We report a simple design strategy for wideband uniform-rate smooth truncation (WURST) pulses that enables ultrafast frequency sweeps to maximize the sensitivity of Carr-Purcell-Meiboom-Gill (CPMG) acquisition in static wideline nuclear magnetic resonance (NMR). Three compelling examples showcase the advantage of ultrafast frequency sweeps over currently employed WURST-CPMG protocols, demonstrating the potential of investigating materials that are typically inaccessible to static wideline NMR techniques, e.g., paramagnetic solids with short homogeneous transverse relaxation times.
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http://dx.doi.org/10.1021/acs.jpclett.3c02758 | DOI Listing |
J Phys Chem C Nanomater Interfaces
February 2023
Department of Chemistry, Texas A&M University, College Station, Texas 77845-3012, United States.
Ferrocene and nickelocene do not react with each other in solution; however, the large impact of the paramagnetic component on the ferrocene H NMR signal linewidth and relaxation times has been quantified. Co-crystallization of ferrocene and nickelocene at any ratio from a solvent can be explained with both pure substances crystallizing in the same space group 2/. As a new phenomenon, when a ferrocene single crystal is exposed to polycrystalline nickelocene in the absence of a solvent, the nickelocene migrates into the ferrocene crystal lattice and a mixed crystal is formed that retains its macroscopic shape.
View Article and Find Full Text PDFJ Phys Chem Lett
December 2023
Institute for Physical Chemistry, University of Münster, Corrensstrasse 28/30, DE-48149 Münster, Germany.
We report a simple design strategy for wideband uniform-rate smooth truncation (WURST) pulses that enables ultrafast frequency sweeps to maximize the sensitivity of Carr-Purcell-Meiboom-Gill (CPMG) acquisition in static wideline nuclear magnetic resonance (NMR). Three compelling examples showcase the advantage of ultrafast frequency sweeps over currently employed WURST-CPMG protocols, demonstrating the potential of investigating materials that are typically inaccessible to static wideline NMR techniques, e.g.
View Article and Find Full Text PDFJ Phys Chem A
November 2023
Department of Chemistry & Biochemistry, Florida State University, Tallahassee, Florida 32306, United States.
Cross-polarization (CP) is a technique commonly used for the signal enhancement of NMR spectra; however, applications to quadrupolar nuclei have heretofore been limited due to a number of problems, including poor spin-locking efficiency, inconvenient relaxation times, and reduced CP efficiencies over broad spectral bandwidths─this is unfortunate, since they constitute 73% of NMR-active nuclei in the periodic table. The Broadband Adiabatic Inversion CP (BRAIN-CP) pulse sequence has proven useful for the signal enhancement of wideline and ultra-wideline (i.e.
View Article and Find Full Text PDFSolid State Nucl Magn Reson
June 2023
Department of Chemical and Biological Physics, Weizmann Institute of Science, Rehovot, 7610001, Israel. Electronic address:
Static satellite-transitions (ST) NMR line shapes from half-integer quadrupolar nuclei could be very informative: they can deliver insight about local motions over a wide range of timescales, and can report on small changes in the local electronic environments as reflected by variations in the quadrupolar parameters. Satellite transitions, however, are typically "invisible" for half-integer quadrupolar nuclei due to their sheer breadth, leading to low signal-to-noise ratio -especially for unreceptive low-gamma or dilute quadrupolar nuclei. Very recently we have introduced a method for enhancing the NMR sensitivity of unreceptive X nuclei in static solids dubbed PROgressive Saturation of the Proton Reservoir (PROSPR), which opens the possibility of magnifying the signals from such spins by repeatedly imprinting frequency-selective X-driven depolarizations on the much more sensitive H NMR signal.
View Article and Find Full Text PDFPhys Chem Chem Phys
September 2022
Department of Chemistry and Biochemistry, Florida State University, Tallahassee, FL 32306, USA.
There are currently no methods for the acquisition of ultra-wideline (UW) solid-state NMR spectra under static conditions that enable reliable separation and resolution of overlapping powder patterns arising from magnetically distinct nuclei. This stands in contrast to the variety of techniques available for spin-1/2 or half-integer quadrupolar nuclei with narrow central transition patterns under magic-angle spinning (MAS). Resolution of overlapping signals is routinely achieved in MRI and solution-state NMR by exploiting relaxation differences between nonequivalent sites.
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