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Sample records for acid complex films

  1. Structural organization of films based on polyaniline/polysulfonic acid complexes depending on the synthesis method

    The optical properties and morphology of complexes based on polyaniline (PANI) and poly(2-acrylamido-2-methyl-1-propanesulfonic acid) (PAMPS), depending on their synthesis conditions, have been characterized by UV-visible spectroscopy and atomic force microscopy. The dependence of the electron absorption spectra of PANI/PAMPS complexes and the surface topography of their films on the initiation way of PANI formation (chemical and enzymatic) and the use of promoters of aniline polymerization has been investigated. The aniline polymerization kinetics with and without polymerization promoters has been studied. All PANI/PAMPS complexes are found to have a nanocomposite time-stable structure.

  2. Improvement of the photo stabilization of PVC films in the presence of thioacetic acid benzothiazole complexes

    The photo stabilization of poly(vinyl chloride) (PVC) films by 2-thioacetic acid benzothiazole with Sn (II), Cd (II), Ni (II), Zn (II) and Cu (II) complexes was investigated. The PVC films containing concentration of complexes 0.5 % by weight were produced by the same casting method from tetrahydrofuran (THF) solvent. The photo stabilization activities of these compounds were determined by monitoring the carbonyl, polyene and hydroxyl indices with irradiation time. The changes in viscosity average molecular weight of PVC with irradiation time were also tracked (using THF as a solvent). The quantum yield of the chain scission (φcs) of these complexes in PVC films was evaluated and found to range between 4.71 x 10-8 and 8.98 x 10-8. Results obtained showed that the rate of photo stabilization of PVC in the presence of the additive follows the trend: Sn(L)2 > Cd(L)2 > Ni(L)2 > Zn(L)2 > Cu(L)2. According to the experimental results obtained, several mechanisms were suggested depending on the structure of the additive. Among them HCl scavenging, UV absorption, peroxide decomposer and radical scavenger for photo stabilizer additives mechanisms were suggested. (author)

  3. Optical characterization and blu-ray recording properties of metal(II) azo barbituric acid complex films

    Smooth thin films of nickel(II), cobalt(II) and zinc(II) complexes with azo barbituric acid were prepared by the spin-coating method. Absorption spectra of the thin films on K9 glass substrates in 300-700 nm wavelength region were measured. Optical constants (complex refractive index N = n + ik) of the thin films prepared on single-crystal silicon substrates in 275-695 nm wavelength region were investigated on rotating analyzer-polarizer type of scanning ellipsometer, and dielectric constant ε (ε = ε1 + iε2) as well as absorption coefficient α of thin films were calculated at 405 nm. In addition, static optical recording properties of the cobalt(II) complex thin film with an Ag reflective layer was carried out using a 406.7 nm blue-violet laser and a high numerical aperture (NA) of 0.90. Clear recording marks with high reflectivity contrast (>60%) at proper laser power and pulse width were obtained, and the size of recording mark was as small as 250 nm. The results indicate that these metal(II) complexes are promising organic recording medium for the blu-ray optical storage system

  4. Optical characterization and blu-ray recording properties of metal(II) azo barbituric acid complex films

    Li, X.Y. [Shanghai Institute of Optics and Fine Mechanics, Chinese Academy of Sciences, Shanghai 201800 (China)], E-mail: xyli@siom.ac.cn; Wu, Y.Q. [Shanghai Institute of Optics and Fine Mechanics, Chinese Academy of Sciences, Shanghai 201800 (China); Key Lab of Functional Inorganic Material Chemistry (Heilongjiang University), Ministry of Education, Haerbin 150080 (China)], E-mail: yqwu@siom.ac.cn; Gu, D.D.; Gan, F.X. [Shanghai Institute of Optics and Fine Mechanics, Chinese Academy of Sciences, Shanghai 201800 (China)

    2009-02-25

    Smooth thin films of nickel(II), cobalt(II) and zinc(II) complexes with azo barbituric acid were prepared by the spin-coating method. Absorption spectra of the thin films on K9 glass substrates in 300-700 nm wavelength region were measured. Optical constants (complex refractive index N = n + ik) of the thin films prepared on single-crystal silicon substrates in 275-695 nm wavelength region were investigated on rotating analyzer-polarizer type of scanning ellipsometer, and dielectric constant {epsilon} ({epsilon} = {epsilon}{sub 1} + i{epsilon}{sub 2}) as well as absorption coefficient {alpha} of thin films were calculated at 405 nm. In addition, static optical recording properties of the cobalt(II) complex thin film with an Ag reflective layer was carried out using a 406.7 nm blue-violet laser and a high numerical aperture (NA) of 0.90. Clear recording marks with high reflectivity contrast (>60%) at proper laser power and pulse width were obtained, and the size of recording mark was as small as 250 nm. The results indicate that these metal(II) complexes are promising organic recording medium for the blu-ray optical storage system.

  5. Study of iron (III) complexed with radiation grafted acrylic acid onto poly (tetrafluoroethylene-Co-perfluoro vinyl ether) films

    To introduce functional moieties to a poly (tetrafluoroethylene-Co-perfluoro vinyl ether) film (PFA) graft copolymerization of vinyl monomer such as acrylic acid (AAc) was attempted by a simultaneous technique in aqueous solution using γ-irradiation. The graft copolymer was complexed with the Fe (III) in aqueous solution. The grafted copolymer-metal complexes were examined by infrared (IR), ultraviolet (UV), energy-dispersive X-ray (EDX) and electron spin resonance (ESR) techniques. The effect of temperature on the trunk copolymer, untreated grafted and treated grafted copolymer films was examined by IR and thermogravimetric analysis (TGA). The overall results suggest octahedral environment for Fe (III) and revealed the high ability of the obtained ligand-metal complexes. Furthermore, scanning electron microscope (SEM) investigation of the grafted and modified films, both unheated and heated (200 degree C) showed changes in the structure and surface morphology. It was found that the modified grafted membranes may make them promising for some practical applications such as the recovery of metal from aqueous systems

  6. Complex chemical composition of colored surface films formed from reactions of propanal in sulfuric acid at upper troposphere/lower stratosphere aerosol acidities

    A. L. Van Wyngarden

    2014-11-01

    Full Text Available Particles in the upper troposphere and lower stratosphere (UT/LS consist mostly of concentrated sulfuric acid (40–80 wt % in water. However, airborne measurements have shown that these particles also contain a significant fraction of organic compounds of unknown chemical composition. Acid-catalyzed reactions of carbonyl species are believed to be responsible for significant transfer of gas phase organic species into tropospheric aerosols and are potentially more important at the high acidities characteristic of UT/LS particles. In this study, experiments combining sulfuric acid (H2SO4 with propanal and with mixtures of propanal with glyoxal and/or methylglyoxal at acidities typical of UT/LS aerosols produced highly colored surface films (and solutions that may have implications for aerosol properties. In order to identify the chemical processes responsible for the formation of the surface films, Attenuated Total Reflectance–Fourier Transform Infrared and 1H Nuclear Magnetic Resonance spectroscopies were used to analyze the chemical composition of the films. Films formed from propanal were a complex mixture of aldol condensation products, acetals and propanal itself. The major aldol condensation products were the dimer (2-methyl-2-pentenal and 1,3,5-trimethylbenzene, which was formed by cyclization of the linear aldol condensation trimer. Additionally, the strong visible absorption of the films indicates that higher order aldol condensation products must also be present as minor species. The major acetal species were 2,4,6-triethyl-1,3,5-trioxane and longer-chain linear polyacetals which are likely to separate from the aqueous phase. Films formed on mixtures of propanal with glyoxal and/or methylglyoxal also showed evidence for products of cross-reactions. Since cross-reactions would be more likely than self-reactions under atmospheric conditions, similar reactions of aldehydes like propanal with common aerosol organic species like glyoxal

  7. Complex chemical composition of colored surface films formed from reactions of propanal in sulfuric acid at upper troposphere/lower stratosphere aerosol acidities

    Van Wyngarden, A. L.; Pérez-Montaño, S.; Bui, J. V. H.; Li, E. S. W.; Nelson, T. E.; Ha, K. T.; Leong, L.; Iraci, L. T.

    2015-04-01

    Particles in the upper troposphere and lower stratosphere (UT/LS) consist mostly of concentrated sulfuric acid (40-80 wt%) in water. However, airborne measurements have shown that these particles also contain a significant fraction of organic compounds of unknown chemical composition. Acid-catalyzed reactions of carbonyl species are believed to be responsible for significant transfer of gas phase organic species into tropospheric aerosols and are potentially more important at the high acidities characteristic of UT/LS particles. In this study, experiments combining sulfuric acid (H2SO4) with propanal and with mixtures of propanal with glyoxal and/or methylglyoxal at acidities typical of UT/LS aerosols produced highly colored surface films (and solutions) that may have implications for aerosol properties. In order to identify the chemical processes responsible for the formation of the surface films, attenuated total reflectance-Fourier transform infrared (ATR-FTIR) and 1H nuclear magnetic resonance (NMR) spectroscopies were used to analyze the chemical composition of the films. Films formed from propanal were a complex mixture of aldol condensation products, acetals and propanal itself. The major aldol condensation products were the dimer (2-methyl-2-pentenal) and 1,3,5-trimethylbenzene that was formed by cyclization of the linear aldol condensation trimer. Additionally, the strong visible absorption of the films indicates that higher-order aldol condensation products must also be present as minor species. The major acetal species were 2,4,6-triethyl-1,3,5-trioxane and longer-chain linear polyacetals which are likely to separate from the aqueous phase. Films formed on mixtures of propanal with glyoxal and/or methylglyoxal also showed evidence of products of cross-reactions. Since cross-reactions would be more likely than self-reactions under atmospheric conditions, similar reactions of aldehydes like propanal with common aerosol organic species like glyoxal and

  8. A solid-state sensor based on ruthenium (II) complex immobilized on polytyramine film for the simultaneous determination of dopamine, ascorbic acid and uric acid

    Khudaish, Emad A., E-mail: ejoudi@squ.edu.om [Sultan Qaboos University, College of Science, Chemistry Department, PO Box 36, PC 123 Muscat (Oman); Al-Ajmi, Khawla Y. [Sultan Qaboos University, College of Science, Chemistry Department, PO Box 36, PC 123 Muscat (Oman); Al-Harthi, Salim H. [Sultan Qaboos University, College of Science, Department of Physics, PO Box 36, PC 123 Muscat (Oman)

