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NMR Spectroscopy. Two-dimensional NMR. http://www.univ-lille1.fr/lcom/RMN2D/resum2D_us/index_us.htm. 1D NMR. Pulse Sequence. Spectrum (EtOH). Four periods in 2D experiment. Preparation spin system relaxes and then excited by r.f.
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NMR Spectroscopy Two-dimensional NMR http://www.univ-lille1.fr/lcom/RMN2D/resum2D_us/index_us.htm
1D NMR Pulse Sequence Spectrum (EtOH)
Four periods in 2D experiment Preparation spin system relaxes and then excited by r.f. Evolution (t1) chemical shifts & spin-spin couplings evolve. This is the timedomain which is incremented during a 2D experiment Mixing r.f. pulses are applied and create observable transverse magnetization Detection (t2) observable transverse magnetization is recorded. It is usually labeled with t2
2D NMR • Primary 2D matrix consists a series of FIDs. • A set of 1D NMR spectra is obtained by Fourier transformation with respect to t2 • The signals of each transformation may differ in amplitude and phase. A second Fourier transformation with respect to t1 yields the final 2D matrix with frequency axes F1 and F2 1. 2. 3.
2D NMR Pulse Sequence Spectrum
2D J-resolved COSY 45.COSY 90.COSY DQF.TOCSY. COSY L.R.TOCSY Relayed COSY. (with one homonuclear relayed). NOESY.ROESY.
HMQC The HMQC experiment provides correlation between protons and their attached heteronuclei through the heteronuclear scalar coupling. HMBC The HMBC experiment suppresses correlations via 1JC,H while 2J, 3J can be conserved. HSQC The HSQC experiment is in fact a double INEPT experiment. This experiment correlates protons with their directly attached heteronuclei. (G. Bodenhausen and D. J. Ruben, Chem. Phys. Lett., 69, 185 (1980)
Basic HMQC Experiment F2 displays the doublets with the spin coupling constant 1J(C-H) in addition to the H,H spin coupling.
HMQC with Decoupling Only singlets are displayed in F2 . These signals are further split by H,H spin couplings.
Basic HMBC Experiment Cross signals caused by 1J of C-6 and C-3 are still observable but those arising from 3J and 2J are predominant.