Search results for "Magic angle"
showing 10 items of 57 documents
Etude par spectroscopies de RMN 23Na, 31P et 1H : effets de la teneur en sel (NaCl) dans des matrices alimentaires
2008
The reduction of salt (NaCl) content in food has become a matter of public health. However, the multiple functions of salt in food make the reduction of its content difficult. The aim of this work was to demonstrate the applicability of NMR innovative techniques in order to characterise the mobility of sodium ions (distinction between ‘free’ and ‘bound’ sodium), to bring a better understanding of the role of salt in the organisation of the food matrix (in particular phosphorous molecules in dairy systems) and to study impact of salt on the mobility of aroma compounds. In a first step, the 23Na NMR study of iota-carrageenan gels validated the quantification of total sodium (Single-Quantum, S…
Spectroscopic and conformational properties of size-fractions separated from a lignite humic acid
2007
Abstract A lignite humic acid (HA) was fractionated by preparative high performance size-exclusion chromatography (HPSEC) in seven different size-fractions. The size-fractions were characterized by cross polarization (CP) magic angle spinning (MAS) 13 C NMR spectroscopy and a further analytical HPSEC elution under UV and fluorescence detection. The alkyl hydrophobic components mainly distributed in the largest molecular-size-fraction, whereas the amount of oxidized carbons increased with decreasing size of fractions. Cross polarization time ( T CH ) and proton spin-lattice relaxation time in the rotating frame ( T 1 ρ (H)) were measured from variable contact time (VCT) experiments. The bulk…
A Straightforward Approach to Multifunctional Graphene
2019
Graphene has been covalently functionalized through a one-pot reductive pathway using graphite intercalation compounds (GICs), in particular KC8 , with three different orthogonally protected derivatives of 4-aminobenzylamine. This novel multifunctional platform exhibits excellent bulk functionalization homogeneity (Hbulk ) and degree of addition while preserving the chemical functionalities of the organic addends through different protecting groups, namely: tert-butyloxycarbonyl (Boc), benzyloxycarbonyl (Cbz) and phthalimide (Pht). We have employed (temperature-dependent) statistical Raman spectroscopy (SRS), X-ray photoelectron spectroscopy (XPS), magic angle spinning solid state 13 C NMR …
Understanding the physicochemical properties of olive kernel to be used as a potential tool in the development of phenol-formaldehyde wood adhesive
2015
Abstract During olive oil production process, a great number of by-products are generated, including olive kernel. These by-products can be used for the development of new products for use in many different industrial applications. The evaluation of the physicochemical properties of these by-products constitutes a key factor in evaluating the potential reutilization of olive oil by-products. In the present study, the physicochemical properties of olive kernel were analyzed. Fourier transform infrared spectroscopy (FT-IR), cross-polarization magic angle spinning 13 C nuclear magnetic resonance (CP/MAS 13 C NMR), Brunauer, Emmett and Teller (BET), scanning electron microscopy (SEM) and thermo…
Multi-layered, covalently supported ionic liquid phase (mlc-SILP) as highly cross-linked support for recyclable palladium catalysts for the suzuki re…
2011
The reaction between an excess of 1,4-bis(3-vinylimidazolium-1-yl) bromide and a mercaptopropyl-modified amorphous silica gel or ordered mesoporous silica SBA-15 in the presence of azobisisobutyronitrile (AIBN) afforded new materials, which have a high loading of imidazolium moieties. These materials, which contain a highly cross-linked polymeric network, have been denoted as multi-layered, covalently supported ionic liquid phase (mlc-SILP) and have been used as support for palladium catalysts containing a high loading of the metal (10 wt%). Such materials were characterized by several techniques (13C magic angle spinning nuclear magnetic resonance, the Brunauer–Emmett–Teller technique, sma…
Dynamics of cross polarization in solid state nuclear magnetic resonance experiments of amorphous and heterogeneous natural organic substances
2008
Nuclear magnetic resonance (NMR) experiments on carbon-13 in the solid state were done with cross polarization (CP) and magic angle spinning (MAS) in order to overcome the low NMR sensitivity of (13)C and the chemical shift anisotropy, respectively. In the present research, CPMAS (13)C-NMR spectra were collected by modulating the contact time needed for cross polarization (variable contact times experiments, VCT) on two different humic acids (a soil-HA and a coal-HA). VCT data were fitted by a model containing either a monotonic or a non-monotonic cross polarization term. The non-monotonic model, which fitted the experimental results better than the monotonic one, provided two cross-polariz…
Advanced CPMAS-13C NMR techniques for molecular characterization of size-separated fractions from a soil humic acid
2006
A humic acid extracted from a volcanic soil was subjected to preparative high-performance size-exclusion chromatography (HPSEC) to reduce its molecular complexity and eleven different size fractions were obtained. Cross-polarization magic-angle spinning 13C NMR (CPMAS 13C NMR) analysis performed with variable contact-time (VCT) pulse sequences showed that the largest molecular-size fractions contained aromatic, alkyl, and carbohydrate-like components. The carbohydrate-like content and the alkyl chain length seemed to decrease with decreasing molecular size. Progressive reduction of aromatic carbon atoms was also observed with decreasing molecular size of the separated fractions. Mathematica…
Effect of Heating Time and Temperature on the Chemical Characteristics of Biochar from Poultry Manure
2014
Poultry manure (PM) chars were obtained at different temperatures and charring times. Chemical-physical characterization of the different PM chars was conducted by cross-polarization magic angle spinning (CPMAS) (13)C NMR spectroscopy and thermal analysis. CPMAS (13)C NMR spectra showed that the chemical composition of PM char is dependent on production temperature rather than on production duration. Aromatic and alkyl domains in the PM chars obtained at the lowest temperatures remained unchanged at all heating times applied for their production. The PM char obtained at the highest temperature consisted only of aromatic structures having chemical nature that also appeared invariant with hea…
Interactions between 2-Aminobenzothiazole and Natural Organic Matter as Evidenced by CPMAS Nitrogen-15 NMR Spectroscopy
2009
Cross-polarization magic angle spinning (CPMAS) 15N nuclear magnetic resonance (NMR) spectroscopy was used to study the interactions between 2-aminobenzothiazole (ABT) and natural organic matter in the presence of the natural enzyme laccase and synthetic air. Through the use of synthesized model compounds, we were able to confirm previous findings by CPMAS 13C NMR spectroscopy that showed the formation of covalent amide bonds. We also provide evidence of the presence of two additional H bonds between ABT and the natural organic matter. Both H bonds involved the amino and thiazole groups of ABT.
Distribution and mobility of phosphates and sodium ions in cheese by solid-state 31 P and double-quantum filtered 23 Na NMR spectroscopy
2010
The feasibility of solid-state magic angle spinning (MAS) (31)P nuclear magnetic resonance (NMR) spectroscopy and (23)Na NMR spectroscopy to investigate both phosphates and Na(+) ions distribution in semi-hard cheeses in a non-destructive way was studied. Two semi-hard cheeses of known composition were made with two different salt contents. (31)P Single-pulse excitation and cross-polarization MAS experiments allowed, for the first time, the identification and quantification of soluble and insoluble phosphates in the cheeses. The presence of a relatively 'mobile' fraction of colloidal phosphates was evidenced. The detection by (23)Na single-quantum NMR experiments of all the sodium ions in t…