The goal of our studies was to determine the nature of interactions between catalytic active samples, such as polypyrrole (PPy) doped with: chloride anions, heteropolyacids such as H5PMo10V2O40, or H4SiW12O40, and oxygen particles. In order to reveal the mechanism of the linkage between the catalysts and oxygen we provided the electron paramagnetic resonance (EPR) measurements of synthesized samples in O2 and N2 flow. Moreover, the X-ray photoelectron spectroscopy (XPS) measurements were performed to show the properties of doped heteropolyacids and the state of nitrogen in polypyrrole matrix. The results of EPR studies of PPy(Cl), PPy(H4SiW12O40), PPy(H5PMo10V2O40) samples, show that the polypyrrole doped with chloride anions interacts much easier with oxygen than polypyrrole doped with heteropolyacids (in the above given order, of preference with the most active polypyrrole system first). It correlates with XPS results, which show that a molybdenium-vanadium anion is more reduced than a silicon-tungsten one. The redox reactions of heteropolyacids involve the oxidation-reduction of the conjugated polymer chain, leaving no or little place for interactions with oxygen. Polypyrrole doped with H4SiW12O40 shows some oxygen sensitivity as observed in the EPR studies, as opposed to polypyrrole doped with H5PMo10V2O40, which is in line with the XPS results. 相似文献
In this paper, several methods of hydrophobization of cotton fabrics using the thio-ene click reaction were compared. Durable, superhydrophobic textiles were obtained in an easy way. Various variants of functionalized silsesquioxanes were used for the hydrophobization of fabrics. The synthesis of bifunctional silsesquioxanes (RSiMe2O)4(ViSiMe2O)4Si8O12 and (RSiMe2O)4(R’SiMe2O)4Si8O12 were performed via hydrothiolation of silsesquioxane derivative (ViSiMe2O)8Si8O12. Alkoxysilyl, alkyl and fluoroalkyl moieties were introduced as functional groups. Samples were prepared using four methods, differing in the modification method and the number of stages. During the research, fabrics were modified via (a) the dip-coating process, (b) carrying out thiol-ene click reactions directly on the surface of the fabric and (c) using both of these methods. The hydrophobicity of the fabric was evaluated by measuring the Water contact angle (WCA). The obtained samples were also examined using infrared analysis (FT-IR), Scanning electron microscope (SEM), and Elemental analysis (SEM–EDS). All analyses were performed before and after the washing process in order to verify the stability of the performed modifications.
A sensitive method of Co(II) determination by adsorptive stripping voltammetry is presented. The method exploits the enhancement of cobalt peak current observed in the system Co(II)-nioxime-cetyltrimethylammonium bromide-piperazine-N,N′-bis(2-ethanesulfonic acid). The calibration plot for an accumulation time of 60 s is linear from 5 × 10−11 to 3 × 10−9 mol L−1. The relative standard deviation is 3.8% for Co(II) determination at concentration 1 × 10−9 mol L−1. The detection limit is 1.7 × 10−11 mol L−1. The validation of the method is performed by the analyses of certified reference materials and comparing the result of Co(II) determination in river water sample by the proposed method with those obtained by ET AAS. The main advantage of this new system is the micro-trace Co(II) determination by adsorptive stripping voltammetry, as compared to those described before, a low concentration of the supporting electrolyte used, and so commercially available reagents without additional purification can be used. 相似文献
Studies in Stereochemistry XIV. Diels-Alder adducts in the resin series; action of peracids and acid-catalysed ring opening of epoxides The synthesis of Diels-Alder compounds of type 2 with a 17-nor-13(14)-atisène skeleton is described (cf. Schemes 1–3). Depending on the nature and configuration of substituents R1 and R2 on the carbon atoms 15 and 16, an epoxide ( 24–33 ) or a ketone ( 35–38 ) or a mixture of epoxide, ketone and lactone is obtained by the action of p-nitroperbenzoic acid on the double bond of these adducts (cf. Scheme 4). A simplified reaction scheme is suggested to explain the formation of the various products. In an acid-catalysed reaction, the epoxides isomerize mainly into ketones. Nevertherless, in some cases, dienes (e.g. 52 ) or hydroxy-γ-lactones of (13R*, 14S*)-configuration (e.g. 50 ) resulting from the opening of the epoxide ring with retention of configuration were obtained. 相似文献
Procedures for trace cobalt determinations by adsorptive stripping voltammetry at in situ and ex situ plated bismuth film electrodes are presented. These exploit the enhancement of the cobalt peak obtained by using the Co(II)–dimethylglyoxime–cetyltrimethylammonium bromide–piperazine-N,N-bis(2-ethanesulfonic acid) system. The calibration graph for an accumulation time of 120 s was linear from 2 × 10–10 to 2 × 10–8 mol L–1. The relative standard deviation from five determinations of cobalt at a concentration of 5 × 10–9 mol L–1 was 5.2%. The detection limit for an accumulation time of 300 s was 1.8 × 10–11 mol L–1. The proposed procedure was applied to cobalt determination in certified reference materials and in tap and river water samples. 相似文献
Structural investigations on powder samples of Y2Ba4Cu7O15–x with different carbonate content have been performed. Powder x-ray Rietveld refinements showed the remarkable influence of carbonate incorporation on the lattice parameters. Most important is the decrease of Tc with increasing carbonate content. We assign these effects to an incorporation of the carbonate ion into the crystal lattice, copper vacancies at the Cu(1) position and a possible misorientation of the copper oxygen single chains. No change of the structure (e. g. superstructure) could be found. 相似文献
The S2-S0 fluorescence excitation spectra ofxanthione (XT) and azulene (AZ) complexed with 1 or 2 molecules of the C1 to C10n-alkanes and the C1 to C6 perfluoro-n-alkanes have been measured. The 1:1 complexes exhibit microscopic solvent shifts, Δ
gn, which are larger for the alkanes than the corresponding perfluoroalkanes, despite the larger molecular polarizability of the latter. The values of Δ
gn increase monotonically with carbon number of the adduct to C10 in 1:1 n-alkane complexes with XT and to C5 in 1:1 n-alkane complexes with AZ. However, Δ
gn exhibits no further increase beyond C2 in 1:1 perfluoro-n-alkane complexes with XT and beyond C3 in 1:1 perfluoro-n-alkane complexes with AZ. The results are interpreted in terms of a model in which the n-alkanes stretch out along the long axis of the chromophore and ‘wet’ its surface whereas the perfluoro-n-alkanes with carbon numbers 3 away from the surface of the chromophore and are ‘non-wetting’. 相似文献
The S2 → S0 fluorescence spectra and quantum yields and the S2 lifetimes of 2,2,3,3-tetramethylindanethione (TMIT) have been measured in several solvents using a synchronously pumped picosecond dye laser excitation system. The S2 nonradiative decay rate is markedly solvent dependent. In inert perfluoroalkane solvents remarkably large S2-S0 fluorescence quantum yields (θf = 0.14) and long S2 lifetimes (τ = 880 ps) are measured. Hydrocarbons are efficient excited-state quenchers. 相似文献