Multinuclear solid-state MAS and CP-MAS NMR study of the binding of triethyl phosphate to a montmorillonite

O’Brien, Paul A.; Williamson, Colin J.; Groombridge, Christopher J.

doi:10.1021/cm00014a014

Cited by 8 publications

(28 citation statements)

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“…Pratum ( 14) used 13 C NMR to study tetramethylammonium-and hexadecyltrimethylammonium-exchanged vermiculite and smectite and reported that these organocations adsorbed on clays cross-polarized very inefficiently, consistent with a high degree of mobility. O'Brien et al (15) studied triethylphosphate adsorption and intercalation on montmorillonite (5-55% w/w organic on clay) using 1 H, 13 C, and 31 P MAS and CP/MAS NMR. They were able to distinguish one liquid-like species and at least two species in a motion-restricted environment.…”

Section: Introductionmentioning

confidence: 99%

“…In a study (17) of pyridine orientation in the interlayers of kaolinite by IR, XRD, and 29 Si CP/MAS NMR, it was shown that pyridine intercalation causes a high field NMR shift of structural 29 Si in kaolinite. 15 N NMR has so far not been used to study organic compound/clay mineral interactions; however, in several studies , 15 N NMR was used to evaluate acid sites on catalysts such as zeolites (19)(20)(21)(22)(23), silica (24), silica-alumina (25,26), and alumina (27). 15 N NMR of enriched compounds is also a very common technique in biochemistry and biotechnology studies (28) because the natural abundance of 15 N is negligible (0.365%) so the 15 N NMR signal from the matrix does not contribute to the spectra.…”

Section: Introductionmentioning

confidence: 99%

“…15 N NMR has so far not been used to study organic compound/clay mineral interactions; however, in several studies , 15 N NMR was used to evaluate acid sites on catalysts such as zeolites (19)(20)(21)(22)(23), silica (24), silica-alumina (25,26), and alumina (27). 15 N NMR of enriched compounds is also a very common technique in biochemistry and biotechnology studies (28) because the natural abundance of 15 N is negligible (0.365%) so the 15 N NMR signal from the matrix does not contribute to the spectra. In environmental studies, 15 N NMR has been used in the study by Ginwalla and Mikita (29) on 15 N-labeled chloramine reactions with aquatic fulvic acid.…”

Section: Introductionmentioning

confidence: 99%

“…15 N NMR of enriched compounds is also a very common technique in biochemistry and biotechnology studies (28) because the natural abundance of 15 N is negligible (0.365%) so the 15 N NMR signal from the matrix does not contribute to the spectra. In environmental studies, 15 N NMR has been used in the study by Ginwalla and Mikita (29) on 15 N-labeled chloramine reactions with aquatic fulvic acid. Besides avoiding the contribution from the matrix to NMR signal, 15 N NMR has been shown to be more sensitive than 13 C NMR in adsorption studies of molecules with lone-pair electrons on N (24,25).…”

Section: Introductionmentioning

confidence: 99%

“…In environmental studies, 15 N NMR has been used in the study by Ginwalla and Mikita (29) on 15 N-labeled chloramine reactions with aquatic fulvic acid. Besides avoiding the contribution from the matrix to NMR signal, 15 N NMR has been shown to be more sensitive than 13 C NMR in adsorption studies of molecules with lone-pair electrons on N (24,25). This is due to larger density changes upon adsorption around N than around C and to the large chemical shift range of N (∼900 ppm) (30).…”

Section: Introductionmentioning

confidence: 99%

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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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Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

See 3 more Smart Citations

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

Ukrainczyk

Smith

1996

Environ. Sci. Technol.

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Mixed alkyl zinc or cadmium complexes with dialkyl thio‐ or selenocarbamates: Precursors for cadmium chalcogenides

Malik

O’Brien

1994

Adv Material for Optics Elec

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A series of new compounds [RME2CNR′2]2 (R and R′ are various alkyl groups, e.g. M  Zn or Cd, R  Me, R′  Et) have been synthesised and characterised. The compounds can be used as single molecular precursors for the deposition of the corresponding binary chalcogenides. In the present paper the range of compounds synthesised and their uses are reviewed. Preliminary observations on the deposition of thin films on glass and GaAs(100) substrates are reported.

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