Simple and efficient decoupling in magic-angle spinning solid-state NMR: the XiX scheme

Detken, Andreas; Hardy, Edme H.; Ernst, Matthias; Meier, Beat H.

doi:10.1016/s0009-2614(02)00335-4

Cited by 238 publications

(219 citation statements)

References 12 publications

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“…The experiments on dry CNC-1 were performed at a sample spinning frequency of 17 kHz utilizing a Varian 3.2 mm double-resonance probehead, whereas the experiments on the never-dried CNCS-1 and rehydrated CNC-1R1 and CNC-1R2 samples were done at MAS frequency of 4 kHz using a Varian 4 mm double-resonance probehead. Single contact ramped CP 19 experiments with a contact time of 0.8 ms were performed using proton decoupling with the help of the XiX sequence 20,21 during the detection of the 13 C NMR signal. We confirmed that the RAMP-CP spectra were quantitative by comparing them to multiple contact RAMP-CP experiments.…”

Section: ■ Experimental Sectionmentioning

confidence: 99%

Correlating Cellulose Nanocrystal Particle Size and Surface Area

Brinkmann¹,

Chen²,

Couillard³

et al. 2016

Langmuir

141

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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. For the publisher's version, please access the DOI link below./ Pour consulter la version de l'éditeur, utilisez le lien DOI ci-dessous.http://doi.org/10.1021/acs.langmuir.6b01376Access and use of this website and the material on it are subject to the Terms and Conditions set forth at Correlating cellulose nanocrystal particle size and surface area Brinkmann, Andreas; Chen, Maohui; Couillard, Martin; Jakubek, Zygmunt J.; Leng, Tianyang; Johnston, Linda J.http://nparc.cisti-icist.nrc-cnrc.gc.ca/fra/droits L'accès à ce site Web et l'utilisation de son contenu sont assujettis aux conditions présentées dans le site LISEZ CES CONDITIONS ATTENTIVEMENT AVANT D'UTILISER CE SITE WEB. NRC Publications Record / Notice d'Archives des publications de CNRC:http://nparc.cisti-icist.nrc-cnrc.gc.ca/eng/view/object/?id=df1fceea-c08d-4b99-8897-d9370e2db3c7 http://nparc.cisti-icist.nrc-cnrc.gc.ca/fra/voir/objet/?id=df1fceea-c08d-4b99-8897-d9370e2db3c7Correlating Cellulose Nanocrystal Particle Size and Surface Area ABSTRACT: Cellulose nanocrystals (CNCs) are negatively charged nanorods that present challenges for characterization of particle size distribution and surface areatwo of the common parameters for characterizing nanomaterials. CNC size distributions have been measured by two microscopy methods: atomic force microscopy (AFM) and transmission electron microscopy (TEM). The agreement between the two methods is good for length measurements, after taking into consideration tip-convolution effects for AFM. However, TEM widths are almost twice as large as AFM heightsan effect that we hypothesize is due to counting of a larger fraction of laterally associated CNCs in the TEM images. Overall, the difficulty of selecting individual particles for analysis and possible bias due to selection of a specific particle size during sample deposition are the main limitations associated with the microscopy measurements. The microscopy results were compared to Zaverage data from dynamic light scattering, which is a useful method for routine analysis and for examining trends in size as a function of sample treatment. Measurements as a function of sonication energy...

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Section: ■ Experimental Sectionmentioning

confidence: 99%

Correlating Cellulose Nanocrystal Particle Size and Surface Area

Brinkmann¹,

Chen²,

Couillard³

et al. 2016

Langmuir

141

View full text Add to dashboard Cite

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“…An adiabatic passage was used with a tangential shape on the proton channel with Δrf = 40 kHz and a contact time of 500 μs (Hediger et al 1995;Ernst and Meier 2010). During the acquisition, XiX proton decoupling was applied at a field strength of 100 kHz (Tekely et al 1994;Detken et al 2002). The 13 C homonuclear correlation experiments used the DREAM sequence (Verel et al 2001) with Δrf = 16 kHz.…”

Section: Spectroscopymentioning

confidence: 99%

Line-Broadening in Low-Temperature Solid-State NMR Spectra of Fibrils

et al. 2017

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Abstract:The temperature-dependent resonance-line broadening of in its amyloid form is investigated in the range between 110 K and 280 K. Significant differences are observed between residues in the structured hydrophobic triangular core, which are broadened the least and can be detected down to 100 K, and in the solvent-exposed parts, which are broadened the most and often disappear from the observed spectrum around 200 K. Below the freezing of the bulk water, around 273 K, the protein fibrils are still surrounded by a layer of mobile water whose thickness decreases with temperature, leading to drying out of the fibrils.

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“…Different efficient decoupling sequences 76,77 were applied to improve resolution, but they showed no improvement. Also higher spinning frequencies (>25 kHz) with or without decoupling did show no improvement as for instance observed for copper containing samples.…”

Section: Heteronuclear Mofsmentioning

confidence: 99%