EASY-GOING deconvolution: Automated MQMAS NMR spectrum analysis based on a model with analytical crystallite excitation efficiencies

Grimminck, Dennis L.A.G.; Meerten, Bas van; Verkuijlen, M.H.W.; Eck, Ernst R. H. van; Meerts, W. Leo; Kentgens, A.P.M.

doi:10.1016/j.jmr.2012.12.012

Cited by 12 publications

(14 citation statements)

References 32 publications

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“…3QMAS NMR provides 2D spectra where the anisotropic part of the quadrupolar interaction is separated from isotropic shift contributions . Indeed, 3QMAS NMR is especially helpful for the analysis of 1D spectra of disordered materials . The disorder can be reflected in the line shapes of the 3QMAS NMR spectra, and translated into interaction parameter distributions.…”

Section: Fitted Peak Parameters and Intensities For The Solid‐state Nmentioning

confidence: 99%

“…Here, we report on the use of 27 Al 3QMAS NMR spectroscopy to differentiate between different Al species in fresh and spent Ru/H‐β (Si/Al=12.5, CP814E, Zeolyst) and Ru/H‐ZSM‐5 (Si/Al=11.5, CBV2314, Zeolyst), including the determination of the related interaction parameter distributions. The obtained data have been fitted with the Czjzek model, which quantitatively establishes the changes in the state of the various aluminum species. The insights obtained from advanced 27 Al 3QMAS NMR studies are compared with FT‐IR spectroscopy data, providing further insights into the changes in acidity (i.e., amount, nature, and location).…”

Section: Fitted Peak Parameters and Intensities For The Solid‐state Nmentioning

confidence: 99%

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Influence of Levulinic Acid Hydrogenation on Aluminum Coordination in Zeolite‐Supported Ruthenium Catalysts: A ²⁷Al 3QMAS Nuclear Magnetic Resonance Study

Luo

Eck²,

Bruijnincx

et al. 2017

ChemPhysChem

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The influence of a highly oxygenated, polar protic reaction medium, that is, levulinic acid in 2‐ethylhexanoic acid, on the dealumination of two zeolite‐supported ruthenium catalysts, namely Ru/H‐β and Ru/H‐ZSM‐5, has been investigated by 27Al triple‐quantum magic‐angle spinning nuclear magnetic resonance spectroscopy (3QMAS NMR). Upon use of these catalysts in the hydrogenation of levulinic acid, the heterogeneity in aluminum speciation is found to increase for both Ru/H‐ZSM‐5 and Ru/H‐β. For Ru/H‐ZSM‐5, the symmetric, tetrahedral framework aluminum species (FAL) were found to be mainly converted into distorted tetrahedral FAL species, with limited loss of aluminum to the solution by leaching. A severe loss of both FAL and extra‐framework aluminum (EFAL) species into the liquid phase was observed for Ru/H‐β instead. The large decrease in tetrahedral FAL species, in particular, results in a significant decrease in strong acid sites, as corroborated by Fourier transform infrared spectroscopy (FT‐IR). This decrease in acidity, evidence of the inferior stability of the strongly acidic sites in Ru/H‐β relative to Ru/H‐ZSM‐5 under the applied conditions, is considered as the main reason for differences seen in catalyst performance.

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Section: Fitted Peak Parameters and Intensities For The Solid‐state Nmentioning

confidence: 99%

Section: Fitted Peak Parameters and Intensities For The Solid‐state Nmentioning

confidence: 99%

Influence of Levulinic Acid Hydrogenation on Aluminum Coordination in Zeolite‐Supported Ruthenium Catalysts: A ²⁷Al 3QMAS Nuclear Magnetic Resonance Study

Luo

Eck²,

Bruijnincx

et al. 2017

ChemPhysChem

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“…The Czjzek distribution is implemented in several public software packages for fitting MAS NMR spectra [115,[117][118][119]. The Czjzek model was recently extended to separate the contributions from the local coordination environments and longer range effects to the effective C Qη -value [120].…”

Section: Distributions Of Chemical Shift and Quadrupolar Parameters Imentioning

confidence: 99%

“…The DMFit [115] and EGdeconv [119] softwares allow for deconvoluting 3QMAS spectra-albeit both give approximate calculations, as the spin dynamics during the rf pulses is not (fully) accounted for-thereby allowing to obtain the entire {x Al [p] , δ iso [p] , C ½p Qη , W iso [p] } parameter quartet from each 27 Al [p] coordination in AS glasses. Figure 17 displays experimental and modeled 3QMAS 27 Al NMR spectra from CaO-Al 2 O 3 -SiO 2 glasses, as reported by Massiot and coworkers [67].…”

Section: Deconvolution Of 1d Mas Nmr Spectra By Numerical Simulationsmentioning

confidence: 99%

27Al NMR Studies of Aluminosilicate Glasses

Edén

2015

Annual Reports on NMR Spectroscopy

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“…In order to describe the distributions, we fitted the MQMAS spectrum with the EGdeconv program. 74 The two tetrahedral sites could be fitted satisfactory with a Czjzek distribution; however, it proved more difficult to fit the octahedral site. The results are summarized in Table 2.…”