    2014-08-01

    A solid-state sensor based on a polytyramine (Pty) film deposited on a glassy carbon electrode doped with a tris(2,2′-bipyridyl)Ru(II) complex (Ru/Pty/GCE) was constructed electrochemically. The surface morphology of the film modified electrode was characterized using electrochemical and surface scanning techniques. A redox property represented by a [Ru(bpy){sub 3}]{sup 3+/2+} couple immobilized at the Pty moiety was characterized using typical voltammetric techniques. A distinct Ru 3d peak obtained at 280.9 eV confirms doping of the Ru species onto the Pty moiety characterized by X-ray photoelectron (XPS). Atomic force microscopy (AFM) images demonstrate that incorporation of Ru decreases the surface roughness of the native Pty film modified electrode. The Ru/Pty/GCE exhibits efficient electrochemical sensing toward the oxidation of dopamine (DA), ascorbic acid (AA) and uric acid (UA) in their mixture. Three well-defined peaks were resolved with a large peak to peak separation and the detection limits of AA, DA and UA are brought down to 0.31, 0.08 and 0.58 μM, respectively. Interference studies and application for DA determination in real samples were conducted with satisfactory results. - Highlights: • XPS data confirm doping of ruthenium onto the polytyramine moiety. • The voltammetric signals of ascorbic acid, dopamine and uric acid are well defined. • The sensor is stable and offers a large adsorption facility for all species. • The sensor is highly sensitive to dopamine oxidation. • The sensor is applied to a real sample with a satisfactory recovery percentage.

  9. A solid-state sensor based on ruthenium (II) complex immobilized on polytyramine film for the simultaneous determination of dopamine, ascorbic acid and uric acid

    A solid-state sensor based on a polytyramine (Pty) film deposited on a glassy carbon electrode doped with a tris(2,2′-bipyridyl)Ru(II) complex (Ru/Pty/GCE) was constructed electrochemically. The surface morphology of the film modified electrode was characterized using electrochemical and surface scanning techniques. A redox property represented by a [Ru(bpy)3]3+/2+ couple immobilized at the Pty moiety was characterized using typical voltammetric techniques. A distinct Ru 3d peak obtained at 280.9 eV confirms doping of the Ru species onto the Pty moiety characterized by X-ray photoelectron (XPS). Atomic force microscopy (AFM) images demonstrate that incorporation of Ru decreases the surface roughness of the native Pty film modified electrode. The Ru/Pty/GCE exhibits efficient electrochemical sensing toward the oxidation of dopamine (DA), ascorbic acid (AA) and uric acid (UA) in their mixture. Three well-defined peaks were resolved with a large peak to peak separation and the detection limits of AA, DA and UA are brought down to 0.31, 0.08 and 0.58 μM, respectively. Interference studies and application for DA determination in real samples were conducted with satisfactory results. - Highlights: • XPS data confirm doping of ruthenium onto the polytyramine moiety. • The voltammetric signals of ascorbic acid, dopamine and uric acid are well defined. • The sensor is stable and offers a large adsorption facility for all species. • The sensor is highly sensitive to dopamine oxidation. • The sensor is applied to a real sample with a satisfactory recovery percentage

  10. The effect of dual complexing agents of lactic and citric acids on the formation of sol-gel derived Ag–PbTiO3 percolative thin film

    Controlling the formation of conductive particles to be nano-scale is important for achieving percolation effect in metal dispersed thin film composite to contribute extraordinary dielectric properties required for miniaturization of electronic devices. In this paper, lactic acid (LA) and citric acid (CA) were used as dual complexing agents to prepare a typical Ag nanoparticle dispersed PbTiO3 (PTO) composite thin film by using a sol-gel method. The phase structure of the thin film and the coordination effect between complexing agent and metallic ions were investigated. It revealed that LA coordinated with Ti4+ and Pb2+ and CA coordinated with Ag+. Lead was fixed inside the gel network by LA and restricted to evaporate during heat treatment thus the pyrochlore phase was prevented from forming in the thin film. Ag+ was coordinated by CA and the diffusion and thus aggregation of silver during gelation and annealing process were weakened. Silver nanoparticles dispersed in the PTO matrix formed with dual complexing agents of LA and CA introduced during the preparation process. The composite thin film of perfect perovskite phase with silver nanoparticles embedded was obtained at the molar ratio of LA/lead = 0.5 and CA/lead = 0.5. The dielectric constant of the thin film with silver nanoparticles is 5 times higher than that without silver nanoparticles. - Highlights: • Ag nanoparticle–PbTiO3 percolative film with high dielectric property is prepared. • Evaporation of lead was prevented by coordinating Pb with lactic acid agent. • Dual complexing agents contribute block and pinning effects to form Ag nanoparticles

  11. Self-assembly and photoelectric properties of cerium complexes with 3,4,9,10-perylenetetracarboxylic acid on nanocrystalline TiO2 films

    王忠胜; 黄春辉; 李富友; 杨术明; 翁诗甫; 付小艺; 吴念祖; 奎热西; 刘凤琴; 钱海杰

    2001-01-01

    Self-assembled (SA) films (PMP, M = Ce3+ or Ce4+) of 3,4,9,10-perylenetetracarboxylic acid (PTA) on nanocrystalline TiO2 films with Ce3+ or Ce4+ as a bridge were fabricated and characterized with UV-Vis, IR, and XPS synchrotron radiation photoelectron spectroscopy (SRPES) which gave the HOMO energy levels for the SA films. It was shown that thin-layer sandwich-type solar cells based on these SA films possess good properties for photoelectric conversion. While PTA-loaded TiO2 electrode (P) generated 26.9% of incident monochromatic photon-to-electron conversion efficiency (IPCE), PMP-sensitized Ti02 electrodes yielded 55.8% and 39.1% for Ce4+ and Ce3+ respectively. PMP films can be considered as a kind of complexes whose HOMO energy levels were proved to be higher than that of film P, which is one of the major reasons for the increase in IPCE from film P to film PMP.

  12. Self-Assembled Film of Tb3+ and Poly(3-Thiophene Acetic Acid) via Layer-by-Layer Complexation Technique and Its Photoluminescence

    辛颢; 李富友; 黄岩谊; 黄春辉

    2002-01-01

    The layer-by-layer complexation technique of polymer and metal ion was successfully utilized to fabricate the ultrathin multilayer film of poly(3-thiophene acetic acid (PTAA) and Tb3+ ion by dipping the substrates alternatively in polymer and Tb3+ ion aqueous solutions. UV-vis measurement revealed that the absorbance has linearity with the bilayer number from layer to layer and the X-ray photoelectron spectrum (XPS) confirmed the existence of Tb3+ ion. The pH of both the polymer and TbCl3 solutions influence the thickness dramatically while the concentration of the solutions is not so sensitive. The luminescent spectrum of the complex film shows the characteristic emission of Tb3+ ion as well as the ligand indicating the formation of the complex.

  13. Acid diffusion through polymer films

    Zhang, P. Linda; Eckert, Andrew R.; Willson, C. Grant; Webber, Stephen E.; Byers, Jeffrey D.

    1997-07-01

    In order to perform 0.2 micrometer processes, one needs to study the diffusion of photoacid generators within the photoresist system, since diffusion during post exposure bake time has an influence on the critical dimension (CD). We have developed a new method to study the diffusion of photoacid generators within a polymer film. This new method is based on monitoring the change of the fluorescence intensity of a pH- sensitive fluorescent dye caused by the reaction with photoacid. A simplified version of this experiment has been conducted by introducing acid vapor to quench the fluorescence intensity of this pH sensor. A thin polymer film is spin cast onto the sensor to create a barrier to the acid diffusion process. During the acid diffusion process, the fluorescence intensity of this pH sensor is measured in situ, using excitation and emission wavelengths at 466 nm and 516 nm, respectively. Fluoresceinamine, the pH sensitive fluorescent dye, is covalently bonded onto the treated quartz substrate to form a single dye layer. Poly(hydroxystyrene) (Mn equals 13k, Tg equals 180 degrees Celsius) in PGMEA (5% - 18% by weight) is spin cast onto this quartz substrate to form films with varying thickness. The soft bake time is 60 seconds at 90 degrees Celsius and a typical film has a thickness of 1.4 micrometers. Trifluoroacetic acid is introduced into a small chamber while the fluorescence from this quartz window is observed. Our study focuses on finding the diffusion constant of the vaporized acid (trifluoroacetic acid) in the poly(hydroxystyrene) polymer film. By applying the Fick's second law, (It - Io)/(I(infinity ) - Io) equals erfc [L/(Dt)1/2] is obtained. The change of fluorescence intensity with respect to the diffusion time is monitored. The above equation is used for the data analysis, where L represents the film thickness and t represents the average time for the acid to diffuse through the film. The diffusion constant is calculated to be at the order of 10

  14. The effect of dual complexing agents of lactic and citric acids on the formation of sol-gel derived Ag–PbTiO{sub 3} percolative thin film

    Su, Yanbo; Hu, Tao; Tang, Liwen; Weng, Wenjian; Han, Gaorong; Ma, Ning; Du, Piyi, E-mail: dupy@zju.edu.cn

    2014-05-02

    Controlling the formation of conductive particles to be nano-scale is important for achieving percolation effect in metal dispersed thin film composite to contribute extraordinary dielectric properties required for miniaturization of electronic devices. In this paper, lactic acid (LA) and citric acid (CA) were used as dual complexing agents to prepare a typical Ag nanoparticle dispersed PbTiO{sub 3} (PTO) composite thin film by using a sol-gel method. The phase structure of the thin film and the coordination effect between complexing agent and metallic ions were investigated. It revealed that LA coordinated with Ti{sup 4+} and Pb{sup 2+} and CA coordinated with Ag{sup +}. Lead was fixed inside the gel network by LA and restricted to evaporate during heat treatment thus the pyrochlore phase was prevented from forming in the thin film. Ag{sup +} was coordinated by CA and the diffusion and thus aggregation of silver during gelation and annealing process were weakened. Silver nanoparticles dispersed in the PTO matrix formed with dual complexing agents of LA and CA introduced during the preparation process. The composite thin film of perfect perovskite phase with silver nanoparticles embedded was obtained at the molar ratio of LA/lead = 0.5 and CA/lead = 0.5. The dielectric constant of the thin film with silver nanoparticles is 5 times higher than that without silver nanoparticles. - Highlights: • Ag nanoparticle–PbTiO{sub 3} percolative film with high dielectric property is prepared. • Evaporation of lead was prevented by coordinating Pb with lactic acid agent. • Dual complexing agents contribute block and pinning effects to form Ag nanoparticles.

