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71.
Alain Chaintreau Wolfgang Fieber Horst Sommer Alexis Gilbert Keita Yamada Naohiro Yoshida Alain Pagelot Detlef Moskau Aitor Moreno Jürgen Schleucher Fabiano Reniero Margaret Holland Claude Guillou Virginie Silvestre Serge Akoka Gérald S. Remaud 《Analytica chimica acta》2013
Isotopic 13C NMR spectrometry, which is able to measure intra-molecular 13C composition, is of emerging demand because of the new information provided by the 13C site-specific content of a given molecule. A systematic evaluation of instrumental behaviour is of importance to envisage isotopic 13C NMR as a routine tool. This paper describes the first collaborative study of intra-molecular 13C composition by NMR. The main goals of the ring test were to establish intra- and inter-variability of the spectrometer response. Eight instruments with different configuration were retained for the exercise on the basis of a qualification test. Reproducibility at the natural abundance of isotopic 13C NMR was then assessed on vanillin from three different origins associated with specific δ13Ci profiles. The standard deviation was, on average, between 0.9 and 1.2‰ for intra-variability. The highest standard deviation for inter-variability was 2.1‰. This is significantly higher than the internal precision but could be considered good in respect of a first ring test on a new analytical method. The standard deviation of δ13Ci in vanillin was not homogeneous over the eight carbons, with no trend either for the carbon position or for the configuration of the spectrometer. However, since the repeatability for each instrument was satisfactory, correction factors for each carbon in vanillin could be calculated to harmonize the results. 相似文献
72.
Tessonnier JP Louis B Walspurger S Sommer J Ledoux MJ Pham-Huu C 《The journal of physical chemistry. B》2006,110(21):10390-10395
On the basis of our previous H/D exchange studies devoted to the quantification of the number of Br?nsted acid sites in solid acids, we report here an innovative approach to determine both the amount and the localization of Mo atoms inside the Mo/ZSM-5 catalyst, commonly used for the methane dehydroaromatization reaction. The influence of Mo introduction in the MFI framework was studied by means of BET, X-ray diffraction, 27Al magic angle spinning NMR, NH3 temperature-programmed desorption, and H/D isotopic exchange techniques. A dependence was found between the decrease of acidic OH groups and the Mo content. Depending on the Si/Al ratio of the zeolite, i.e., the proximity of two Br?nsted acid sites, the Mo atoms substitute a different number of OH groups. Consequently, a chemical structure was proposed to describe the geometry of the Mo complex in the channels of the ZSM-5 zeolite. 相似文献
73.
We study the dynamics of tethered chains of length N on adsorbing surfaces, considering the dilute case; for this we use the bond fluctuation model and scaling concepts. In particular, we focus on the mean-square displacement of single monomers and of the center of mass of the chains. The characteristic time tau of the fluctuations of a free chain in a good solvent grows as tau approximately N(a), where the coefficient a obeys a=2nu+1. We show that the same coefficient also holds at the critical point of adsorption. At intermediate time scales single monomers show subdiffusive behavior; this concurs with the behavior calculated from scaling arguments based on the dynamical exponent a. In the adsorbed state tau(perpendicular), the time scale for the relaxation in the direction perpendicular to the surface, becomes independent of N; tau(perpendicular) is then the relaxation time of an adsorption blob. In the direction parallel to the surface the motion is similar to that of a two-dimensional chain and is controlled by a time scale given by tau(parallel) approximately N(2nu(2)+1)L(-2Delta(nu/nu)), where nu(2) is the Flory exponent in two dimensions, nu is the Flory exponent in three dimensions, and Deltanu=nu(2)-nu. For the motion parallel to the surface we find dynamical scaling over a range of about four decades in time. 相似文献
74.
P. Schmid K. Uran F. Macherey M. Ebert H.-J. Ullrich D. Sommer F. Friedel 《Analytical and bioanalytical chemistry》2009,393(8):1863-1870
The formation of Fe–Zn intermetallic compounds, as relevant in the commercial product galvannealed steel sheet, was investigated
by scanning electron microscopy and different methods of X-ray diffraction. A scanning electron microscope with high resolution
was applied to investigate the layers of the galvannealed coating and its topography. Grazing incidence X-ray diffraction
(GID) was preferred over conventional Bragg–Brentano geometry for analysing thin crystalline layers because of its lower incidence
angle α and its lower depth of information. Furthermore, in situ experiments at an environmental scanning electron microscope (ESEM)
with an internal heating plate and at an X-ray diffractometer equipped with a high-temperature chamber were carried out. Thus,
it was possible to investigate the phase evolution during heat treatment by X-ray diffraction and to display the growth of
the ζ crystals in the ESEM. 相似文献
75.
76.
77.
Hanns Sommer 《Chaos, solitons, and fractals》2009,39(3):1027-1036
A model for the process of knowledge acquisition is presented that shows how naive realism emerges from a quantum mechanical background. We formalise this process of emergence and obtain in this way an illustrative insight to some of the most fundamental physical theories: GRW-theory and E∞-theory. 相似文献
78.
Simulations of polyelectrolyte dynamics in an externally applied electric field in confined geometry
We consider the dynamics of charged polymers in free solution in a slit geometry under the influence of an electrical field, applied at an angle to the plane parallel walls of the confinement. The simulations are carried out using the Brownian dynamics method with explicit counterions and implicit hydrodynamics. The hydrodynamic interactions between all the particles and the plane parallel walls are taken into account using a diffusion matrix which depends on slit geometry and the actual polyelectrolyte-solute conformations. We observe a selective transport of the charged polymers, as a function of the degree of polymerization and slit height. 相似文献
79.
Elmar Cohors-Fresenborg Silke Kramer Frank Pundsack Johann Sjuts Norbert Sommer 《ZDM》2010,42(2):231-244
The relationship between practised monitoring activities and performance, especially in mathematics was examined within three nested studies. The first study deals with problems of faulty term rewritings submitted to three groups of subjects—10th to 13th graders, differing in their mathematical performance—whose task was to find the mistakes. Moreover, a questionnaire on the practice and appreciation of monitoring activities was developed. The third study, first, repeats the first study with a similar population and secondly adds interviews with some of the subjects while solving additional items concerning faulty term rewritings. Studies 1 and 3 show similar success in finding mistakes and in the replies to the questionnaire within the various groups. Furthermore, the third study points up that the subject’s answers do neither predict the practised monitoring nor the success in the test. However, the success correlates significantly with the practised monitoring. For a deeper understanding concerning the role of metacognition in explaining performance, the second study examined two of the groups who had already been involved in the first study. These were assigned some problems of a matrices test as used in cognitive psychology. While trying to solve the problem, their eye movements were recorded by means of an eye-tracker. Afterwards they had to justify their solutions in an interview. The eye movements were analysed, the verbal comments classified. Again, the groups differ in their problem solving success, dependant on the quality of the monitoring practised. Altogether, the results of the three studies elucidate the importance of practised metacognitive monitoring activities not only for success in school algebra, but furthermore the ability and the willingness to do it is deeper anchored in a person than just a trained behaviour for school algebra. 相似文献
80.
We are proposing a lattice model with chemical input for the computer modelling of the polymer glass transition. The chemical input information is obtained by a coarse graining procedure applied to a microscopic model with full chemical detail. We use this information on Bisphenol-A-Polycarbonate to predict it's Vogel-Fulcher temperature out of a dynamic Monte Carlo Simulation. The microscopic structure of the lattice model is that of a genuine amorphous material, and the structural relaxation obeys the time temperature superposition. 相似文献