Search results for "analytical"
showing 10 items of 9586 documents
New insights in the formation of silanol defects in silicalite-1 by water intrusion under high pressure.
2010
International audience; The "water-silicalite-1" system is known to act as a molecular spring. The successive intrusion-extrusion cycles of liquid water in small crystallites (6 × 3 × 0.5 μm(3)) of hydrophobic silicalite-1 were studied by volumetric and calorimetric techniques. The experiments displayed a decrease of the intrusion pressure between the first intrusion-extrusion cycle and the consecutive ones, whereas the extrusion pressures remained unchanged. However, neither XRD studies nor SEM observations revealed any structural and morphological modifications of silicalite-1 at the long-range order. Such a shift in the value of the intrusion pressure after the first water intrusion-extr…
First signals of electrochemically oxidized species of TTF and TMT-TTF : a study by in situ spectroelectrochemical FTIR and DFT calculations
2003
A first study by in situ FTIR spectroelectrochemistry of TTF and TTM-TTF has been undertaken. The oxidation, in this case, is caused only by electrochemistry, which constitutes a clear advantage over chemical oxidation since no side products are present in the solution. In this context, we obtained the signals of neutral, radical cation, and dication species of TTF and TTM-TTF. The experimental conditions were chosen in order to avoid the possible formation of π-dimer species and to obtain a satisfactory signal-to-noise ratio. A weak signal was detected for TTF and a stronger one for TTM-TTF. The changes induced by the oxidation process in the IR spectra of TTF and TTM-TTF have been analyze…
FT-Raman and QM/MM study of the interaction between histamine and DNA
2006
The interaction between histamine and highly polymerized calf-thymus DNA has been investigated using FT-Raman spectroscopy and the hybrid QM/MM (quantum mechanics/molecular mechanics) methodology. Raman spectra of solutions containing histamine and calf-thymus DNA, at different molar ratios, were recorded. Solutions were prepared at physiological settings of pH and ionic strength, using both natural and heavy water as the solvent. The analysis of the spectral changes on the DNA Raman spectra when adding different concentrations of histamine allowed us to identify the reactive sites of DNA and histamine, which were used to built two minor groove and one intercalated binding models. They were…
Amorphous TiO2 in LP-OMCVD TiNxOy thin films revealed by XPS
2001
Abstract TiN(O)–TiO 2 thin films were prepared on Si(1 0 0) by the low pressure organo metallic chemical vapor deposition (LP-OMCVD) method, using ammonia and titanium isopropoxide as precursors. In order to complete previous characterizations, an Ar + bombardment/XPS coupled study was carried out. This method is based on the fact that the behavior of a compound towards an ion bombardment is a function of its composition. In particular, Ar + bombardment of TiO 2 (whatever its form) leads to a preferential sputtering of oxygen atoms with subsequent reduction of titanium and formation of Ti 3+ and Ti 2+ easily detectable by XPS from a significant broadening of the Ti 2p lines. In the opposite…
Stimulated Raman and Cars Spectroscopy of ν1 and 2ν2 (A1) Bands of 12CF4
1994
Two experimental coherent Raman techniques, stimulated Raman and coherent anti-Stokes Raman spectroscopy (CARS), were employed to study the Raman spectrum of CF 4 in the 900 cm −1 region. The stimulated Raman and CARS spectra of the ν 1 band of CF 4 were recorded at high resolution. The analysis of these spectra enabled some spectroscopic constants of this band to be refined and higher order constants to be determined for the first time. The first high-resolution CARS spectrum of the 2ν 2 (A 1 ) harmonic band is also presented. The rotational transitions of this band up to J = 40 were assigned and the first set of spectroscopic constants for this sub-level were determined. These results imp…
High-resolution stimulated Raman spectroscopy and analysis of the ν 1 band of osmium tetroxide
2012
D.B.P. and R.Z.M. acknowledge the financial support of the Ministry of Science and Innovation through research grant no. FIS2009-08069.
Nitroanilines as Quenchers of Pyrene Fluorescence
2012
The quenching of pyrene and 1‐methylpyrene fluorescence by nitroanilines (NAs), such as 2‐, 3‐, and 4‐nitroaniline (2‐NA, 3‐NA, and 4‐NA, respectively), 4‐methyl‐3‐nitroaniline (4‐M‐3‐NA), 2‐methyl‐4‐nitroaniline (2‐M‐4‐NA), and 4‐methyl‐3,5‐dinitroaniline (4‐M‐3,5‐DNA), are studied in toluene and 1,4‐dioxane. Steady‐state fluorescence data show the higher efficiency of the 4‐NAs as quenchers and fit with a sphere‐of‐action model. This suggests a 4‐NA tendency of being in close proximity to the fluorophore, which could be connected with their high polarity/hyperpolarizability. In addition, emission and excitation spectra evidence the formation of emissive pyrene—NA ground‐state complexes in…
Trace elemental composition of curry by inductively coupled plasma optical emission spectrometry (ICP-OES)
2008
A methodology based on inductively coupled plasma optical emission spectrometry (ICP-OES) after microwave-assisted acid digestion was developed to determine the content of traces elements in curry samples from the Spanish market. The methodology was validated in terms of accuracy by the analysis of citrus and tomato leaf reference materials achieving comparable results with the certified values. The trace metal content of curry samples was compared with data available from previously published reports concerning Indian samples, especially in terms of heavy metal composition, in order to guarantee the quality of the commercially available spices in the European countries. Values found for th…
Attenuated Total Reflection-Fourier transform infrared analysis of the fermentation process of pineapple
2005
Abstract A direct and reagent free procedure has been developed to monitor the fermentation process of pine apple nectar using Attenuated Total Reflectance Fourier-transform mid-infrared spectrometry (FT-IR) and multivariate analysis. A classical 4 2 design for standards was employed for calibration using the information in the spectral range from 907 to 1531 cm −1 of the first order derivative spectra after mean centering of infrared data. The root mean square error of calibration (RMSEC) of 0.040, 0.021, 0.063 and 0.074% w/w were obtained for glucose, fructose, saccharose and ethanol, respectively, and a mean relative validation error of 2.9, 2.1, 2.6 and 3.6% was achieved for glucose, fr…
Optical saturation thermal lens spectrometry in non-polar solvents
1997
Abstract A model for thermal lens spectrometry (TLS) in partial optical saturation conditions which was previously applied to polar solutes in aqueous media is now checked with non-polar organic dyes and metal dithizonates in carbon tetrachloride. Some literature data are also examined. Most data can be consistently explained on the basis of the molecular structures, the sensitivity increasing with the capability of the solute to rapidly communicate the absorbed energy to the solvent molecules.