  15. Complex chemical composition of colored surface films formed from reactions of propanal in sulfuric acid at upper troposphere/lower stratosphere aerosol acidities

    Van Wyngarden, A. L.; Pérez-Montaño, S.; Bui, J. V. H.; Li, E. S. W.; Nelson, T.E.; Ha, K. T.; L. Leong; Iraci, L.T.

    2014-01-01

    Particles in the upper troposphere and lower stratosphere (UT/LS) consist mostly of concentrated sulfuric acid (40–80 wt %) in water. However, airborne measurements have shown that these particles also contain a significant fraction of organic compounds of unknown chemical composition. Acid-catalyzed reactions of carbonyl species are believed to be responsible for significant transfer of gas phase organic species into tropospheric ...

  16. Europium complexes with trifluoroacetic acid

    Synthesis conditions and spectra-luminescent properties of different-ligand europium complexes of the composition Eu (TFA)2x2D, where TFA = anion of trifluoroacetic acid, D = 1,10-phenanthroline, 2,2-dipyridyl, triphenylphosphinoxide, hexamethyl-phosphotriamide, were studied. The compounds prepared have been characterized by the methods of elementary chemical analysis, IR and luminescence spectroscopy. It is shown that in the complex compounds two methods of coordination of the acid residue functional groups are realized, i.e. monodentate and bridge functions. The compounds were tested for resistance to UV light effect and to heating in the air. Complex with 2,2-dipyridyl proved the most thermally stable complex in the series studied, its decomposition temperature being 240 deg C

  17. Growth of nitric acid hydrates on thin sulfuric acid films

    Iraci, Laura T.; Middlebrook, Ann M.; Wilson, Margaret A.; Tolbert, Margaret A.

    1994-05-01

    Type I polar stratospheric clouds (PSCs) are thought to nucleate and grow on stratospheric sulfate aerosols (SSAs). To model this system, thin sulfuric acid films were exposed to water and nitric acid vapors (1 - 3 × 10-4 Torr H2O and 1 - 2.5 × 10-6 Torr HNO3) and subjected to cooling and heating cycles. FTIR spectroscopy was used to probe the phase of the sulfuric acid and to identify the HNO3/H2O films that condensed. Nitric acid trihydrate (NAT) was observed to grow on crystalline sulfuric acid tetrahydrate (SAT) films. NAT also condensed in/on supercooled H2SO4 films without causing crystallization of the sulfuric acid. This growth is consistent with NAT nucleation from ternary solutions as the first step in PSC formation.

  18. Growth of nitric acid hydrates on thin sulfuric acid films

    Iraci, Laura T.; Middlebrook, Ann M.; Wilson, Margaret A.; Tolbert, Margaret A.

    1994-01-01

    Type I polar stratospheric clouds (PSCs) are thought to nucleate and grow on stratospheric sulfate aerosols (SSAs). To model this system, thin sulfuric acid films were exposed to water and nitric acid vapors (1-3 x 10(exp -4) Torr H2O and 1-2.5 x 10(exp -6) Torr HNO3) and subjected to cooling and heating cycles. Fourier Transform Infrared (FTIR) spectroscopy was used to probe the phase of the sulfuric acid and to identify the HNO3/H2O films that condensed. Nitric acid trihydrate (NAT) was observed to grow on crystalline sulfuric acid tetrahydrate (SAT) films. NAT also condensed in/on supercooled H2SO4 films without causing crystallization of the sulfuric acid. This growth is consistent with NAT nucleation from ternary solutions as the first step in PSC formation.

  19. Salicylic acid electrooxidation. A surface film formation

    Baturova, M.D.; Vedenjapin, A.; Baturova, M.M. [N.D. Zelinsky Inst. of Organic Chemistry, Russian Academy of Sciences, Moscow (Russian Federation); Weichgrebe, D.; Danilova, E.; Rosenwinkel, K.H. [Univ. of Hannover, Inst. of Water Quality and Waste Management Hannover (Germany); Skundin, A. [A.N. Frumkin Inst. of Electrochemistry, Russian Academy of Sciences, Moscow (Russian Federation)

    2003-07-01

    A possibility to use electrochemical treatment for salicylic acid (SA) removal from waste water was studied. It was found that SA can be oxidized at platinum anode with formation of harmless products. Features of anodic process, in particular, formation of solid film on anode surface as well as properties of the film were investigated. (orig.)

  20. Complexes of salicylic acid and its derivatives

    A generalization and systematization have been made of literature data on complexing of various elements, including beryllium, cadmium, boron, indium, rare-earth elements, actinides, and transition elements with salicylic acid and it derivatives (amino-, nitro- and halosalicylic acids). The effect of the position and nature of the substitute, in the case of salicylic acid derivatives, on the complexing process is discussed. Certain physicochemical properties of the complexes under consideration are described along with data indicative of their stability

  1. Electrophoretic deposition of tannic acid-polypyrrolidone films and composites.

    Luo, Dan; Zhang, Tianshi; Zhitomirsky, Igor

    2016-05-01

    Thin films of polyvinylpyrrolidone (PVP)-tannic acid (TA) complexes were prepared by a conceptually new strategy, based on electrophoretic deposition (EPD). Proof of concept investigations involved the analysis of the deposition yield, FTIR and UV-vis spectroscopy of the deposited material, and electron microscopy studies. The analysis of the deposition mechanism indicated that the limitations of the EPD in the deposition of small phenolic molecules, such as TA, and electrically neutral polymers, similar to PVP, containing hydrogen-accepting carbonyl groups, can be avoided. The remarkable adsorption properties of TA and film forming properties of the PVP-TA complexes allowed for the EPD of materials of different types, such as huntite mineral platelets and hydrotalcite clay particles, TiO2 and MnO2 oxide nanoparticles, multiwalled carbon nanotubes, TiN and Pd nanoparticles. Moreover, PVP-TA complexes were used for the co-deposition of different materials and formation of composite films. In another approach, TA was used as a capping agent for the hydrothermal synthesis of ZnO nanorods, which were then deposited by EPD using PVP-TA complexes. The fundamental adsorption and interaction mechanisms of TA involved chelation of metal atoms on particle surfaces with galloyl groups, π-π interactions and hydrogen bonding. The films prepared by EPD can be used for various applications, utilizing functional properties of TA, PVP, inorganic and organic materials of different types and their composites. PMID:26878711

  2. Ruthenium nitrosyl complexes in nitric acid solutions

    Nine nitrosyl ruthenium complexes have been separated and identified in aqueous solutions of nitric acid. The separation method was low temperature, gradient elution, reverse phase partition chromatography using tri-n-butyl phosphate on a kiesel gel 60 support using 106Ru labelled complexes in the nitric acid phase. The identification of the complexes was deduced from the relationships between the products of aquation and nitration and paper chromatography using both methyl-iso-propyl ketone and nitric acid-acetone elutions. The proportion of each complex at equilibrium in various concentrations of nitric acid have been measured. The rates of nitration in 10 M nitric acid, and of aquation in 0.45 M nitric acid have been determined at 00C. (author)

  3. Photoactive thin films of polycaprolactam doped with europium (III) complex using phenylalanine as ligand

    Santos Garcia, Irene Teresinha, E-mail: irene@iq.ufrgs.br [Departamento de Fisico-Quimica, Instituto de Quimica, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves 9500, Bairro Agronomia, CEP 91501-970, Porto Alegre, RS (Brazil); Velleda Ribeiro, Patricia; Silva Correa, Diogo; Neto da Cunha, Igor Michel; Lenin Villarreal Carreno, Neftali [Instituto de Quimica e Geociencias, Universidade Federal de Pelotas, Campus Capao do Leao, s/n. CEP 96010-900, Pelotas, RS (Brazil); Ceretta Moreira, Eduardo [PPGEE, Universidade Federal do Pampa, Campus Bage, Bage- RS (Brazil); Severo Rodembusch, Fabiano [Departamento de Quimica Organica, Instituto de Quimica, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves 9500, Bairro Agronomia, CEP 91501-970, Porto Alegre, RS (Brazil)

    2011-12-01

    A photoactive complex based on europium(III) using the amino acid phenylalanine as ligand was prepared and characterized. The obtained europium(III)/phenylalanine complex presents an effective energy transfer from ligands to the rare earth center. The observed photoluminescent behavior for europium(III)/phenylalanine complex was similar to the well known europium(III)/ acetyl-{beta}-acetonate hydrate. New photoactive polyamide thin films were prepared using polycaprolactam as host of these complexes. The structural characterizations of the films were studied through Rutherford backscattering (RBS), Fourier transform infrared (FTIR) and Raman spectroscopies. The polyamide films doped with the amino acid and acetyl-{beta}-acetonate rare earth complexes maintain the original photoluminescent behavior, narrow emission bands corresponding to transitions {sup 5}D{sub 0} {yields} {sup 7}F{sub 0-4}, which indicates that this polymer is an excellent host to these complexes.

  4. Complexation of americium with humic acid

    As a part of the interlaboratory comparison exercise for the complexation of humic acid and colloid generation (COCO-Club activities) in the CEC project MIRAGE-II, the complexation of americium with humic acid has been studied in our laboratory. Two humic acids were used for the study: Aldrich-HA(H+) which is a reference humic acid of the COCO-Club and Bradford-HA(H+) from Lake Bradford, Florida. A wide concentration range of humic acid and different ratios of Am to humic acid have been investigated between pH 5 and 6 with the ionic strength of 0.1 M and 1.0 M. The complexation has been studied by UV-spectroscopy, Laser-induced Photoacoustic Spectroscopy (LPAS) and ultrafiltration. LPAS is used for the submicromolar concentration range where the sensitivity of UV spectroscopy is not accessible. Ultrafiltration is used for low Am to humic acid ratios where both spectroscopic methods are not applicable. Varying the humic acid concentration over three orders of magnitude, only a 1:1 type of binding is observed. No significant variation of the stability constant is found in the investigated range of pH and ionic strength. However, the precipitation tendency and the loading capacity of humic acid are found to depend sensitively on pH and ionic strength. The complexation study provides a deep insight into the influence of humic acid on the migration behaviour of fission products and actinides in the geosphere. (orig.)

