Nuclear magnetic resonance spectroscopy

Goodman, B. A.; Chudek, J. A.

doi:10.1007/978-94-011-0727-3_4

Cited by 5 publications

(4 citation statements)

References 47 publications

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“…In this study, the resonant peak of IV Al split into two distinct components at higher magnetic field, as in another publication (Goodman and Chudek, 1994). For WC illite after acid treatment, the ratio of the integral values between IV Al and VI Al signals, decreased from 0.73 to 0.58 compared to that of the hydrated sample.…”

Section: @86supporting

confidence: 75%

Modeling description and spectroscopic evidence of surface acid–base properties of natural illites

Liu

2001

Water Research

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Section: @86supporting

confidence: 75%

Modeling description and spectroscopic evidence of surface acid–base properties of natural illites

Liu

2001

Water Research

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“…They have also been applied to clay studies concerning microstructure, adsorption of organics, fractal dimensions, metal loading, and aggregation . Solid-state NMR techniques have been widely applied to aspects of clay chemistry such as lattice structure ( 29 Si, 27 Al), interlayer cations ( 23 Na, 113 Cd, 133 Cs), and organic adsorption ( 1 H, 13 C, 31 P) .…”

Section: Introductionmentioning

confidence: 99%

Crystallization of a Layered Silicate Clay as Monitored by Small-Angle X-ray Scattering and NMR

Carrado

Gregory

et al. 2000

Chem. Mater.

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The 48-h hydrothermal crystallization of a magnesium silicate clay called hectorite has been investigated in detail. Tetraethylammonium (TEA) ions are used to aid crystallization and become incorporated as the exchange cations within the interlayers. Data from smallangle X-ray scattering (SAXS) using aliquots ex situ are consistent with results obtained previously by X-ray powder diffraction (XRD), thermal gravimetric analysis (TGA), atomic force microscopy (AFM), and IR. All these techniques see clay crystallites beginning to form within the first few hours of reaction. 29 Si NMR displays a visible clay silicate peak after just 1 h. Solid-state 13 C NMR shows evidence of TEA-clay formation in as little as 30 min and also that 80% of the final TEA loading is accomplished in the first 10-12 h. Up to 36 h more is needed to incorporate the remaining 20% of TEA, indicating that a slower event is dominating at the later stages of crystallization. Data from 13 C NMR and SAXS are compared to and are consistent with data from earlier AFM experiments. All present a scenario where initial nucleation and crystallization end after about 14 h, after which this occurs to a lesser extent and primarily agglomeration of particles is taking place. The SAXS data show this in progressively increasing power law values, indicating more "open" structures that condense into more dense structures with time. In addition, the first in situ study of clay crystallization of any kind was performed by in situ SAXS. A possible clay crystallization mechanism is proposed.

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“…Solid state NMR techniques have been used for in situ spectroscopic investigations of adsorption processes ( , ) and heterogenous catalytic processes ( , ) and for surface characterization of catalysts and various organic and inorganic adsorbents ( , ). The application of NMR in soil science and geochemistry has been limited to structural characterization of minerals, soil organic matter, and whole soils () and to studies of water structure on clay surfaces and interlamellar regions ( , ).…”

Section: Introductionmentioning

confidence: 99%

Solid State ¹⁵N NMR Study of Pyridine Adsorption on Clay Minerals

Ukrainczyk

Smith

1996

Environ. Sci. Technol.

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A solid state nuclear magnetic resonance (NMR) method is presented for spectroscopic adsorption studies of organic pollutant compounds on surfaces of powders under environmentally relevant hydration conditions. The applicability of the solid state NMR spectroscopy was investigated using pyridine as a model adsorbate and a clay mineral, hectorite, as an adsorbent. Solid state 15N magic angle spinning (MAS) and cross-polarization (CP)/MAS NMR methods were used to study adsorption of [15N]pyridine on fully hydrated and on dehydrated homoionic K-, Ca-, Mg-, and Al-hectorites. Powder X-ray diffraction (XRD) was used to determine the expansion of basal spacings and to confirm intercalation of pyridine into clay interlayers. With the exception of hydrated Al-hectorite, more intense signals were obtained with MAS than with CP/MAS, and cross-polarization was less efficient on dehydrated clay/pyridine samples than on hydrated ones, indicative of a higher mobility of pyridine in the interlayers of dehydrated clays compared to hydrated ones. Pyridine interacted primarily through hydrogen bonding to the interlayer water on the hydrated hectorites. On the dehydrated K-hectorite (d 001 = 10.7 Å before pyridine adsorption), pyridine solvated the interlayers. Dehydrated Ca- and Mg-hectorites (d 001 = 12.9 and 12.8 Å, respectively, before pyridine adsorption) retained one layer of hydration water to which pyridine hydrogen bonds. Intercalation of pyridine was facilitated by the presence of water, the extreme case being Al-hectorite where almost no intercalation was observed without water. Spinning sidebands were only observed for the pyridine resonance between −90 and −94 ppm. This anisotropic species is assigned to the pyridine keying into the ditrigonal hole, hydrogen bonded to the proton of structural OH. The results clearly show that 15N NMR of an adsorbed N-containing organic compound is a powerful tool for identifying and distinguishing various surface complexes and adducts on hydrated mineral surfaces.

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Nuclear magnetic resonance spectroscopy

Cited by 5 publications

References 47 publications

Modeling description and spectroscopic evidence of surface acid–base properties of natural illites

Modeling description and spectroscopic evidence of surface acid–base properties of natural illites

Crystallization of a Layered Silicate Clay as Monitored by Small-Angle X-ray Scattering and NMR

Solid State ¹⁵N NMR Study of Pyridine Adsorption on Clay Minerals

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Nuclear magnetic resonance spectroscopy

Cited by 5 publications

References 47 publications

Modeling description and spectroscopic evidence of surface acid–base properties of natural illites

Modeling description and spectroscopic evidence of surface acid–base properties of natural illites

Crystallization of a Layered Silicate Clay as Monitored by Small-Angle X-ray Scattering and NMR

Solid State 15N NMR Study of Pyridine Adsorption on Clay Minerals

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Solid State ¹⁵N NMR Study of Pyridine Adsorption on Clay Minerals