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Improving the sensitivity of J
coupling measurements in solids with application to disordered materials
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39. Anti-phase single-quantum coherences are not directly detected as they do not induce a voltage in the NMR coil (Tr[I−AxBz] = 0), but during the t2 acquisition period, they evolve into sine-modulated in-phase magnetization (anti-phase NMR signal) under the scalar coupling.
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It has been shown previously that for magic angle spinning (MAS) solid state NMR the refocused INADEQUATE spin-echo (REINE) experiment can usefully quantify scalar (J) couplings in disordered solids. This paper focuses on the two z filter components in the original REINE pulse sequence, and investigates by means of a product operator analysis and fits to density matrix simulations the effects that their removal has on the sensitivity of the experiment and on the accuracy of the extracted J couplings. The first z filter proves unnecessary in all the cases investigated here and removing it increases the sensitivity of the experiment by a factor ∼1.1–2.0. Furthermore, for systems with broad isotropic chemical shift distributions (namely whose full widths at half maximum are greater than 30 times the mean J coupling strength), the second z filter can also be removed, thus allowing whole-echo acquisition and providing an additional √2 gain in sensitivity. Considering both random and systematic errors in the values obtained, J couplings determined by fitting the intensity modulations of REINE experiments carry an uncertainty of 0.2–1.0 Hz (∼1−10 %).
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