  5. Influence of complexing agent on the growth of chemically deposited Ni3Pb2S2 thin films

    Ho Soonmin

    2014-09-01

    Full Text Available Ni3Pb2S2 thin films were prepared by chemical bath deposition method. Here, the objective of this research was to investigate the influence of complexing agent on the properties of films.These films were characterized using atomic force microscopy, UV-Visible spectro photometer and X-ray diffraction. It was found that, as the concentration of tartaric acid increased, film thickness increased, but, the band gap reduced. For the films prepared using 0.1M of tartaric acid, the films were uniform and completely covered the substrates.

  6. Characterization and complexation of humic acid

    This paper summarizes the research contributions to the CEC project MIRAGE II, particularly the research area: complexation and colloids (COCO). The first part of the paper comprises the characterization of humic and fulvic acids from different origins: a commercial product from Aldrich Co. used as a reference humic acid and site specific humic acids from Gorleben (FRG), Boom Clay (B) and Fanay Augeres (F) aquifer systems. The second part includes the complexation of trivalent actinides: Am(III) and Cm(III) with various humic acids. A number of different methods have been applied for the complexation study: spectrophotometry, ultrafiltration, laser-indused photoacoustic spectroscopy (LPAS) and time resolved laser fluorescence spectroscopy (TRLFS). The evaluation process of complexation constant is discussed extensively and the well consolidated results are presented, which can be directly used for the geochemical modelling of the radionuclide migration. (orig.)

  7. Complex coacervates of hyaluronic acid and lysozyme

    Water, Jorrit J.; Schack, Malthe M.; Velazquez-Campoy, Adrian;

    2014-01-01

    Complex coacervates of hyaluronic acid and lysozyme, a model protein, were formed by ionic interaction using bulk mixing and were characterized in terms of binding stoichiometry and protein structure and stability. The complexes were formed at pH 7.2 at low ionic strength (6 mM) and the binding...... stoichiometry was determined using solution depletion and isothermal titration calorimetry. The binding stoichiometry of lysozyme to hyaluronic acid (870 kDa) determined by solution depletion was found to be 225.9 ± 6.6 mol, or 0.1 bound lysozyme molecules per hyaluronic acid monomer. This corresponded well...... with that obtained by isothermal titration calorimetry of 0.09 bound lysozyme molecules per hyaluronic acid monomer. The complexation did not alter the secondary structure of lysozyme measured by Fourier-transform infrared spectroscopy overlap analysis and had no significant impact on the Tm of...

  8. Complex film of chitosan and carboxymethyl cellulose nanofibers.

    Kawasaki, Takuma; Nakaji-Hirabayashi, Tadashi; Masuyama, Kazuhira; Fujita, Satoshi; Kitano, Hiromi

    2016-03-01

    A polymer film composed of a mixture of chitosan (Ch) and carboxymethyl cellulose sodium salt (CMC) nanofibers was deposited on a glass surface. The thin film of the Ch-CMC mixture obtained was stable, and fibroblast adhesion to the film was lowest when the weight ratio of Ch to CMC was 4:6. The ζ-potential and contact angle of the mixture film indicated that a polyion complex of Ch and CMC was formed. The mechanical strength of the film composed of Ch-CMC nanofiber complexes was much higher than that of the film composed of Ch-water-soluble CMC complexes (non-nanofiber), likely because the entanglement of nanofibers was enhanced by electrostatic attractions. These results indicate that the charge-neutralized nanofiber film was highly effective in suppressing cell adhesion and therefore is a promising material for biomedical applications. PMID:26700238

  9. Methods for producing complex films, and films produced thereby

    Duty, Chad E.; Bennett, Charlee J. C.; Moon, Ji -Won; Phelps, Tommy J.; Blue, Craig A.; Dai, Quanqin; Hu, Michael Z.; Ivanov, Ilia N.; Jellison, Jr., Gerald E.; Love, Lonnie J.; Ott, Ronald D.; Parish, Chad M.; Walker, Steven

    2015-11-24

    A method for producing a film, the method comprising melting a layer of precursor particles on a substrate until at least a portion of the melted particles are planarized and merged to produce the film. The invention is also directed to a method for producing a photovoltaic film, the method comprising depositing particles having a photovoltaic or other property onto a substrate, and affixing the particles to the substrate, wherein the particles may or may not be subsequently melted. Also described herein are films produced by these methods, methods for producing a patterned film on a substrate, and methods for producing a multilayer structure.

  10. Preparation and Properties of Vegetable-Carboxymethylcellulose (CMC) Complex FilmsЦ Water Bamboo-CMC,Chinese Cabbage-CMC etc.Complex Films

    2007-01-01

    1 Results Various kinds of biodegradable polymers have been researched[1].In our previous papers,cellulose-alginic acid[2],cellulose-agar[3],vegetable-carboxymethylcellulose (CMC) etc.complex films have been researched.Recently,some other kinds of vegetable such as water bamboo,Chinese cabbage,eggplant,spinach,naked oats,and basella,asparagus and pumpkin were used to perpare vegetable-CMC complex films.Every kind of vegetable has different content of water,cellulose,protein,carbohydrate and a small amou...

  11. Catalytically active cobalt and copper complexes in polyelectrolyte multilayer films

    In this work an approach to obtain effective and easy reusable heterogeneous catalyst, LbL deposition of polyelectrolytes followed by covalently binding with cobalt (II) and copper (II) ions were described. Immobilization of metal complexes via covalent attachment to insoluble template is an attractive method to facilitate catalyst recovery, recycling. The reaction in the heterogeneous catalysis goes in the interface of catalyst and reaction solution and it is important to create a catalyst with large surface area. We have used polycations as polyethyleneimine (BPEI), quaternized poly(4- vynilpyridine) (QPVP) and polyanions as poly(acrylic acid) (PAA), poly(styrene sulphonate) sodium salt (PSS) and the electrostatic layer-by-layer assembly technique to make uniform thin film coating on SiO2 nanoparticles and glass slides with controllable thickness, roughness and mechanically durability. The stability of metals within multilayers in reaction condition were tested. We compared the amount of metal in PEMs of different polyelectrolytes. The stability constants of complex forming processes of the polymer-metal complexes in water and in alcohol were calculated by modified method of Bjerrum. Catalytic activity of immobilized catalysts was investigated for oxidation of toluene by molecular oxygen. Catalysts were separated from reaction mixture easily and had been used for this reaction five times without significant loss of activity. Key words: catalysis, layer-by-layer (LbL), polymer-metal complexes, oxidation, cobalt and copper immobilization

  12. A Complexity View of Acid Deposition

    朱建林; 方见树

    2003-01-01

    We show that acid deposition is analogous to complex systems composed of a series of interconnected components.Frequency-size distributions of weekly hydrogen deposition (WHD) of precipitation are consistent with double power-law in two different regimes separated by a crossover WHD. The distribution of variations in acid deposition over a week interval is remarkably symmetrical, with long tail extending over eight orders of magnitude. The acid deposition fluctuations exhibit fractal Brown motion with two different temporal scaling regimes and long-range correlation exists in the series. The power-laws in the acid deposition dynamics are considered to be indicators of seff-organization of atmosphere under environmental pollution stress.

  13. Sprayed films of europium complexes toward light conversion devices

    Rare-earth complexes have become subject of intensive research due to the high quantum efficiency of their emission, very narrow bands, and excellent fluorescence monochromaticity. The chemical design and characterization of Eu complexes based on β-diketone ligands hexafluoroacetylacetate (hfac) and dibenzoylmetanate (dbm) is reported here. K[Eu(dbm)4] and K[Eu(hfac)4] complexes were immobilized as thin films by using the spray technique, a promising methodology for practical applications. The latter provides not only a faster layer deposition but also larger coated areas compared to conventional methods, such as layer-by-layer (LbL) and Langmuir–Blodgett (LB). The growth of the sprayed films was monitored through microbalance (QCM) and ultraviolet–visible (UV–Vis) absorption spectroscopy, which reveal a higher mass and absorbance per deposited layer of K[Eu(dbm)4] film. Micro-Raman images display a more homogeneous spatial distribution of the K[Eu(dbm)4] complex throughout the film, when compared to K[Eu(hfac)4] film. At nanometer scale, atomic force microscopy (AFM) images indicate that the roughness of the K[Eu(hfac)4] film is approximately one order of magnitude higher than that for the K[Eu(dbm)4] film, which pattern is kept at micrometer scale according to micro-Raman measurements. The photoluminescence data show that the complexes remain as pure red emitters upon spray immobilization. Besides, the quantum efficiency for the sprayed films are found equivalent to the values achieved for the powders, highlighting the potential of the films for application in light conversion devices. - Highlights: • Rare earth complexes thin films based on β-diketone ligands. • Spraying procedures to fabricate layer-by-layer (LbL) luminescent thin films. • Chemical design of Eu complexes based on hfac and dbm β-diketones ligands immobilized as sprayed films. • Pure red emitters upon spray immobilization. • Sprayed luminescent thin films for potential

  14. Oral absorption of hyaluronic acid and phospholipids complexes in rats

    Si-Ling Huang; Pei-Xue Ling; Tian-Min Zhang

    2007-01-01

    AIM: To prepare a complex of hyaluronic acid (HA) and phospholipids (PL), and study the improvement effect of PL on the oral absorption of HA.METHODS: The complex of HA-PL (named Haplex) was prepared by film dispersion and sonication method, its physico-chemical properties were identified by infrared spectra and differential scanning calorimetry (DSC). The oral absorption of Haplex was studied. Thirty-two healthy rats were divided into 4 groups randomly: (1) a normal saline (NS) control group; (2) an HA group; (3) a mixture group and (4) a Haplex group. After intragastric administration, the concentration of HA in serum was determined.RESULTS: The physico-chemical properties of Haplex were different from HA or PL or their mixture. After Haplex was administered to rats orally, the serum concentration of HA was increased when compared with the mixture or HA control groups from 4 h to 10 h (P < 0.05). The ΔAUCo-12 h of Haplex was also greater than that of the other three groups (P < 0.05).CONCLUSION: The method of film dispersion and sonication can prepare HA and PL complex, and PL can enhance the oral absorption of exogenous HA.

