Synthesis and characterization of aspartate polymer complexes

Oligomeric polyester, namely poly(tetramethylene asparate) (PTMA), was synthesized From D ,L ‐aspartic acid and 1,4‐butanediol by a melt codensation technique. Polyester–metal complexes were synthesized by the reaction of PTMA with hydrated acetates of Fe(III), Pd(IV), and UO₂(II) in DMSO. The polyester–metal complexes were characterized by elemental analysis, UV–Vis, IR spectral studies, magnetic susceptibility measurements and ¹H‐NMR. Mossbauer spectra of mixed samples of Pd‐PTMA and Fe(II)‐PTMA with a ratio of 1 : 2 mol showed the iron(III) oxide formed in early stages of the decomposition at 250°C is mainly fine‐grained and as the temperature is increased, well‐crystalline hematic is formed. Above 250°C, the Mossbauer spectrum showed the typical six‐line pattern of magnetically oriented Fe(III) oxide, but at 800°C, the spectrum showed quadrupole interaction characteristic of PdFe₂O₄ spinel. The metal ions were found to be six—coordinated with two water molecules as additional ligands besides oxygen and nitrogen atoms of polyester repeating units. Thermogravimetric analysis (DTA‐TG) showed that co‐ordination polymers are thermally more stable than polyester; the activation parameters for both decomposition steps were calculated and discussed. © 2004 Wiley Periodicals, Inc. J Appl Polym Sci 93: 942–947, 2004     

Physicochemical investigation of radiation‐grafted poly(acrylic acid)‐graft‐poly(tetrafluoroethylene–ethylene) copolymer membranes and their use in metal recovery from aqueous solution

ET‐g‐PAAc membranes were obtained by radiation grafting of acrylic acid onto poly(tetrafluoroethylene–ethylene) copolymer films using a mutual technique. The ion selectivity of the grafted membranes was determined toward K⁺, Ag⁺, Hg²⁺, Co²⁺, and Cu²⁺ in a mixed aqueous solution. The ion‐exchange capacity of the grafted membranes was measured by back titration and atomic absorption spectroscopy. The Hg²⁺ ion content of the membrane was more than that of either the K⁺ or Ag⁺ ions. The presence of metal ions in the membranes was studied by infrared and energy‐dispersive spectroscopy measurements. Scanning electron microscopy of the grafted and metal‐treated grafted membranes showed modification of the morphology of the surface due to the adsorption of K⁺ and Ag⁺ ions. No change was observed for the surface of the membrane that was treated with Hg²⁺ ions. The thermal stability of different membranes was improved more with Ag⁺ and Hg²⁺ ions than with K⁺ ions. It was found that the modified grafted membranes possessed good hydrophilicity, which may make them promising candidates for practical applications, such as for cation‐exchange membranes in the recovery of metals from an aqueous solution. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 85: 2692–2698, 2002     

Biologically active polymers. IV. Synthesis and antimicrobial activity of tartaric acid polyamides

New bactericidal polyamides with quaternary ammonium or phosphonium salts were prepared, and their antimicrobial activities were explored. The polyamides were synthesized by the polycondensation of diethyl‐l‐tartrate or chloromethylated diethyl‐l‐tartrate with ethylenediamine in dry absolute ethanol. The polyamides were modified to yield polymers with either quaternary ammonium or phosphonium salts. The polymers were characterized with elemental microanalysis and ¹H‐NMR and IR spectra. The antimicrobial activity of the polymers bearing onium salts was studied against Gram‐negative bacteria (Escherichia coli, Pseudomones aeruginosa, Shigella sp., and Salmonella typhae), Gram‐positive bacteria (Bacillus subtilis and Bacillus cereus), and a fungus (Trichophytum rubrum) by the cut‐plug and viable‐cell‐count methods. Although all the polymers showed high antibacterial activity, some had no antifungal activity. The tributyl phosphonium salt of the polyamide was more effective against both Gram‐negative and Gram‐positive bacteria than the triethyl ammonium and triphenyl phosphonium salts of the polyamide. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 102: 4780–4790, 2006     

Synthesis of well‐defined,functionalized polymer latex particles through semicontinuous emulsion polymerization processes

