The NMR signals of isotopically or chemically dilute nuclear spins S in solids can be enhanced by repeatedly transferring polarization from a more abundant species I of high abundance (usually protons) to which they are coupled. The gain. in power sensitivity as compared with conventional observation of the rare spins approaches N/ (I + l)'Y/IN s S (S + I}'Y/, or '" 10 3 for S = 13C, 1= IH in organic solids. The transfer of polarization is accomplished by any of a number of double resonance methods. High-frequency resolution of the S-spin signal is obtained by decoupling of the abundant spins. The experimental requirements of the technique are discussed and a brief comparison of its sensitivity with other procedures is made. Representative applications and experimental results are mentioned.
The NMR free induction decay from a spinning sample having inhomogeneous anisotropic interactions (chemical shifts, first order quadrupole couplings) takes the form of a train of rotational spin echoes. The Fourier transform of the echo envelope is a sharp spectrum from which the effects of anisotropy have been removed. The Fourier transform of the echo shape contains information concerning the anisotropies: This information can be extracted by a moment analysis. The effects of localized homonuclear spin–spin interactions are to convert the ’’isotropic’’ spectrum into a characteristic powder pattern. Second order quadrupole coupling produces a similar effect. It is shown in this case that the usual second-order level shifts cannot be used to calculated this pattern, which must be described by a proper average Hamiltonian theory. Finally it is shown that rotational spin echoes provide a convenient means of studying very slow random molecular rotations (τc≲1 sec).
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