  15. Complex Pharmacology of Free Fatty Acid Receptors

    Milligan, Graeme; Shimpukade, Bharat; Ulven, Trond;

    2016-01-01

    G protein-coupled receptors (GPCRs) are historically the most successful family of drug targets. In recent times it has become clear that the pharmacology of these receptors is far more complex than previously imagined. Understanding of the pharmacological regulation of GPCRs now extends beyond...... pharmacology have shaped understanding of the complex pharmacology of receptors that recognize and are activated by nonesterified or "free" fatty acids (FFAs). The FFA family of receptors is a recently deorphanized set of GPCRs, the members of which are now receiving substantial interest as novel targets for...... the treatment of metabolic and inflammatory diseases. Further understanding of the complex pharmacology of these receptors will be critical to unlocking their ultimate therapeutic potential....

  16. Formation of complex anodic films on porous alumina matrices

    Alexander Zahariev; Assen Girginov

    2003-04-01

    The kinetics of growth of complex anodic alumina films was investigated. These films were formed by filling porous oxide films (matrices) having deep pores. The porous films (matrices) were obtained voltastatically in (COOH)2 aqueous solution under various voltages. The filling was done by re-anodization in an electrolyte solution not dissolving the film. Data about the kinetics of re-anodization depending on the porosity of the matrices were obtained. On the other hand, the slopes of the kinetic curves during reanodization were calculated by two equations expressing the dependence of these slopes on the ionic current density. A discrepancy was ascertained between the values of the calculated slopes and those experimentally found. For this discrepancy a possible explanation is proposed, related to the temperature increase in the film, because of that the real current density significantly increases during re-anodization.

  17. Lactic Acid and Biosurfactants Production from Residual Cellulose Films.

    Portilla Rivera, Oscar Manuel; Arzate Martínez, Guillermo; Jarquín Enríquez, Lorenzo; Vázquez Landaverde, Pedro Alberto; Domínguez González, José Manuel

    2015-11-01

    The increasing amounts of residual cellulose films generated as wastes all over the world represent a big scale problem for the meat industry regarding to environmental and economic issues. The use of residual cellulose films as a feedstock of glucose-containing solutions by acid hydrolysis and further fermentation into lactic acid and biosurfactants was evaluated as a method to diminish and revalorize these wastes. Under a treatment consisting in sulfuric acid 6% (v/v); reaction time 2 h; solid liquid ratio 9 g of film/100 mL of acid solution, and temperature 130 °C, 35 g/L of glucose and 49% of solubilized film was obtained. From five lactic acid strains, Lactobacillus plantarum was the most suitable for metabolizing the glucose generated. The process was scaled up under optimized conditions in a 2-L bioreactor, producing 3.4 g/L of biomass, 18 g/L of lactic acid, and 15 units of surface tension reduction of a buffer phosphate solution. Around 50% of the cellulose was degraded by the treatment applied, and the liqueurs generated were useful for an efficient production of lactic acid and biosurfactants using L. plantarum. Lactobacillus bacteria can efficiently utilize glucose from cellulose films hydrolysis without the need of clarification of the liqueurs. PMID:26293409

  18. Characterization and bacterial adhesion of chitosan-perfluorinated acid films.

    Bierbrauer, Karina L; Alasino, Roxana V; Muñoz, Adrián; Beltramo, Dante M; Strumia, Miriam C

    2014-02-01

    We reported herein the study and characterization of films obtained by casting of chitosan solutions in perfluorinated acids, trifluoroacetic (TFA), perfluoropropionic (PFPA), and perfluorooctanoic (PFOA). The films were characterized by FTIR, solid state (13)C NMR, X-ray, AFM, contact angle, thermogravimetric effluent analysis by mass spectrometry, and rheology. The results showed a marked influence of chain length of the perfluorinated acids on the hydrophobic/hydrophilic ratio of the modified chitosan films which was evidenced by the different characteristics observed. The material that showed greater surface stability was chitosan-PFOA. Chitosan film with the addition of PFOA modifier became more hydrophobic, thus water vapor permeability diminished compared to chitosan films alone, this new material also depicted bacterial adhesion which, together with the features already described, proves its potential in applications for bioreactor coating. PMID:24189195

  19. Biotransformation of plutonium complexed with citric acid

    Francis, A.J.; Dodge, C.J.; Gillow, J.B. [Environmental Sciences Department, Brookhaven National Laboratory, Upton, New York, 11973 (United States)

    2005-07-01

    Full text of publication follows: The presence of organic ligands in radioactive wastes is a major concern because of the potential for increasing the transport of radionuclides from disposal sites. Microorganisms present in radioactive wastes can affect the long-term stability of radionuclides associated with organic ligands. Biotransformation of radionuclides complexed with organic ligands should result in the precipitation of the radionuclides and retard their migration. In this study we investigated the biotransformation of {sup 242}Pu{sup 4+} (10{sup -8} to 10{sup -5} M) in the presence of equimolar and excess citric acid by Pseudomonas fluorescens. Analysis of {sup 242}Pu-citrate by electro-spray ionization-mass spectrometry (ESI-MS) indicated the presence of a bi-ligand Pu-cit{sub 2} complex. Analysis of Th-citrate complex, an analog for Pu-citrate, indicated the formation of a 2:3 complex. Citric acid under aerobic conditions was metabolized by P. fluorescens at a rate of 4.9 {mu}M/h, and decreased to 4.0 and 3.8 {mu}M/h in the presence of 10{sup -8} and 10{sup -6} M of Pu, respectively. The pH of the medium containing citric acid alone increased from 6.5 to 7.1, while the pH of the samples containing Pu increased from 6.8 to 7.9. The high ionic strength (0.9 M) of the medium reduced citric acid metabolism by 50% in comparison to 0.1 M ionic strength. Initially, Pu added to the growth medium as Pu-citrate remained in solution as Pu{sup 4+}. Selective solvent extraction by thenyl-tri-fluoro-acetone (TTA) as well as micro-filtration (0.03 {mu}m) of the medium after biodegradation studies indicated that Pu was present as the polymeric form. The Pu polymer formation was dependent on the Pu:citrate ratio as well as the extent of citrate metabolism. The high ionic strength solution containing 10{sup -5} M 1:1 Pu-citrate complex showed only 27% citrate degradation but had the highest percentage ({approx}80%) of polymer formation, suggesting the Pu was soluble only

  20. Biotransformation of plutonium complexed with citric acid

    Full text of publication follows: The presence of organic ligands in radioactive wastes is a major concern because of the potential for increasing the transport of radionuclides from disposal sites. Microorganisms present in radioactive wastes can affect the long-term stability of radionuclides associated with organic ligands. Biotransformation of radionuclides complexed with organic ligands should result in the precipitation of the radionuclides and retard their migration. In this study we investigated the biotransformation of 242Pu4+ (10-8 to 10-5 M) in the presence of equimolar and excess citric acid by Pseudomonas fluorescens. Analysis of 242Pu-citrate by electro-spray ionization-mass spectrometry (ESI-MS) indicated the presence of a bi-ligand Pu-cit2 complex. Analysis of Th-citrate complex, an analog for Pu-citrate, indicated the formation of a 2:3 complex. Citric acid under aerobic conditions was metabolized by P. fluorescens at a rate of 4.9 μM/h, and decreased to 4.0 and 3.8 μM/h in the presence of 10-8 and 10-6 M of Pu, respectively. The pH of the medium containing citric acid alone increased from 6.5 to 7.1, while the pH of the samples containing Pu increased from 6.8 to 7.9. The high ionic strength (0.9 M) of the medium reduced citric acid metabolism by 50% in comparison to 0.1 M ionic strength. Initially, Pu added to the growth medium as Pu-citrate remained in solution as Pu4+. Selective solvent extraction by thenyl-tri-fluoro-acetone (TTA) as well as micro-filtration (0.03 μm) of the medium after biodegradation studies indicated that Pu was present as the polymeric form. The Pu polymer formation was dependent on the Pu:citrate ratio as well as the extent of citrate metabolism. The high ionic strength solution containing 10-5 M 1:1 Pu-citrate complex showed only 27% citrate degradation but had the highest percentage (∼80%) of polymer formation, suggesting the Pu was soluble only in the presence of excess citric acid. However, the extensive

  1. 21 CFR 172.315 - Nicotinamide-ascorbic acid complex.

    2010-04-01

    ... 21 Food and Drugs 3 2010-04-01 2009-04-01 true Nicotinamide-ascorbic acid complex. 172.315 Section... HUMAN CONSUMPTION Special Dietary and Nutritional Additives § 172.315 Nicotinamide-ascorbic acid complex. Nicotinamide-ascorbic acid complex may be safely used in accordance with the following prescribed...

  2. Influence of citric acid on the morphology and magnetic properties of barium ferrite thin films

    Hexagonal barium ferrite (BaFe12O19) thin films were fabricated by spin coating of precursors from sol-gel methods. Different amount of citric acid was added. Weight loss and changes of chemical bonds during the heat treatment below 500 deg. C were recorded by thermogravity analyzer and Fourier transform infrared spectroscopy, respectively. The morphology of the films, i.e. the amount of acicular crystallites in the film, was controlled by adjusting the quantity of citric acid. The X-ray diffraction shows that the films are c-axis oriented, but the crystallization is less perfect with the increase of the citric acid. With the increase of the citric acid, the percentage of the acicular crystallites increased. At the same time, the coercivity force increased. The acicular crystallites were not exchange-coupled to the platelet crystallites. The citric acid was understood to form complex with iron ions and accelerate the exothermal auto-combustion. The c-axis oriented growth of the film was thus deteriorated.