The design of a semicontinuous emulsion polymerization process, primarily based on theoretical calculations, has been carried out with the objective of achieving overall independent control over the latex particle size, the monodispersity in the particle size distribution, the homogeneous copolymer composition, the concentration of functional groups (e.g., carboxyl groups), and the glass‐transition temperature with n‐butyl methacrylate/n‐butyl acrylate/methacrylic acid as a model system. The surfactant coverage on the latex particles is very important for maintaining a constant particle number throughout the feed process, and this results in the formation of monodisperse latex particles. A model has been set up to calculate the surfactant coverage from the monomer feed rate, surfactant feed rate, desired solid content, and particle size. This model also leads to an equation correlating the polymerization rate to the instantaneous conversion of the monomer or comonomer mixture. This equation can be used to determine the maximum polymerization rate, only below or at which monomer‐starved conditions can be achieved. The maximum polymerization rate provides guidance for selecting the monomer feed rate in the semicontinuous emulsion polymerization process. The glass‐transition temperature of the resulting carboxylated poly(n‐butyl methacrylate‐co‐n‐butyl acrylate) copolymer can be adjusted through variations in the compositions of the copolymers with the linear Pochan equation. © 2003 Wiley Periodicals, Inc. J Appl Polym Sci 88: 30–41, 2003     

The interrelation among network structures,molecular transport of solvent,and creep behaviors of TiB2 ceramic containing butyl rubber composites

Swelling of polymer composites in solvents has become one of the major problems in the use of polymer composites exposed to petroleum products. As a possible solution to the problem, this experimental study was conducted to examine the potential application of TiB₂ ceramic in butyl rubber (IIR) composites. The effect of TiB₂ content on the curing kinetics of IIR composites was studied using a torque rheometer technique. The effect of TiB₂ on the network structure was investigated in terms of the crosslinking density, interparticle distance between conducting particles, surface tension, glass transition temperature, degree of crystallinity, scanning electron microscopy, and X‐ray analysis. Moreover, the effect of TiB₂ content on the molecular transport of solvent (kerosene) was examined by means of degree of swelling, solvent interaction parameters, volume fraction of rubber, interparticle distance after swelling, penetration rate of solvent, mean diffusion coefficient, cohesive energy density of polymer, standard entropy, standard enthalpy, and standard free energy of IIR composites. It was ascertained that with increasing TiB₂ content the degree of swelling shifts to a lower value. The main reason was interpreted as the introduction of good interface adhesion of TiB₂ with rubber matrix, which tends to block the diffusion of solvent molecules. The effect of TiB₂ content on hardness, tensile strength, Young's modules, and elongation at break is discussed. An apparent steady‐state creep of butyl rubber IIR/TiB₂ composites is evident under different constant stresses at room temperature. The strain rate of steady‐state creep showed a dependence on stress and TiB₂ volume fraction. The stress sensitivity parameter, viscosity coefficient, and activation volume for samples loaded with different content of TiB₂ were estimated. It is apparent that these new composites should be very useful for solvent permeation resistance at high TiB₂ loading level with good mechanical properties. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 98: 2226–2235, 2005     

Electrocardiogram Signal Denoising Using Discrete Wavelet Transform

The most common noises in ECG （electrocardiogram） signal processing are BW （baseline wandering） and the 50 or 60 Hz PLI （power line interferences）. In order to remove these two major source of noises, we have used the recent powerful DWT （discrete wavelet transform） signal processing in ECG signals which are obtained from MIT-BIH Arrhythmia Database. The results indicate that DWT is a good method for filtering noises without changing the morphology of ECG, and can be applied to all types of ECG signals, whether normal or presenting arrhythmias.     

Gestational and lactational exposure to dichlorinated bisphenol A induces early alterations of hepatic lipid composition in mice

Objective

Using non-invasive magnetic resonance (MR) techniques and a histological approach, we assessed the outcomes of perinatal exposure at a low dose of 3,3′-DCBPA (2-chloro-4-[1-(3-chloro-4-hydroxyphenyl)-1-methylethyl]phenol) and/or 3,5-DCBPA (2,6-dichloro-4-[1-(4-hydroxyphenyl)-1-methylethyl]phenol) on mice livers.

Materials and methods

Fertilized female Swiss mice were injected intraperitoneally during gestation and lactation with either vehicle control, 20 μg/kg/day of BPA, 3,5-DCBPA, 3,3′-DCBPA or a mixture (mix-DCBPA). Complementary methods were used to evaluate, in male and female pups, (1) liver structure by texture analysis of images obtained through MR imaging (MRI) and histology, (2) hepatic lipid composition through in vivo ¹H MR spectroscopy (¹H MRS).

