Solid-state 33S MAS NMR of inorganic sulfates

Wagler, Todd A.; Daunch, William A.; Panzner, Matthew J.; Youngs, Wiley J.; Rinaldi, Peter L.

doi:10.1016/j.jmr.2004.07.011

Cited by 30 publications

(53 citation statements)

References 40 publications

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“…The more recent study 9 gives C Q ) 0.97 MHz and η Q ) 0.50. The 33 S isotropic shift in K 2 SO 4 was reported at 334 ( 3 ppm 5 and 336 ppm.…”

Section: Resultsmentioning

confidence: 90%

“…9 Considering that the first value was obtained from a stationary spectrum, 5 and the second value has been obtained from MAS spectrum at a substantially higher magnetic field, 9 the later is likely to be more accurate. The results of a recent study 14 confirm the data of ref 9. A peak position in 33 S MAS spectrum for K 2 SO 4 has been also reported in ref 10, but it does not state if a correction for the second order quadrupolar shift has been made.…”

Section: Resultsmentioning

confidence: 99%

“…Most likely, the anisotropy was not detected previously because the spectra in ref 5 were obtained only for a stationary sample at one magnetic field with significantly lower signal-to-noise ratio. In a later study, 9 on another hand, no measurements of stationary samples were made, and the anisotropy was averaged by the MAS.…”

Section: Resultsmentioning

confidence: 99%

“…The technique, however, has seen very few applications, with just over 10 publications on the subject being produced in the past 25 years. [5][6][7][8][9][10][11][12][13][14][15][16] The problem arises mainly from the great difficulty in obtaining the spectra. The only magnetically active isotope, 33 S, has a low natural abundance of 0.75%, and is a spin 3/2 quadrupolar nucleus with rather small magnetogyric ratio γ (absolute resonance frequency Θ ) 7.676 MHz).…”

Section: Introductionmentioning

confidence: 99%

“…An additional complication commonly encountered in SS NMR of low-γ nuclei is rather long relaxation times. In a case of 33 S, T 1 values as long as tens of seconds can be expected, 8,9 seriously hindering signal averaging. One should note that previously published 33 S SS NMR data deal mainly with situations of rather small quadrupolar interactions.…”

Section: Introductionmentioning

confidence: 99%

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High Field ³³S Solid State NMR and First-Principles Calculations in Potassium Sulfates

et al. 2009

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Vous avez des questions? Nous pouvons vous aider. Pour communiquer directement avec un auteur, consultez la première page de la revue dans laquelle son article a été publié afin de trouver ses coordonnées. Si vous n'arrivez pas à les repérer, communiquez avec nous à PublicationsArchive-ArchivesPublications@nrc-cnrc.gc.ca. Questions? Contact the NRC Publications Archive team atPublicationsArchive-ArchivesPublications@nrc-cnrc.gc.ca. If you wish to email the authors directly, please see the first page of the publication for their contact information. NRC Publications Archive Archives des publications du CNRCThis publication could be one of several versions: author's original, accepted manuscript or the publisher's version. / La version de cette publication peut être l'une des suivantes : la version prépublication de l'auteur, la version acceptée du manuscrit ou la version de l'éditeur. NRC Publications Record / Notice d'Archives des publications de CNRC:http://nparc.cisti-icist.nrc-cnrc.gc.ca/eng/view/object/?id=0b178185-620e-4262-8966-6e518a9bdcdf http://nparc.cisti-icist.nrc-cnrc.gc.ca/fra/voir/objet/?id=0b178185-620e-4262-8966-6e518a9bdcdf High Field S Solid State NMR and First-Principles Calculations in Potassium SulfatesIgor Moudrakovski,* Stephen Lang, Serguei Patchkovskii, and John Ripmeester Steacie Institute for Molecular Sciences, National Research Council, 100 Sussex DriVe, Ottawa, K1A 0R6, Ontario, Canada ReceiVed: August 25, 2009; ReVised Manuscript ReceiVed: October 16, 2009 A set of potassium sulfates presenting a variety of sulfur environments (K 2 SO 4 , KHSO 4 ,K 2 S 2 O 7 , and K 2 S 2 O 8 ) has been studied by 33 S solid state NMR at 21 T. Low natural abundance (0.75%) and small gyromagnetic ratio of 33 S presented a serious challenge even at such a high magnetic field. Nevertheless, using the QCPMG technique we were able to obtain good signals from the sites with C Q values approaching 16 MHz. Assignment of the sites and the relative orientations of the EFG tensors were assisted by quantum mechanical calculations using the Gaussian 98 and CASTEP packages. The Gaussian 98 calculations were performed using the density functional method and gauge independent atomic orbitals on molecular clusters of about 100-120 atoms. The CASTEP calculations utilized periodic boundary conditions and a gauge-including projector augmentedwave pseudopotential approach. Although only semiquantitative agreement is observed between the experimental and calculated parameters, the calculations are a very useful aid in the interpretation of experimental data.

