Solid state NMR characterization of formation of poly(ϵ‐caprolactone)/maghnite nanocomposites by in situ polymerization

Results of multinuclear MAS NMR spectroscopy are reported for poly (ε‐caprolactone)/maghnite nanocomposite formation, with ε‐caprolactone in situ polymerized in the presence of maghnite, a proton exchanged montmorillonite clay. Exfoliated and intercalated materials with different maghnite loading in the range 3–15 wt % were investigated. ¹H NMR evidences Brønsted acid hydroxyl groups in the silicate layers and shows that their broad signal at 7.6 ppm present in the parent clay disappears in the nanocomposite material. ²⁷Al MAS NMR results show that beside the hexacoordinated aluminum signal, two additional peaks corresponding to two different tetrahedral Al sites are present in the clay framework. The NMR signal intensity of only one of them was found to be affected in the nanocomposites compared with the parent maghnite, suggesting that these specific aluminum sites are the reactive ones at the initial stages of the polymerization. However almost no changes occurred in the ²⁹Si NMR spectra, confirming that the polymer grafting, as indicated earlier by atomic force microscopy, took place on the aluminum tetracoordinated sites rather than on the silicon sites. A mechanism of maghnite surface catalyzed polymerization of ε‐caprolactone was proposed, involving Brønsted and Lewis acid sites. © 2007 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 45: 3060–3068, 2007     

Défaut d'exactitude des modéles¶de Néron toriques sur un corps local

Let R be a complete discrete valuation ring with mixed characteristic. Denote by K its field of fractions and by k its residue field. Let 0 →A ^K →B ^K →C ^K → 0 be an exact sequence of abelian varieties over K and consider the corresponding complex of Nérons models 0 →A→B→C→ 0, over R. We assume that the identity component B _k ⁰ of the special fibre B _k of B is a torus and we study the defect of exactmess at B in this last sequence.

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Re?u: 4 décembre 1997/ Version revisée: 15 décembre 1997     

Short-range order and F ion diffusion inside the Pb1 − xAlxF2 + x solid solution Part II: Al NMR investigation and proposal of clustering process

A ²⁷Al nuclear magnetic resonance (NMR) investigation at room temperature of the Pb_{1 − x}Al_xF_{2 + x} (0 ≤ x ≤ 0.12) solid solution and of the ordered Pb₉Al₂F₂₄ phase is carried out. Two different types of aluminium ions are identified and their ratio is determined as a function of x. A clustering process based on the formation of column clusters, more and more extended when x increases, is proposed on the basis of results issued from the ¹⁹F (Part I) and ²⁷Al NMR investigations.     

Synthesis and antibacterial activities of water‐soluble methacrylate polymers containing quaternary ammonium compounds

New water‐soluble methacrylate polymers with pendant quaternary ammonium (QA) groups were synthesized and used as antibacterial materials. The polymers with pendant QA groups were obtained by the reaction of the alkyl halide groups of a previously synthesized functional methacrylate homopolymer with various tertiary alkyl amines containing 12‐, 14‐, or 16‐carbon alkyl chains. The structures of the functional polymer and the polymers with QA groups were confirmed with Fourier transform infrared and ¹H and ¹³C NMR. The degree of conversion of alkyl halides to QA sites in each polymer was determined by ¹H NMR to be over 90% in all cases. The number‐average molecular weight and polydispersity of the functional polymer were determined by size exclusion chromatography to be 32,500 g/mol and 2.25, respectively. All polymers were thermally stable up to 180 °C according to thermogravimetric analysis. The antibacterial activities of the polymers with pendant QA groups against Staphylococcus aureus and Escherichia coli were determined with broth‐dilution and spread‐plate methods. All the polymers showed excellent antibacterial activities in the range of 32–256 μg/mL. The antibacterial activity against S. aureus increased with an increase in the alkyl chain length for the ammonium groups, whereas the antibacterial activity against E. coli decreased with increasing alkyl chain length. © 2006 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 44: 5965–5973, 2006     

SIMPLE TECHNIQUES FOR DETERMINING THE SMALL-SIGNAL EQUIVALENT CIRCUIT OF MESFET’s

Simple techniques for determining the broadband small signal equivalent circuit (SSEC) of MESFETs are presented in this paper. The intrinsic elements are calculated using two-dimensional method from the Y parameters, which are obtained from the Fourier analysis of the device transient response to voltage-step perturbations at the drain and gate electrodes. Whereas, the parasitic external elements are determined by simple approximations used in transmission line modeling. In addition, a new technique is also proposed to determine the source and drain series resistances. A comparison of the SSEC of three different MESFETs technologies shows that the MESFETs on GaN and 4H-SiC are suitable for high power applications. The method used to determine the intrinsic elements is validated with simulated data obtained by Monte Carlo method.     

Transient creep during transformation in Cd-Zn alloys

Transient creep of Cd-2 wt. % Zn and Cd-17·4 wt. % Zn alloys has been studied under different constant stresses ranging from 6·4 MPa to 12·7 MPa near the transformation temperature. The results of both compositions showed two transient deformation regions, the low temperature region (below 483 K) and the high temperature region (above 483 K). From the transient creep described by the equation _tr=Bt ⁿ, where _tr andt are the transient creep strain and time. The parametersB andn were calculated. The parameterB was found to change with the applied stress from 0·3×10^–4 to 3×10^–4 and from 0·6×10^–4 to 18×10^–4 for Cd-2 wt. % Zn and Cd-17·4 wt. % Zn, respectively. The exponentn was found to change from 0·8 to 0·95 for both alloys. The parameterB was related to the steady state creep rate through the equation , the exponent was found to be 0·5 for Cd-2 wt. % Zn and 0·6 for the eutectic composition. The activation energies of transient creep in the vicinity of the transformation regions (above 483 K) were found to be 50·2 kJ/mole for Cd-2 wt. % Zn and 104·7 kJ/mole for the eutectic composition characterizing the mechanisms of grain boundary diffusion and volume diffusion in Cd, respectively.     

Spectrofluorimetric determination of guanethidine sulphate,guanfacine hydrochloride,guanoclor sulphate and guanoxan sulphate in tablets and biological fluids,using benzoin

A sensitive and rapid Spectrofluorimetric method for the determination of guanethidine sulphate, guanfacine hydrochloride, guanoclor sulphate and guanoxan sulphate in tablets and spiked human serum and urine samples is described. The method is based on the reaction of monosubstituted guanidino compounds in an aqueous potassium hydroxide solution with benzoin, in the presence of -mercaptoethanol and sodium sulphite. Highly fluorescent derivatives were obtained, with excitation and emission maximum wavelengths around 325 and 430 nm, respectively. In optimal reaction conditions, the linearity ranges were 0.04–0.28 g/ml, with relative standard deviations less than 2%. The method has been successfully applied to the determination of these drugs in tablets. The results are highly correlated with the B.P. method. Chloroform (or for guanoxan dichloromethane) was used to extract the drugs from serum and urine at basic pH, followed by the proposed fluorimetric method. The limit of detection is 0.02 g/ml for the selected drugs.