Section: ■ Introductionmentioning

confidence: 97%

Lithium Doping of MgAl₂O₄ and ZnAl₂O₄ Investigated by High-Resolution Solid State NMR

Blaakmeer¹,

Rosciano

Eck³

2015

J. Phys. Chem. C

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Lithium-doped spinels could function as solid state electrolytes in batteries in which all components have the spinel structure. In this study we prepared lithium-doped MgAl 2 O 4 and ZnAl 2 O 4 . Advanced solid state 7 Li, 25 Mg, and 27 Al NMR have been used to investigate the structure of these spinels and the structural changes that take place therein upon lithium doping. The spinel structure is well retained, although the amount of tetrahedral aluminum increases with increased lithium content. Using MQMAS experiments, the presence of two tetrahedral sites is discovered in both doped and undoped spinels. It is shown that the spinel structure of MgAl 2 O 4 is heterogeneous, which leads to distributions in chemical shift and quadrupolar parameters. The heterogeneity is also shown in 25 Mg spectra obtained with the quadrupolar Carr−Purcell−Meiboom−Gill (QCPMG) and sideband selective Double Frequency Sweep-QCPMG (ssDFS-QCPMG) pulse sequences. Lithium mobility is measured using static variable temperature 7 Li NMR experiments. A low fraction of mobile lithium was found (3−4%) for magnesium spinels. The lithium doped ZnAl 2 O 4 sample shows practically no mobility. This sample has significantly less disorder and less cation site inversion than the magnesium samples. ■ INTRODUCTIONLithium-ion batteries nowadays dominate the market for portable devices. For their automotive applications there are, however, significant improvements to make, which include improving safety, recyclability, and reducing mass. Solid state batteries show potential in these properties. In solid state batteries the liquid electrolyte has been replaced by a solid electrolyte. Much research has been performed in finding new solid electrolyte materials with high conductivity. The current focus is on lithium-ion materials, ranging from crystalline materials to polymers, amorphous composites, and glasses. 1,2 LiPON is an example of a solid state electrolyte that is being used for commercial applications, 3 but its performance is limited by the low ionic conductivity (ca. 10 −6 S/cm at 300 K).Research on new solid electrolytes is focused on two fields: sulfide-based and oxide-based materials. Sulfide materials such as the Li 2 S−P 2 S 5 glass-ceramics, 4 Li 10 GeP 2 S 12 and its derivatives, 5,6 or Argyrodite-type compounds 7−9 have shown excellent conductivity, up to 10 −2 S/cm at room temperature. While these materials are attractive, their preparation is complicated, as it needs to be carried out in protected atmosphere, and the resulting powders are not stable in contact with certain oxide cathode materials, requiring costly and complex coatings. 10 Oxide-type solid electrolytes have the advantage of being more easily synthesized, but their conductivity is in general lower than that of sulfides. Examples include the LATP or LAGP materials with Nasicon-type structure, 11,12 the A-site deficient perovskites such as Li 3x La (2/3)-x □ (1/3)−2x TiO 3 (LLTO), 13 or the large family of garnet-type materials. 14−16 All these compounds exhibit high con...

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EASY-GOING deconvolution: Automated MQMAS NMR spectrum analysis based on a model with analytical crystallite excitation efficiencies

Cited by 12 publications

References 32 publications

Influence of Levulinic Acid Hydrogenation on Aluminum Coordination in Zeolite‐Supported Ruthenium Catalysts: A ²⁷Al 3QMAS Nuclear Magnetic Resonance Study

Influence of Levulinic Acid Hydrogenation on Aluminum Coordination in Zeolite‐Supported Ruthenium Catalysts: A ²⁷Al 3QMAS Nuclear Magnetic Resonance Study

27Al NMR Studies of Aluminosilicate Glasses

Lithium Doping of MgAl₂O₄ and ZnAl₂O₄ Investigated by High-Resolution Solid State NMR

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EASY-GOING deconvolution: Automated MQMAS NMR spectrum analysis based on a model with analytical crystallite excitation efficiencies

Cited by 12 publications

References 32 publications

Influence of Levulinic Acid Hydrogenation on Aluminum Coordination in Zeolite‐Supported Ruthenium Catalysts: A 27Al 3QMAS Nuclear Magnetic Resonance Study

Influence of Levulinic Acid Hydrogenation on Aluminum Coordination in Zeolite‐Supported Ruthenium Catalysts: A 27Al 3QMAS Nuclear Magnetic Resonance Study

27Al NMR Studies of Aluminosilicate Glasses

Lithium Doping of MgAl2O4 and ZnAl2O4 Investigated by High-Resolution Solid State NMR

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Influence of Levulinic Acid Hydrogenation on Aluminum Coordination in Zeolite‐Supported Ruthenium Catalysts: A ²⁷Al 3QMAS Nuclear Magnetic Resonance Study

Influence of Levulinic Acid Hydrogenation on Aluminum Coordination in Zeolite‐Supported Ruthenium Catalysts: A ²⁷Al 3QMAS Nuclear Magnetic Resonance Study

Lithium Doping of MgAl₂O₄ and ZnAl₂O₄ Investigated by High-Resolution Solid State NMR