lecture4-Relaxation1讲课.ppt

Relaxation Relaxation Relaxation Other Relaxation Mechanisms T1 and T2 Longitudinal Relaxation (T1) Transverse Relaxation (Mxy→Equilibrium) T1 and T2 400 MHz NMR Spectrometer 400 MHz Superconducting Magnet Superconducting Magnet Locking the Magnetic Field Shimming Sample Spinning NMR Sample Position(prior to release into probe) NMR Sample Probe NMR Experiments PFT-NMR Experiment On-resonance Brf viewed in the rotating frame As before, The NMR Practitioner’s Convention RF applied along x-axis Populations of Spin States and RF Pulses 90? and 180? pulses Elements in Organic Chemistry H : Best NMR element 1H , I = ? (sharp lines), a = 99.98% , high frequency (n = 100 MHz) 2H , I =1 (broad lines), a = 0.02%, n = 15.4 MHz, Q=0.038 C : 12C , I = 0 (no signal in NMR) 13C , I = ? (sharp lines), a = 1.1% , n = 25.3 MHz N : 14N , I =1 (broad lines), a = 99.6%, n = 7.2 MHz, Q=1.0 15N , I = ? (sharp lines), a = 0.4% , n = 10.1 MHz O : 16O , I = 0 (no signal in NMR) 17O , I =5/2 (broad lines), a = 0.04%, n = 13.5 MHz, Q=-0.037 Elements in Organic Chemistry C-13 NMR: Quantitative?? In C-13, some carbons can have long relaxation time: If the relaxation delay is not long enough, the long relaxation carbons will not achieve full amplitude NOEs varies for the various carbons The efficiency of the pulse vary depending if a signal is in the center of the window or on the side. C-13 NMR Shifts Some Advantages of C-13 NMR The chemical shift range for carbon NMR is about 200 for typical organic compounds — there is less overlap between peaks JCC is not usually observed -: Probability of neighboring 13C is 1:104 — each unique carbon give rise to a single peak By looking at the multiplicity of each carbon signal we can tell the number of protons attached -: the 13C-1H interaction can be decoupled Additional Elements in Organic Chemistry Halogens: 19F, Cl, Br, I 31P, S B, 29Si Na Co, Cd, W, Pt, Hg… Liquid Helium -269°C (4.2 K) Liquid Nitrogen -196°C (77.4 K) N