Magn Reson Chem
September 2021
Through-space heteronuclear correlation (D-HETCOR) experiments based on heteronuclear multiple-quantum correlation (D-HMQC) and refocused insensitive nuclei enhanced by polarization transfer (D-RINEPT) sequences have been proven to be useful approaches for the detection of the spatial proximity between half-integer quadrupolar nuclei in solids under magic-angle spinning (MAS) conditions. The corresponding pulse sequences employ coherence transfers mediated by heteronuclear dipolar interactions, which are reintroduced under MAS by radiofrequency irradiation of only one of the two correlated nuclei. We investigate herein using numerical simulations of spin dynamics and solid-state NMR experiments on magnesium aluminoborate glass how the choice of the channel to which the heteronuclear dipolar recoupling is applied affects the transfer efficiency of D-HMQC and D-RINEPT sequences between B and Al nuclei.
View Article and Find Full Text PDFChem Commun (Camb)
January 2021
A large amount of polymeric vanadyl species owing to higher interaction energy between vanadia and anatase than rutile and the synergistic effect of vanadium oxides, anatase and rutile TiO2 contributes to an excellent NH3-SCR activity of the vanadia-based catalysts with high rutile content and low specific surface area.
View Article and Find Full Text PDFThe unambiguous characterization of different acid sites in zeolites is of great importance for understanding their catalytic performance and the rational design of highly efficient zeolite catalysts. In addition to various well-characterized extra-framework Al species, a tri-coordinated framework aluminum species can also serve as a Lewis acid site in zeolites, which is "NMR-invisible" owing to its extremely distorted local environment. Here we provide a feasible and reliable approach to elucidate the acidic nature of the tri-coordinated framework Al in dehydrated H-ZSM-5 zeolites sensitivity-enhanced two-dimensional (2D) multiple nuclear correlation NMR experiments coupled with trimethylphosphine oxide (TMPO) probe molecules.
View Article and Find Full Text PDFAg/γ-AlO is widely used for catalyzing various reactions, and its performance depends on the valence state, morphology and dispersion of Ag species. However, detailed anchoring mechanism of Ag species on γ-AlO remains largely unknown. Herein, we reveal that the terminal hydroxyls on γ-AlO are responsible for anchoring Ag species.
View Article and Find Full Text PDFWe introduce two MAS schemes that allow manipulating the satellite-transition (ST) populations of half-integer quadrupolar nuclei, and which both exhibit improved robustness to the quadrupolar coupling constant (C). These schemes, called quadruple frequency sweep (QFS) or quadruple WURST (QWURST) are the sums of two DFS or four WURST to efficiently invert the ST populations of nuclei subject to large or small quadrupole interactions, simultaneously. These quadruple sweeps methods only require 6% more rf-power than the double sweeps ones.
View Article and Find Full Text PDFSolid State Nucl Magn Reson
September 2018
We demonstrated that the heteronuclear correlation experiments between two quadrupolar nuclei, Na and Al, with close Larmor frequencies can be achieved via D-HMQC and D-RINEPT approaches by using a diplexer connected to a conventional probe in magic-angle-spinning solid-state NMR. Low-power heteronuclear dipolar recoupling schemes can be applied on Na or Al to establish polarization transfers between the central transitions of Na and Al for a model compound, NaAlO. Further, we showed a practical implementation of the two dimensional Na-Al dipolar-based heteronuclear correlation experiment on a heterogeneous catalyst, NaCO/γ-AlO.
View Article and Find Full Text PDFCrystallization of AlPO4-5 with AFI structure under solvent-free conditions has been investigated. Attention was mainly focused on the characterization of the intermediate phases formed at the early stages during the crystallization. The development in the long-range ordering of the solid phases as a function of crystallization time was monitored by XRD, SEM, IR, UV-Raman, and MAS NMR techniques.
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