Results

Principal component analysis of texture parameters showed no structural modification of the liver with BPA and DCBPA treatments. Accordingly, no hepatic microvesicular steatosis was observed through hematoxylin–eosin staining. Compared to control, MRS revealed no difference in lipid composition for BPA, 3,5-DCBPA or 3,3′-DCBPA groups. However, MRS detected a significant increase in the mix-DCBPA groups for the saturated component of fatty acids (FA), total unsaturated FA bond index and polyunsaturated FA bond index.

Conclusion

Prior to any structural changes, polyunsaturated fatty acids significantly increased in young male and female mice exposed perinatally at a low dose to a mixture of dichlorinated BPA.

     

Quantized H∞ filtering for state‐delayed systems with finite frequency specifications

This paper presents a novel design approach for the finite frequency (FF) H_∞ filtering problem for discrete‐time state‐delayed systems with quantized measurements. The system state and output are assumed affected by FF external noises. Attention is focused on the design of a stable filter that guarantees the stability and a prescribed ?₂ gain performance level for the filtering error system in the FF domain of input noises. Sufficient conditions for the solvability of this problem are developed by choosing an appropriate Lyapunov‐Krasovskii functional based on the delay partitioning technique and using the FF ?₂ gain definition combined with the generalized S‐procedure. Then, by means of Finsler's lemma, the derived conditions are linearized and additional slack variables are further introduced to more flexible result. Final filter design conditions are consequently established in terms of linear matrix inequalities in three different frequency ranges, ie, low‐, middle‐ and high‐frequency range. Finally, a simulation example is presented to illustrate the effectiveness and the merits of the proposed approach.     

Hierarchical porous carbon templated with silica spheres of a diameter of 14 nm from pure chitosan or a chitosan/ZnCl<Subscript>2</Subscript> solution

Nitrogen-containing mesoporous carbons with the use of colloidal silica spheres of (14 nm) and chitosan as a carbon precursor were obtained. A removal of such small template particles from carbonized silica–chitosan composite is difficult and HF with a minimum concentration of 15 wt% should be used. By varying the silica-to-chitosan ratio, the porous characteristic of products is controlled. The modification by ZnCl₂ with a molar Zn-to-C (in chitosan mass) ratio of ‘6’ results in the development of microporosity; however it is accompanied by a significant reduction of mesopore volume (V_mes). The addition of ZnCl₂ in a ratio of ‘5.25’ and pH adjustment to 5.8 increase the volumes of micropores, small mesopores, BET surface area to 1975 m²/g, and preserve V_mes of 4.15 cm³/g. The novelty of the presented strategy is the creation of microporosity in the hard-templated materials by incorporating ZnCl₂ into the mixture of Ludox HS-40 template and chitosan precursor, as well as the investigation on how the pH of synthesis influences the final porosity. The pH of a silica–chitosan–zinc solution, equal to 3.9, provides some coordination of Zn²⁺ by –OH and –NH₂ groups, whereas pH adjustment to 5.8 results in the precipitation of a new template—Zn(OH)₂.     

Synthesis,Characterization, and Applications of Some New Trimeric‐Type Cationic Surfactants

In recent years, trimeric surfactants have created excitement in the surfactant field because of their properties, which have been found to be better than monomeric or dimeric homologues. Only a limited number of trimeric surfactants have been synthesized and studied so far, probably owing to the difficulty in synthesis. In this article, we synthesized some novel star‐shaped trimeric cationic surfactants based on the alkylation of the 3 hydroxyl groups of the phloroglucinol nuclei as a core (i.e., spacer) with 3 dodecyl or 3 octyl groups (as tails) for the surfactant. The chemical structures were confirmed by nuclear magnetic resonance, Fourier transform infrared, mass spectrometry, and elemental analysis; also the critical micelle concentration was determined by electrical conductivity measurements. These surfactants were used in the synthesis of mesoporous silica nanoparticles by the sol–gel method. The silica particles shape and size were determined using field emission scanning electron microscopy and high‐resolution transmission electron microscopy images. Furthermore, the corrosion inhibitor capability of these surfactants was investigated by monitoring the corrosion rate of iron sheets in 0.5 M hydrochloric acid in the presence and in the absence of different surfactants at 45°C based on the weight loss method. We have used cetyltrimethylammonium bromide (CTAB) as a positive control, the obtained results showed a high inhibition efficiency at very low concentrations, and the prepared trimeric surfactants exhibited a higher anticorrosion efficiency than the CTAB surfactants.