Modelling one‐ and two‐dimensional solid‐state NMR spectra

Massiot, Dominique; Fayon, Franck; Capron, Mickäel; King, Ian J.; Calvé, Stéphanie Le; Alonso, Bruno; Durand, Jean‐Olivier; Bujoli, Bruno; Gan, Zhehong; Hoatson, Gina L.

doi:10.1002/mrc.984

Cited by 3,824 publications

(3,798 citation statements)

References 21 publications

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“…All curve fittings were performed using the Dmfit software. 58 The 27 Al NMR spectra were obtained using p/12 pulses, 1000 scans and a recycling delay of 0.5 s at a rf-field of 94 kHz. The 31 P spectra were obtained using a pulse length of 1.8 ms, 64 scans and with a recycle delay of 60 s. The chemical shifts of 27 Al, and 31 P were externally referenced to 1 M Al(NO 3 ) 3(aq) , and 85% H 3 PO 4(aq) , respectively.…”

Section: Sample Preparationmentioning

confidence: 99%

Local silico-aluminophosphate interfaces within phosphated H-ZSM-5 zeolites

Bij

Weckhuysen

2014

Phys. Chem. Chem. Phys.

127

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In order to elucidate phosphorus-zeolite H-ZSM-5 interactions, a variety of phosphorus-modified zeolite H-ZSM-5 materials were studied in a multi-spectroscopic manner. By deploying single pulse 27 Al, 31 P MAS NMR, 2D heteronuclear 27 Al-31 P correlation (HETCOR), 27 Al MQ MAS NMR spectroscopy, TPD of pyridine monitored by FT-IR spectroscopy, and Scanning Transmission X-ray Microscopy (STXM) the interplay and influence of acidity, thermal treatment and phosphorus on the structure and acidity of H-ZSM-5 were established. It was found that while acid treatment did not affect the zeolite structure, thermal treatment leads to the breaking of Si-OH-Al bonds, a decrease in the strong acid site number and the formation of terminal Al-OH groups. No extra-framework aluminium species was observed. Phosphorus precursors interact with the zeolitic framework through hydrogen bonds and physical coordination, as phosphorus species can be simply washed out with hot water. After phosphatation and thermal treatment two effects occur simultaneously, namely (i) phosphorus species transform into water insoluble condensed poly-phosphoric acid and (ii) phosphoric acid binds irreversibly to the terminal Al-OH groups of partially dislodged four-coordinated framework aluminium, forming local silico-aluminophosphate interfaces.These interfaces are potentially the promoters of hydrothermal stability in phosphated zeolite H-ZSM-5.

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Section: Sample Preparationmentioning

confidence: 99%

Local silico-aluminophosphate interfaces within phosphated H-ZSM-5 zeolites

Bij

Weckhuysen

2014

Phys. Chem. Chem. Phys.

127

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“…Temperatures were calibrated using the 207 Pb resonance of lead nitrate as previously described [20,21]. Deconvolution of the spectra was done using the DMfit software [22]. A 1 M LiCl solution and tetramethyl silane (TMS) were used as references for 6/7 Li and 29 Si, respectively.…”

Section: Solid State Nmrmentioning

confidence: 99%

Structural and dynamic characterization of Li12Si7 and Li12Ge7 using solid state NMR

Dupke

Langer

Pöttgen

et al. 2012

Solid State Nuclear Magnetic Resonance

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“…QuadFit is tailored towards fitting of NMR spectra from amorphous materials, but is also equally applicable to spectra from crystalline materials (http://go.warwick.ac.uk/quadfit). DMFit is a program written by Massiot [41] which has basic processing capabilities and extensive fitting abilities for both 1D and 2D data. SIMPSON [42] has been developed to produce very accurate simulations of NMR spectra given a set of spins, their interactions and a pulse sequence using density matrix theory.…”

Section: Lineshape Analysis and Simulation Of Experimentsmentioning

confidence: 99%

Recent technique developments and applications of solid state NMR in characterising inorganic materials

Hanna

Smith

2010

Solid State Nuclear Magnetic Resonance

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A broad overview is given of some key recent developments in solid state NMR techniques that have driven enhanced applications to inorganic materials science. Reference is made to advances in hardware, pulse sequences and associated computational methods (e.g. first principles calculations, spectral simulation), along with their combination to provide more information about solid phases. The resulting methodology has allowed more nuclei to be observed and more structural information to be extracted. Cross referencing between experimental parameters and their calculation from the structure has seen an added dimension to NMR as a characterisation probe of materials. Emphasis is placed on the progress made in the last decade especially from those nuclei that were little studied previously. The general points about technique development and the increased range of nuclei observed are illustrated through a range of specific exemplars from inorganic materials science.

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Modelling one‐ and two‐dimensional solid‐state NMR spectra

Cited by 3,824 publications

References 21 publications

Local silico-aluminophosphate interfaces within phosphated H-ZSM-5 zeolites

Local silico-aluminophosphate interfaces within phosphated H-ZSM-5 zeolites

Structural and dynamic characterization of Li12Si7 and Li12Ge7 using solid state NMR

Recent technique developments and applications of solid state NMR in characterising inorganic materials

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