  3. Complex formation of calcium with humic acid and polyacrylic acid

    In order to understand the migration behavior of radionuclides in the underground, it is also important to estimate the effect of the competing cations originally present in the groundwater. In this connection, the complexation of Ca(II) with Aldrich humic acid has been examined. For the study at trace concentrations (∝ 10-10 M) of Ca(II), the solvent extraction of 45Ca with TTA and TOPO in cyclohexane has been used. At macro concentrations (10-4 M) of Ca(II), the measurement of the free Ca2+ ion concentration with a calcium selective electrode has been conducted. To estimate the polyelectrolyte effect of humic acid separately from its heterogeneous composition effect, polyacrylic acid ([-CH2CH(COOH)-]n) has been selected as a representative of the homogeneous polymeric weak acids and its complexation with Ca(II) has also been examined. The values of log βα have been obtained at pH 5 ∝ 7 in 0.1, 0.4 and 1.0 M NaCl, where βα is the apparent formation constants defined by βα = [ML]/([M][R]). In this definition, [ML] and [M] are the concentrations of bound and free Ca2+ respectively, [R] is the concentration of dissociated proton exchanging sites. log βα of humate decreases from 2.19 ∝ 2.92 (depending on pH and ionic strength 1.0 α of polyacrylate (1.36 ∝ 3.24 for I = 0.1 ∝ 1.0). For both humate and polyacrylate, log βα decreases linearly with log[Na+], where [Na+] is the bulk concentration of sodium ion. Their dependences of log βα on ionic strength are stronger than those of log β of monomeric carboxylates such as oxalate and EDTA, indicating the large electrostatic effect of crowded negative charges on the macromolecules of humic or polyacrylic acid. (orig.)

  4. Comparison of topotactic fluorination methods for complex oxide films

    Moon, E. J., E-mail: em582@drexel.edu; Choquette, A. K.; Huon, A.; Kulesa, S. Z.; May, S. J., E-mail: smay@coe.drexel.edu [Department of Materials Science and Engineering, Drexel University, Philadelphia, Pennsylvania 19104 (United States); Barbash, D. [Centralized Research Facilities, Drexel University, Philadelphia, Pennsylvania 19104 (United States)

    2015-06-01

    We have investigated the synthesis of SrFeO{sub 3−α}F{sub γ} (α and γ ≤ 1) perovskite films using topotactic fluorination reactions utilizing poly(vinylidene fluoride) as a fluorine source. Two different fluorination methods, a spin-coating and a vapor transport approach, were performed on as-grown SrFeO{sub 2.5} films. We highlight differences in the structural, compositional, and optical properties of the oxyfluoride films obtained via the two methods, providing insight into how fluorination reactions can be used to modify electronic and optical behavior in complex oxide heterostructures.

  5. Comparison of topotactic fluorination methods for complex oxide films

    E. J. Moon

    2015-06-01

    Full Text Available We have investigated the synthesis of SrFeO3−αFγ (α and γ ≤ 1 perovskite films using topotactic fluorination reactions utilizing poly(vinylidene fluoride as a fluorine source. Two different fluorination methods, a spin-coating and a vapor transport approach, were performed on as-grown SrFeO2.5 films. We highlight differences in the structural, compositional, and optical properties of the oxyfluoride films obtained via the two methods, providing insight into how fluorination reactions can be used to modify electronic and optical behavior in complex oxide heterostructures.

  6. Fabrication of Superhydrophobic and Luminescent Rare Earth/Polymer complex Films.

    Wang, Zefeng; Ye, Weiwei; Luo, Xinran; Wang, Zhonggang

    2016-01-01

    The motivation of this work is to create luminescent rare earth/polymer films with outstanding water-resistance and superhydrophobicity. Specifically, the emulsion polymerization of styrene leads to core particles. Then core-shell-structured polymer nanoparticles are synthesized by copolymerization of styrene and acrylic acid on the core surface. The coordination reaction between carboxylic groups and rare earth ions (Eu(3+) and Tb(3+)) generates uniform spherical rare earth/polymer nanoparticles, which are subsequently complexed with PTFE microparticles to obtain micro-/nano-scaled PTFE/rare earth films with hierarchical rough morphology. The films exhibit large water contact angle up to 161° and sliding angle of about 6°, and can emit strong red and green fluorescence under UV excitation. More surprisingly, it is found that the films maintain high fluorescence intensity after submersed in water and even in aqueous salt solution for two days because of the excellent water repellent ability of surfaces. PMID:27086735

  7. SURFACE OF GELATIN MODIFIED POLY(L-LACTIC ACID) FILM

    Xin Hou; Bao-long Zhang; Feng She; Yuan-lu Cui; Ke-yu Shi; Kang-de Yao

    2003-01-01

    In this paper, the surface structure of poly(L-lactic acid) (PLLA) film modified with gelatin was investigated. The PLLA film specimens were treated directly with aqueous alkali solution to provide their surfaces with carboxyl groups, so that these functional groups could become the reactive sites for gelatin immobilization. The functional groups of the PLLA films were identified by ATR-FTIR spectra and XPS spectra, the changes in surface morphology were observed by using environmental scanning electron microscopy (ESEM), and the hydrophilicity of modified PLLA films was examined by water contact angle measurement. Experimental results showed that the gelatin was immobilized with water-soluble carbodiimide (EDC) onto the PLLA film's surfaces, and the gelatin content on the polymer surface was related to carboxylic group formed in the controlled hydrolysis process. Rough surfaces caused by hydrolysis will predominantly favor the adhesion and growth of cell; and the hydrophilicity of these surfaces after the modification procedure is enhanced.

  8. Partly Imidized Polyamic Acid and Its Uniaxial Stretched Polyimide Films

    MA Peng-chang; HOU Yong

    2013-01-01

    Partly imidized polyamic acid(PAA) has been used to prepare high performance polyimide films.The behaviors of two polyamic acids derived from pyromellitic dianhydride(PMDA)/4,4'-oxydianiline(ODA) and 3,Y,4,4'-biphenyltetracarboxylic diahhydride(BPDA)/paraphenylenediamine(PPD) containing dehydrating agents composed of acetic anhydride and a tertiary amine as the catalyst were investigated.The gel point was dependent on imidization degree in despite of temperature and the molar ratio of catalyst to acetic acid.Imdization content was about 35% for PMDA/ODA and about 22% for BPDA/PPD.The effect of catalyst on imidization possessed an order of triethylamine>3-methylpyridine>pyridine>isoquinoline>2-methylpyridine.The stretching of the films greatly reduced the coefficient of linear thermal expansion(CTE) either in the longitudinal direction or transversal direction.Compared to the film from polyamic acid,the partly imidized film had greater stretching ratio,so that the uniaxial stretched polyimide film from partly imidized PAA had higher tensile strength and tensile modulus,but lower elongation in the stretching direction.

  9. Ni(II) complexes of dithiophosphonic acids

    Afshin Saadat; Alireza Banaee; Patrick McArdle; Karim Zare; Khodayar Gholivand; Ali Asghar Ebrahimi Valmoozi

    2014-07-01

    The reaction of 2,4-bis(4-methoxyphenyl)-1,3,2,4-dithiadiphosphetane-2,4-disulfide (Lawesson reagent) with isobutanol, cyclohexylamine and phenylethylamine produced (4-methoxy-phenyl)-phosphonodithioic acid o-isobutyl ester HS2P(p-C6H4OMe) (OCH2CH(CH3)2) (I), [S2P(C6H11NH)(p-C6H4OMe) H3N+C6H11] (II) and [S2P(phCH2CH2NH) (p-C6H4OMe)H3N+CH2CH2ph] (III), respectively. The reaction of alcohol with Lawesson reagent produced neutral product (I) while that with amines led to an ion pair (II, III). Furthermore, reaction of I, II and III with NiCl2.6H2O in methanol produced novel complexes: IV, V and VI. The compounds were characterized by 1H, 13C and 31P NMR, IR spectroscopy and elemental analysis. The single crystal X-ray structures of IV and V showed that the nickel complexes are square planar. Compound V formed a three-dimensional supramolecular structure via intermolecular P-O…H-N hydrogen bonds. The Xray crystallography of V showed that those three hydrogens of +NH3 cation produced three hydrogen bonds with different distances. The new compounds were additionally tested in view of their anti-bacterial properties. The ligands containing amine substituents exhibited more activity toward tested bacteria than their alcohol substituents, while the Ni(II) complexes including alcohol substituents exhibited high potential.

  10. Gelatin-Pectin Composite Films from Polyion Complex Hydrogels

    Composite films from gelatin and low-methoxyl pectin were prepared by either ionic complexation or covalent cross-linking. The ionic interactions between positively charged gelatin and negatively charged pectin produced physically reversible hydrogels. The resultant homogeneous gels had improved mec...

  11. Surface investigation of chitosan film with fatty acid monolayers

    Esam A. El-hefian

    2009-05-01

    Full Text Available The surface pressure- molecular area (-A isotherm curves of two fatty acids of different chain lengths, i.e. stearic (C18 and arachidic (C20 acids, were obtained by using Langmuir-Blodgett (LB technique. Results showed clear isotherm plots with limiting mean molecular area around 21 Å2 for both acids. However, the monolayer was found to collapse at higher than 33 mN m-1 and 21 mN m-1 for stearic acid and arachidic acid respectively. The effect of Langmuir-Blodgett monolayers of the acids was investigated by atomic force microscopy (AFM. Chitosan film, before and after dipping in water, was also studied by means of AFM so that it could be used for comparison. It was found that the surface of chitosan was more homogeneous and smoother after dipping in water. In addition, more homogeneous surfaces were achieved after transferring a layer of the fatty acid onto the substrate.

  12. Occurrence of single-electron phenomenon in CdS nanoclusters in Langmuir-Blodgett films of -octadecyl succinic acid

    G Hemakanthi; Aruna Dhathathreyan

    2002-10-01

    Cadmium complex of -octadecyl succinic acid (ODSA) in Langmuir films at air/water interface has been studied using surface pressure-molecular area ( - ) and surface potential-molecular area ( - ) isotherms. The metal complex formed, transferred as LB film onto solid substrates, was analysed using FT-IR and was subjected to sulphidation reaction. Antisymmetric and symmetric carboxylate stretching vibrations have been used to determine the nature of the ODSA/cation complexes. CdS formed after sulphidation of the cadmium complex (ODSACd) showed possible single-electron phenomenon indicating the nanosized nature of clusters formed. Atomic Force Microscopy (AFM) measurements carried out confirmed the size of these CdS clusters.

  13. Characterization of nanostructured As{sub 2}S{sub 3} thin films synthesized at room temperature by chemical bath deposition method using various complexing agents

    Ubale, Ashok U., E-mail: ashokuu@yahoo.com; Kantale, J.S.; Choudhari, D.M.; Mitkari, V.N.; Nikam, M.S.; Belkhedkar, M.R.

