Spin decoupling broadband

In C NMR spectroscopy, three kinds of heteronuclear spin decoupling are used In proton broadband decoupling of C NMR spectra, decoupling is carried out unselectively across a frequency range which encompasses the whole range of the proton shifts. The speetrum then displays up to n singlet signals for the n non-equivalent C atoms of the moleeule. 

SUSAN Spin decoupling employing ultra-broadband inversion sequences generated via simulated annealing (broadband decoupling sequence) 9.2... 

In DOUBLE ENDOR (Sect. 4.3) the spin system is simultaneously irradiated with two rf fields. The frequencies of both fields have to be set independently from each other. Generation of rf fields by broadband DOUBLE ENDOR instruments are often strong enough for solid state studies at low temperature. In spin decoupling experiments (Sect. 4.4), however, the amplitude of one of the two fields (namely the decoupling field) should be as large as possible, whereas in studies of multiple quantum transitions ) (Sect. 4.5) two strong rf fields have to be applied. 

Shaka AJ and Keeler J (1987) Broadband spin decoupling in isotropic liquids. Progress in NMR Spectroscopy 19 47-129. 

Decoupling (Section 13 17) In NMR spectroscopy any process that destroys the coupling of nuclear spins between two nuclei Two types of decoupling are employed in NMR spectroscopy Broadband decoupling removes all the H- C couplings ojf resonance decoupling removes all H- C couplings except those between directly bonded atoms... 

Figures 1.9a and b demonstrate the effeet of proton broadband deeoupling in the C NMR speetrum of a mixture of ethanol and hexadeuterioethanol. The C//j and CH2 signals of ethanol appear as intense singlets upon proton broadband deeoupling while the CD3 and CD2 resonanees of the deuteriated eompound still display their septet and quintet fine strueture deuterium nuelei are not affected by H decoupling because their Larmor frequeneies are far removed from those of protons further, the nuelear spin quantum number of deuterium is 7/3=/ in keeping with the general multiplieity rule (2nx Ix+ 1, Seetion 1.4), triplets, quintets and septets are observed for CD, CD2 and CD3 groups, respeetively. The relative intensities in these multiplets do not follow Paseal s triangle (1 1 1 triplet for CD 1 3 4 3 1 quintet for CD2 1 3 6 7 6 3 1 septet for CD3).

The main contribution to the spin-lattice relaxation of C nuclei which are connected to hydrogen is provided by the dipole-dipole interaction (DD mechanism, dipolar relaxation). For such C nuclei a nuclear Overhauser enhancement of almost 2 will be observed during H broadband decoupling according to ... 

Most 13C spectra are run on Fourier-transform NMR (FT-NMR) spectrometers using broadband decoupling of proton spins so that each chemically distinct carbon shows a single unsplit resonance line. As with NMR, the chemical shift of each 13C signal provides information about a carbon s chemical environment in the sample. In addition, the number of protons attached to each carbon can be determined using the DEPT-NMR technique. 

The basic components of the solid state spectrometer are the same as the solution-phase instrument data system, pulse programmer, observe and decoupler transmitters, magnetic system, and probes. In addition, high-power amplifiers are required for the two transmitters and a pneumatic spinning unit to achieve the necessary spin rates for MAS. Normally, the observe transmitter for 13C work requires broadband amplification of approximately 400 W of power for a 5.87-T, 250-MHz instrument. The amplifier should have triggering capabilities so that only the radiofrequency (rf) pulse is amplified. This will minimize noise contributions to the measured spectrum. So that the Hartmann-Hahn condition may be achieved, the decoupler amplifier must produce an rf signal at one-fourth the power level of the observe channel for carbon work. 

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