin-Spin Coupling 3) Intensity(Area) of Signal 4) Relaxation(T1,T2) 5) NOE

13. Chemical Shift TMS TMS:Tetra- Methyl-Silane Chemical shift

14. Chemical Shift Table -CH2- 13 C Chemical Shift

15. Spin-Spin Coupling A B C D E CH3-CH2-O-C-CH=CH-CH3 A C O E D B

16. Intensity(Area) Information

17. Integration 1.00 1.02 0.99 1.02 1.99 2.02 2.03

18. Various measurement methods 1 dimension (1H,13C,DEPT,…….) 2 dimension (COSY,NOESY,TOCSY,HMBC,HMQC,…) 3 dimension (COSY,NOESY,TOCSY,HMBC,HMQC,…) 4 dimension (COSY,NOESY,TOCSY,HMBC,HMQC,…)

19. 1 dimensional NMR(1D NMR) 50mg samples,Solvent acetone-d6

20. 2 dimensional NMR X Y X : 1H, 13C, 1H Y : 1H, 1H, 15N

21. 2 dimensional NMR

22. 2 dimensional NMR(2 D NMR) Methylene carbon of B,G,H,J is shown two correlation signals with Proton, this methylene proton is non-equivalent.

23. 3 dimensional NMR X Y Z X : 1H Y: 13C Z : 31P

24. Three Dimensional NMR 3D NMR is standard with the Eclipse + NMR spectrometer

25. 4-Dimensional NMR Data Processing Delta’s Standard Multi-Dimensional NMR Data processing tool uses the same user interface as 1D and 2D data processing

26. 4 dimensional NMR X Y Z A X : 1H Y : 13C Z : 15N A : 31P

28. Application field of NMR Liquid NMR Structure elucidation of natural product,polymer etc natural product,polymer etc Stereo- structure elucidation protein etc protein etc Molecular diffusion Relaxation measurement Dynamic measurement Solid NMR NMR Imaging Structure elucidation Stereo-structure information Relaxation information Spin density Relaxation information Dynamic information (Flow imaging)