    2013-09-02

    Nanostructured binary As{sub 2}S{sub 3} thin films were deposited onto glass substrates by chemical bath deposition method from complexed and uncomplexed baths using complexing agents acetic acid, ethylenediaminetetraacetic acid, oxalic acid and tartaric acid. The effect of complexing agent on structural, electrical, morphological and optical properties of As{sub 2}S{sub 3} is reported. The synthesized films were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), electrical resistivity and optical absorption measurements. The deposited films are nanocrystalline in nature with monoclinic lattice. The films deposited from uncomplexed bath and from ethylenediaminetetraacetic acid complexes are non-porous and become porous for other complexes. The electrical resistivity and optical band gap is also found complex dependent. - Highlights: • Nanocrystalline n-type As{sub 2}S{sub 3} films were grown by chemical bath deposition method. • Effect of complex on structural, electrical and optical properties was reported. • The film morphology highly depends on complex used in deposition process.

  14. Thin films of perovskite-type complex oxides

    Hanns-Ulrich Habermeier

    2007-10-01

    Full Text Available Complex oxides represent a class of materials with a plethora of fascinating, intrinsic physical functionalities. The intriguing interplay of charge, spin, and orbital ordering in these systems superimposed by lattice effects opens a scientifically rewarding playground for both fundamental and application-oriented research. In particular, the possibility of externally modifying the properties of thin-film complex oxides by epitaxial strain or artificial boundaries, and thus potentially generating novel properties at the interfaces between films, opens a new perspective. Here, the development of physical vapor deposition based preparation technologies for complex oxide thin films is reviewed, with examples taken from current research in high-temperature superconducting cuprates, magnetically ordered manganites, and Na–cobaltates. It covers the main trends of in situ process and growth control to fabricate single-crystal, single-layer thin films, heterostructures, and superlattices. Furthermore, using the combination of ferromagnetic and superconducting oxides as a case study, the emerging field of engineering the electronic structure at the interface, and thus design of new functionalities, is highlighted.

  15. Mixed-metal hydroxycarboxylic acid complexes

    Formation constants for mixed-metal complexes, Kmmc, between uranium(VI), as the central metal ion, and each one of the metal ions, iron(III), aluminium(III), indium(III) and copper(II) have been determined using data from potentiometric measurements. In each case one of the hydroxycarboxylic acids, citric, tartaric or malic, was used as a ligand. At 298.15 K the values of -log Kmmc for the investigated systems are uranyl iron(II) citrate, 2.45; uranyl iron(III) malate, 7.37; uranyl aluminium(III) citrate, 8.21; uranyl aluminium(III) tartarate, >12; uranyl aluminium(III) malate, 8.06; uranyl indium(III) citrate, 11.3; uranyl indium(III) tartarate, 7.88; uranyl indium(III) malate, 7.45; uranyl copper(II) citrate -1.41; uranyl copper(II) tartarate, -1.17; and uranyl copper(II) malate, -1.11. (author)

  16. Characterisation and application of new carboxylic acid-functionalised ruthenium complexes as dye-sensitisers for solar cells

    Duprez, Virginie; Biancardo, Matteo; Krebs, Frederik C

    2007-01-01

    A series of ruthenium complexes with and without TiO2, anchoring carboxylic acid groups have been synthesised and characterised using nuclear magnetic resonance (NMR), UV-vis and luminescence. These complexes were adsorbed on thin films of the wide band-gap semiconductor anatase and were tested as...

  17. Dispersion Process and Effect of Oleic Acid on Properties of Cellulose Sulfate- Oleic Acid Composite Film

    Guo Chen

    2015-04-01

    Full Text Available The cellulose sulfate (CS is a newly developed cellulose derivative. The work aimed to investigate the effect of oleic acid (OA content on properties of CS-OA film. The process of oleic acid dispersion into film was described to evaluate its effect on the properties of the film. Among the formulations evaluated, the OA addition decreased the solubility and water vapor permeability of the CS-OA film. The surface contact angle changed from 64.2° to 94.0° by increasing CS/OA ratio from 1:0 to 1:0.25 (w/w. The TS increased with OA content below 15% and decreased with OA over 15%, but the ε decreased with higher OA content. The micro-cracking matrices and micro pores in the film indicated the condense structure of the film destroyed by the incorporation of oleic acid. No chemical interaction between the OA and CS was observed in the XRD and FTIR spectrum. Film formulation containing 2% (w/w CS, 0.3% (w/w glycerol and 0.3% (w/w OA, showed good properties of mechanic, barrier to moisture and homogeneity.

  18. Effects of complexing agents on electrochemical deposition of FeS x O y thin films

    Supee, Aizuddin; Ichimura, Masaya

    2016-08-01

    FeS x O y thin films were deposited on indium–tin-oxide (ITO)-coated glass substrates at 15 °C via galvanostatic electrochemical deposition from an aqueous solution containing 100 mM Na2S2O3 and 30 mM FeSO4. The effects of l(+)-tartaric acid (C4H4O6) and lactic acid [CH3CH(OH)COOH] at different concentrations were investigated. All the deposited films were amorphous. With the complexing agents, the thickness was increased, and the oxygen content was reduced significantly compared with the sample deposited without the complexing agents. In the photoelectrochemical measurement, p-type conductivity was confirmed. The photoresponsivity was not influenced significantly by the complexing agent, suggesting that the oxygen content does not drastically affect the properties of the deposited films probably because the local bonding configuration around Fe atoms in FeS x O y is similar to that in FeS2.

  19. Resistive humidity sensor based on vanadium complex films

    A resistive-type relative humidity (RH) sensor based on vanadium complex (VO2(3-fl)) film is reported in this study. Gold electrodes were deposited on the glass substrates in a co-planar structure. A thin film of vanadium complex was coated as a humidity-sensing material on the top of the pre-patterned electrodes. The humidity-sensing principle of the sensor was based on the conductivity change of coated sensing element upon adsorption/desorption of water vapor. The resistance of the humidity sensor measured at 1 kHz decreased linearly with increasing the humidity in the range of 35%–70% RH. The overall resistance of the sensor decreases 11 times. An equivalent circuit for the VO2(3-fl) based resistive-type humidity sensor was developed. The properties of the sensor studied in this work make it beneficial for use in the instruments for environmental monitoring of humidity. (semiconductor devices)

  20. Electropolymerized Molecularly Imprinted Polypyrrole Film for Sensing of Clofibric Acid

    Bianca Schweiger

    2015-02-01

    Full Text Available Piezoelectric quartz crystals and analogous gold substrates were electrochemically coated with molecularly imprinted polypyrrole films for pulsed amperometric detection (PAD of clofibric acid, a metabolite of clofibrate. Cyclic voltammetry data obtained during polymerization and deposited weight estimations revealed a decrease of the polymerization rate with increasing clofibric acid concentration. XPS measurements indicated that clofibric acid could be removed after imprinting with an aqueous ethanol solution, which was further optimized by using PAD. Zeta potential and contact angle measurements revealed differences between molecularly imprinted (MIP and non-imprinted polymer (NIP layers. Binding experiments with clofibric acid and other substances showed a pronounced selectivity of the MIP for clofibric acid vs. carbamazepine, but the response of MIP and NIP to 2,4-dichlorophenoxyacetic acid was higher than that for clofibric acid. A smooth surface, revealed by AFM measurements, with roughness of 6–8 nm for imprinted and non-imprinted layers, might be a reason for an excessively low density of specific binding sites for clofibric acid. Furthermore, the decreased polymerization rate in the presence of clofibric acid might not result in well-defined polymer structures, which could be the reason for the lower sensitivity.

  1. Deoxyribonucleic acid-based hybrid thin films for potential application as high energy density capacitors

    Joyce, Donna M.; Venkat, Narayanan; Ouchen, Fahima; Singh, Kristi M.; Smith, Steven R.; Grabowski, Christopher A.; Terry Murray, P.; Grote, James G.

    2014-03-01

    Deoxyribonucleic acid (DNA) based hybrid films incorporating sol-gel-derived ceramics have shown strong promise as insulating dielectrics for high voltage capacitor applications. Our studies of DNA-CTMA (cetyltrimethylammonium) complex/sol-gel ceramic hybrid thin film devices have demonstrated reproducibility and stability in temperature- and frequency-dependent dielectric properties with dielectric constant k ˜ 5.0 (1 kHz), as well as reliability in DC voltage breakdown measurements, attaining values consistently in the range of 300-350 V/μm. The electrical/dielectric characteristics of DNA-CTMA films with sol-gel-derived ceramics were examined to determine the critical energy storage parameters such as voltage breakdown and dielectric constant.

  2. Chemodynamics of soft nanoparticulate complexes: Cu(II) and Ni(II) complexes with fulvic acids and aquatic humic acids

    Town, R.M.; Leeuwen, van H.P.; Buffle, J.

    2012-01-01

    The dynamics of metal complexation by small humic substances (fulvic acid and aquatic humic acid, collectively denoted as "fulvic-like substance", FS) are explored within the framework of concepts recently developed for soft nanoparticulate complexants. From a comprehensive collection of published e

  3. Surface Functionalization of Hyaluronic Acid Hydrogels by Polyelectrolyte Multilayer Films

    Yamanlar, Seda; Sant, Shilpa; Boudou, Thomas; Picart, Catherine; Khademhosseini, Ali

    2011-01-01

    Hyaluronic acid (HA), an anionic polysaccharide, is one of the major components of the natural extracellular matrix (ECM). Although HA has been widely used for tissue engineering applications, it does not support cell attachment and spreading and needs chemical modification to support cellular adhesion. Here, we present a simple approach to functionalize photocrosslinked HA hydrogels by deposition of poly(L-lysine) (PLL) and HA multilayer films made by the layer-by-layer (LbL) technique. PLL/...