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“…The more recent study 9 gives C Q ) 0.97 MHz and η Q ) 0.50. The 33 S isotropic shift in K 2 SO 4 was reported at 334 ( 3 ppm 5 and 336 ppm.…”

Section: Resultsmentioning

confidence: 90%

Section: Resultsmentioning

confidence: 99%

Section: Resultsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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High Field ³³S Solid State NMR and First-Principles Calculations in Potassium Sulfates

et al. 2009

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New Approaches to the Characterization of Drug Candidates by Solid‐StateNMR

Vogt

Clawson

Strohmeier

et al. 2011

Pharmaceutical Sciences Encyclopedia

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Solid‐state NMR (SSNMR) spectroscopy has been found to be very useful technique for pharmaceutical development. This technique is currently applied for the study of pharmaceutical solids, ranging from detailed structural studies of active pharmaceutical ingredients (APIs) forms to analysis of complex drug products and formulations. The study suggests that solid‐state structure of a pharmaceutical product can influence its properties, manufacturability, and stability. It is essential to regulate and control over solid‐state structure and subsequent properties. The studies show that SSNMR is closely related to the widely used technique of solution‐state NMR and possesses many of the same features. Further the study concludes that field of pharmaceutical SSNMR continues to advance at a rapid rate and will develop new molecular classes and new formulations and delivery modes in near future.

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Toward recording ³³S NMR spectra of cross‐linked elastomers: Relaxation dynamics perspective

Marhabaie

Tékély

2016

Concepts Magnetic Resonance

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We discuss from the perspective of relaxation dynamics the feasibility of recording NMR spectra of 33S nuclei bound to cross‐link junctions in cross‐linked elastomers (i.e. vulcanized rubber). Assuming the quadrupolar relaxation mechanism due to fluctuating electric field gradients, the calculations of transverse and longitudinal 33S relaxation times encompassing a large range of correlation times, static magnetic fields, and quadrupolar coupling constants reveal that both relaxation processes will constitute significant bottlenecks in recording the 33S spectra of cross‐linked elastomers inherently endowed with a large distribution of motional modes. In the rubbery state, the observable 33S NMR signal will result from motionally averaged, central transition magnetization of the 33S nuclei in cross‐link junctions involved in large amplitude, high‐frequency motions.

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Solid-state 33S MAS NMR of inorganic sulfates

Cited by 30 publications

References 40 publications

High Field ³³S Solid State NMR and First-Principles Calculations in Potassium Sulfates

High Field ³³S Solid State NMR and First-Principles Calculations in Potassium Sulfates

New Approaches to the Characterization of Drug Candidates by Solid‐StateNMR

Toward recording ³³S NMR spectra of cross‐linked elastomers: Relaxation dynamics perspective

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Solid-state 33S MAS NMR of inorganic sulfates

Cited by 30 publications

References 40 publications

High Field 33S Solid State NMR and First-Principles Calculations in Potassium Sulfates

High Field 33S Solid State NMR and First-Principles Calculations in Potassium Sulfates

New Approaches to the Characterization of Drug Candidates by Solid‐StateNMR

Toward recording 33S NMR spectra of cross‐linked elastomers: Relaxation dynamics perspective

Contact Info

Product

Resources

About

High Field ³³S Solid State NMR and First-Principles Calculations in Potassium Sulfates

High Field ³³S Solid State NMR and First-Principles Calculations in Potassium Sulfates

Toward recording ³³S NMR spectra of cross‐linked elastomers: Relaxation dynamics perspective