Pre-irradiation induced grafting of styrene into crosslinked and non-crosslinked polytetrafluoroethylene films for polymer electrolyte fuel cell applications. II: Characterization of the styrene grafted films

Crosslinked and non-crosslinked polytetrafluoroethylene films (RX-PTFE and V-PTFE films, respectively) were irradiated by γ-ray and then grafted with styrene in liquid phase. Microscope FT-IR spectroscopy, TGA, solid state ¹³C CP/MAS and high resolution HS/MAS NMR spectroscopy, wide-angle X-ray diffraction (WAXD) study were used to get the structural information of the styrene grafted RX-PTFE and V-PTFE films. From microscope FT-IR spectra of the grafted RX-PTFE films, the “grafting front mechanism” was proved. TGA analysis showed that the grafted films have a small degradation step and two main degradation steps. In the ¹³C CP/MAS NMR spectra of the non-grafted films, there are no signal due to the absence of the hydrogen atom. While in the spectra of the grafted films, there are signals attributed to the polystyrene grafts. In the ¹³C HS/MAS NMR spectra of the grafted films, the relative intensity of the peaks attributed to the polystyrene grafts increased while the relative intensity of the peak attributed to PTFE matrix decreased with the increase in the DOG. From WAXD patterns, the intensity of the crystalline peak decrease with the increase in the DOG. The grafted films were sulfonated by chlorosulfonic acid and the results of highest IEC value exceeded 3.0. Those results will be reported in the near future.     

Removal of the impurities from environmental water samples for tritium measurement by liquid scintillation counting

Liquid scintillation counting is the most popular method for tritium measurement, however, it takes much time and a lot of doing to distill off the impurities before mixing the sample water and liquid scintillation cocktail. We have investigated the possibility of an alternative method to the distillation. We have found out that the filtration can be an alternative to distillation for the environmental water samples before electrolytic enrichment.     

The crystal structures of α- and β-CdUO4

The structural parameters of α- and β-CdUO₄ crystals are determined by X-ray powder diffraction technique. α-CdUO₄ is rhombohedral and cell parameters are a = 6.233(3) Å and α = 36.12(5)°. β-CdUO₄ crystallizes in a C-centered orthorhombic cell with a = 7.023(4), b = 6.849(3), c = 3.514 (2) Å. The space groups are $\text{R}\text{3}\text{m}$ for α-CdUO₄ and Cmmm for β-CdUO₄. α-CdUO₄: 1U in (000), 1Cd in ($\text{1}\text{2}\text{1}\text{2}\text{1}\text{2}$), 2O(1) in ±(uuu), 2O(2) in ±(vvv); u = 0.113, v = 0.350, Z = 1. β-CdUO₄: 2U in ($\text{000;}\text{1}\text{2}\text{1}\text{2}\text{0}$), 2Cd in ($\text{1}\text{2}\text{0}\text{1}\text{2}\text{; 0}\text{1}\text{2}\text{,}\text{1}\text{2}$), 4O(1) in ($\text{0, ±y, 0;}\text{1}\text{2}\text{,}\text{1}\text{2}\text{±y, 0}$), 4O(2) in ($\text{±x, 0,}\text{1}\text{2}\text{;}\text{1}\text{2}\text{±x,}\text{1}\text{2}\text{,}\text{1}\text{2}$); x = 0.159, y = 0.278, Z = 2. β-CdUO₄ contains collinear uranyl UO²⁺₂ groups with a UO(1) distance of 1.91 Å, located either along or parallel to the c axis whereas the UO(1) bond length in α-CdUO₄ is 1.98 Å which is longer than the usual uranyl bond length.     

An infeasible interior-point arc-search algorithm for nonlinear constrained optimization

Numerical Algorithms - In this paper, we propose an infeasible arc-search interior-point algorithm for solving nonlinear programming problems. Most algorithms based on interior-point methods are...     

Catalytic asymmetric desymmetrization of cyclic meso-1,3- and 1,4-diols by a phosphinite derivative of quinidine

Asymmetric monobenzoylation reactions of cyclic meso-1,3- and 1,4-diols were catalyzed by a phosphinite derivative of quinidine to afford the corresponding monobenzoylated diol with good yield and enantioselectivity. [reaction: see text]     

Stereoselective synthesis of (Z)-fluoroalkenes directed to peptide isosteres: copper mediated reaction of trialkylaluminum with 4,4-difluoro-5-hydroxyallylic alcohol derivatives

Copper mediated alkyl-transfer reaction of trialkylaluminum (R₃Al) with (E)-4,4-difluoro-5-hydroxyallylic alcohol derivative smoothly proceeded to give the corresponding 2-alkylated 4-fluoro-5-hydroxyhomoallylic alcohol derivative with completely Z and 2,5-syn selective manner. Regio- and stereoselective conversion of the C5-hydroxyl group of the fluoroolefin thus obtained to amino group could be achieved through one-pot mesylation and azidation reaction.     

A novel method for preparation of 2-(methyl- or phehnylthio)alkanoic esters

Ethyl 2-acetylalkanoate gave ethyl 2-(methyl- or phenylthio)alkanoate in high yield on treatment wiht CH₃SSO₂CH₃, PhSSO₂Ph, or PhSSPh in the presence of small excess of EtONa in EtOH. Application of the present method to synthesis of pellitorine and the queen substance is also described.