Biomedical subjects
Publications and source records attributed to A Samoson.
A field and method independent canonical representation of high-resolution spectra of quadrupole nuclei enables universal analyses of experimental data. The best accuracy from 1D measurements is achieved if DOR and MQ-MAS methods are combined.
Two-dimensional triple-quantum (2D-3Q) 23Na MAS NMR spectroscopy has been applied for the investigation of sodium cations in dehydrated zeolites NaY, NaEMT, NaZSM-5 and NaMOR. The experiments have shown that the new 2D-3Q technique allows the determination of the isotropic chemical shifts and quadrupolar couplings of sodium cations with SOQE (second-order quadrupolar effect) parameters of up to ca. 4 MHz. In the present work, SOQE parameters of 1.0-1.2 MHz were found for sodium cations located at positions SI in the hexagonal prisms of dehydrated zeolites NaY and NaEMT. The sodium cations located in the 10-ring and 12-ring channels of dehydrated zeolites NaZSM-5 and NaMOR, respectively, are characterized by a SOQE parameter of 2.0 MHz while a value of 3.1 MHz was determined for sodium cations in the sidepockets of the channels in dehydrated NaMOR.
A generalized description of sideband suppression with inversion pulses is presented. As an example of optimization, a sequence with three inversion pulses is demonstrated.
The 27Al NMR spectra of calcium tungstate aluminate sodalite (CAW), Ca8[Al12O24](WO4)2, and the 23Na NMR spectra of sodium aluminosilicate sodalites of general composition Na9[Si6Al6O24]A2 with A = B(OH)4- (SBS), SCN- (SRS) and A2 = SO4(2-) (SSS), MoO4(2-) (SMS) have been measured using magic-angle spinning (MAS) and double-rotation (DOR) techniques. Rotor synchronized pulse excitation is applied in the DOR experiments. Dramatic line narrowing is observed in the DOR spectra of all samples. The 27Al DOR NMR spectra of CAW measured at 9.4 and 11.7 T and spinning rates of 800-1150 Hz of the outer and 5 kHz of the inner rotor show seven sharp central lines accompanied by a manifold of spinning sidebands. These lines correspond to the seven crystallographically inequivalent Al sites of the CAW framework derived from X-ray structure analysis. From the difference of the line positions in the 9.4 and 11.7 T spectra the quadrupole coupling constant, QCC, quadrupole induced shift, sigma qs, and isotropic chemical shift, delta cs, of each Al site have been calculated. QCC values in the range of 5 to 9 MHz are obtained which reflect the strong tetragonal distortion of the AlO4 tetrahedra in CAW. delta cs shows only small changes in the range between 74.4 and 77.2 ppm. A tentative assignment of all lines to the distinct Al sites is derived from the correlation between QCC and a "shear strain parameter" describing quantitatively the distortion of the AlO4 tetrahedra.(ABSTRACT TRUNCATED AT 250 WORDS)
A theory of dynamic angle spinning (DAS) and double rotation (DOR) NMR is described using average Hamiltonian and irreducible tensor methods. Sideband intensities in DAS and DOR spectra are analyzed by both the moment and Bessel function methods, and general formulae are derived. Results show that the DAS moments depend on the relative rotor phase between the first and the second evolution periods, whereas the second and third DOR moments are independent of the relative phase between the inner and outer rotors. Sideband intensities in DAS spectra also depend on the relative rotor phases between evolution at the first and second angles, as well as on the ratio of time spent at each angle. Sideband intensities and phases in DOR spectra are related to the relative rotor phases between the inner and outer rotors, and the sideband pattern is determined by the ratio of the inner and outer rotor spinning speeds. An inversion symmetry of the odd numbered DOR sidebands at the relative rotor phase gamma r = 0 degree, 180 degrees permits the elimination of these sidebands. Finally, numerical simulations are implemented and shown to agree with experimental results. Quadrupolar parameters can therefore be recovered either by calculating the second and third moments or by simulating the sideband intensities and phases.