Separated quadrupole and shift interactions of 2H NMR spectra in paramagnetic solids by asymmetric pulse sequences.

ABSTRACT

Separated pure-quadrupole (PQ) and -shift (PS) spectra of 2H nuclear magnetic resonance (NMR) of paramagnetic solids are obtained and correlated by simple pulse sequences that can acquire the full magnetization under ideal conditions. Two-dimensional NMR signals obtained using an asymmetric π-pulse-inserted quadrupole-echo (APIQE) sequence yielded separated spectra through the skew operation of an affine transform (AT) before a Fourier transform. Modified APIQE sequences that acquire whole echo signals were fabricated, and separated PQ and PS spectra were obtained by applying a combination of AT, such as rotation and skew operations, to the signal data. These methods were demonstrated for diamagnetic Zn(CD3CO2)2⋅2H2O and paramagnetic Nd(CD3CO2)3⋅1.5H2O. Further, the dynamics of the D2O molecule and [Co(D2O)6]2+ ion in paramagnetic CoSiF6⋅6D2O was analyzed based on the temperature dependence of the separated spectra.