  4. Light amplification in dye-doped DNA-surfactant complex films

    Kawabe, Yutaka; Wang, Lili; Koyama, T.; Horinouchi, Suguru; Ogata, Naoya

    2000-11-01

    We observed amplified spontaneous emission (laser action without cavities) from several kinds of dyes doped in films of salmon DNA (deoxyribonucleic acid) derivatives. We employed laser dye Rhodamine-6G, Pyrromethene 556, and nonlinear optical dye DMASDPB for dopants. Most of sample films with several micrometers thickness were prepared as follows: 1) DNA aqueous solution was mixed with hexadecyltrimethylammonium chloride aqueous solution. 2) precipitated DNA-lipid complex and dyes were dissolved in ethanol or chloroform. 3) Films were formed on substrates by casting from the solution. The amplified spontaneous emission was observed when the films were pumped with a nanosecond laser of 532 nm at the intensity above a threshold value. Spectral narrowing occurred at the threshold energy, and it was accompanied with superlinear dependence of the emission intensity on the pumping intensity. Dye molecules in DNA films can be intercalated in the double helix structure. Because molecules are separated form one another, it is possible to increase chromophore concentration without fluorescence quenching due to aggregation. Furthermore, it is known that DNA shows a good conducting property. We will discuss the possibility of optical and electronic devices utilizing these characteristics.

  5. Photodissociation spectroscopy of the Mg+-acetic acid complex

    We have studied the structure and photodissociation of Mg+-acetic acid clusters. Ab initio calculations suggest four relatively strongly bound ground state isomers for the [MgC2H4O2]+ complex. These isomers include the cis and trans forms of the Mg+-acetic acid association complex with Mg+ bonded to the carbonyl O atom of acetic acid, the Mg+-acetic acid association complex with Mg+ bonded to the hydroxyl O atom of acetic acid, or to a Mg+-ethenediol association complex. Photodissociation through the Mg+-based 3p+, MgOH+, Mg(H2O)+, CH3CO+, and MgCH3+. At low energies the dominant reactive quenching pathway is through dehydration to Mg(H2O)+, but additional reaction channels involving C-H and C-C bond activation are also open at higher energies

  6. Complexes of low oxidated /sup 99/Tc with salicylic acid

    While several complexes of technetium with hydroxycarboxylic acids in solution are well known, little has been done about complexes of technetium with phenolcarboxylic acids. M.A. Kayssi suggested the use of sulphosalicylic acid as a reagent for the quantitative determination of technetium. The resulting complex shows a spectrophotometric maximum at 460 nm; the author supposes that the complex could contain technetium in the (V) oxidation state. In this paper the reaction between technetium and salicylic acid at concentrations between 10/sup -4/ and 5 x 10/sup -2/ M, in a pH range of 2 to 4.5, has been studied. The pH does not seem to influence the reaction, while the salicylic acid concentration is particularly significant

  7. Flotation extraction of rhodanide indium complexes from acidic solutions

    Principle possibility of flotation extraction of indium rhodanide complexes from acid solutions (H2SO4, HCl, HBr, HF, HNO3, HI, H3PO4, CH3COOH, HClO4) is shown. Optimum conditions for their extraction are created in the range of moderate (0.01-0.1 g-eq./l acid in solution) acidity when using quaternary compounds, containing from 13 to 18 carbon atoms in the alkyl part as collectors. It is established experimentally that indium is extracted from weakly acidic solutions in the form of mixed complex anions according to ion exchange mechanism, from strong acidic ones - mainly in the form of acid complexes similar to addition reactions

  8. Studies On Some Acid Divalent-Metal Nitrilotriacetate Complexes

    N. E. Milad

    2000-10-01

    Full Text Available IR and 1H-NMR studies on nitrilotriacetic acid (H3NTA suggest that the acid exists in the zwitterion form, which allows the existence of intermolecular hydrogen bonding. A tetrahedral structure is established for eleven (1:1 anhydrous acid-metal (II nitrilotriacetates complexes. The ten Dq values for the colored complexes were determined spectrophotometrically. The pKa values for the eleven acid metal complexes [M(HNTA].(OH23] were determined and compared with the corresponding pKa values of the [M(OH2n]+2 ions and also with the log β1 values of the corresponding [M(NTA]- complexes. X-ray diffraction studies on the ligand and on eight of these complexes are described.

  9. Formation of linear polyenes in poly(vinyl alcohol) films catalyzed by phosphotungstic acid, aluminum chloride, and hydrochloric acid

    Tretinnikov, O. N.; Sushko, N. I.; Malyi, A. B.

    2016-07-01

    Formation of linear polyenes-(CH=CH)n-via acid-catalyzed thermal dehydration of polyvinyl alcohol in 9- to 40-µm-thick films of this polymer containing hydrochloric acid, aluminum chloride, and phosphotungstic acid as dehydration catalysts was studied by electronic absorption spectroscopy. The concentration of long-chain ( n ≥ 8) polyenes in films containing phosphotungstic acid is found to monotonically increase with the duration of thermal treatment of films, although the kinetics of this process is independent of film thickness. In films containing hydrochloric acid and aluminum chloride, the formation rate of polyenes with n ≥ 8 rapidly drops as film thickness decreases and the annealing time increases. As a result, at a film thickness of less than 10-12 µm, long-chain polyenes are not formed at all in these films no matter how long thermal duration is. The reason for this behavior is that hydrochloric acid catalyzing polymer dehydration in these films evaporates from the films during thermal treatment, the evaporation rate inversely depending on film thickness.

  10. Starch-lipid complexes: Interesting material and applications from amylose-fatty acid salt inclusion complexes

    Aqueous slurries of high amylose starch can be steam jet cooked and blended with aqueous solutions of fatty acid salts to generate materials that contain inclusion complexes between amylose and the fatty acid salt. These complexes are simply prepared on large scale using commercially available steam...

  11. Characterization and complexation of humic acids. Part 1

    This paper summarizes the research contributions to the CEC Mirage II project, particularly the research area on complexation and colloids (COCO). The first part of the paper comprises the characterization of humic and fulvic acids from different origins: a commercial product from the Aldrich Co. used as a reference humic acid and site-specific humic acids from Gorleben (Germany), Boom Clay (Belgium) and Fanay Augeres (France) aquifer systems. The second part includes the complexation of trivalent actinides: Am(III) and Cm(III) with various humic acids. A number of different methods have been applied for the complexation study: spectrophotometry, ultrafiltration, laser-induced photo-acoustic spectroscopy (LPAS) and time-resolved laser fluorescence spectroscopy (TRLFS). The evaluation process of complexation constant is discussed extensively and the well consolidated results are presented, which can be directly used for the geochemical modelling of the radionuclide migration

  12. Development of pectin films with pomegranate juice and citric acid.

    Azeredo, Henriette M C; Morrugares-Carmona, Rosario; Wellner, Nikolaus; Cross, Kathryn; Bajka, Balazs; Waldron, Keith W

    2016-05-01

    The influence of pomegranate juice (PJ, replacing water as solvent) and citric acid (CA) on properties of pectin films was studied. PJ provided the films with a bright red color, and acted as a plasticizer. Increasing PJ/water ratio from 0/100 to 100/0 resulted in enhanced elongation (from 2% to 20%), decreased strength (from 10 to <2 MPa) and modulus (from 93 to <10 MPa), increased water vapor permeability (WVP, from 3 to 9 g.mm.kPa(-1).h(-1).m(-2)), and decreased insoluble matter (IM, from 35% to 24%). Although a crosslinking effect by CA was not confirmed, it has been suggested to occur from its effects on films. CA noticeably increased IM (from <10% to almost 40%); moreover, when measured on a dry film basis, the CA effects presented a noticeable tendency to increases strength and modulus, and to decrease WVP. The red color density was decreased by CA, suggesting a destabilization of anthocyanins. PMID:26769510

  13. Bioinspired lubricating films of cellulose nanofibrils and hyaluronic acid.

    Valle-Delgado, Juan José; Johansson, Leena-Sisko; Österberg, Monika

    2016-02-01

    The development of materials that combine the excellent mechanical strength of cellulose nanofibrils (CNF) with the lubricating properties of hyaluronic acid (HA) is a new, promising approach to cartilage implants not explored so far. A simple, solvent-free method to produce a very lubricating, strong cellulosic material by covalently attaching HA to the surface of CNF films is described in this work. A detailed analysis of the tribological properties of the CNF films with and without HA is also presented. Surface and friction forces at micro/nanoscale between model hard surfaces (glass microspheres) and the CNF thin films were measured using an atomic force microscope and the colloid probe technique. The effect of HA attachment, the pH and the ionic strength of the aqueous medium on the forces was examined. Excellent lubrication was observed for CNF films with HA attached in conditions where the HA layer was highly hydrated. These results pave the way for the development of new nanocellulose-based materials with good lubrication properties that could be used in biomedical applications. PMID:26674836

  14. Investigation of neodymium complexes with hydroxyethyliminodiacetic acid by spectrography

    The electron absorption spectra of NdCl3 solution in the presence of oxyethylimidinodiacetic acid (H2L) in a wide range of pH (1.35-11) were studied. It is shown by the isomolar series method that neodymium forms mono-, di- and sesquialteral complexes with H2L. The absorption spectra of the corresponding solid and dissolved complexes of neodymium with oxyethyliminodiacetic acid were investigated

  15. Visible Absorption Properties of Retinoic Acid Controlled on Hydrogenated Amorphous Silicon Thin Film

    Tsujiuchi, Yutaka; Masumoto, Hiroshi; Goto, Takashi

    2008-02-01

    Langmuir-Blodgett (LB) films of retinoic acid and LB films of retinoic acid mixed with a peptide that contains an alanine-lysine-valine (AKV) amino acid sequence deposited on a hydrogenated amorphous silicon (a-Si:H) film prepared by electron cyclotron resonance (ECR) plasma sputtering were fabricated, and their light absorption spectrums were compared. A specific visible light absorption at approximately 500 nm occurred in a film that had a film thickness of more than 80 nm and a hydrogen concentration of more than 20% in the sputtering process gas. Mixing the AKV sequence peptide with retinoic acid caused a 6 nm blueshift, from 363 to 357 nm, of the absorption maximum of the composite LB film on a SiO2 substrate. Using the same peptide, a large 30 nm blueshift, from 500 to 470 nm, was induced in the composite LB film on the a-Si:H film.

  16. Composition of nitrosyl ruthenium complexes in nitric acid

    The composition of nitrosyl ruthenium complexes in nitric acid has been determined. The analysis was carried out by low temperature, gradient elution, reversed-phase partition chromatography. Paper chromatography, using methyl isopropyl ketone and nitric acid-acetone, were also carried out to obtain complementary data. (author)

  17. Stability constant of the lanthanum complex with humic acid

    The work described here is a study on the formation of trivalent lanthanum complex with humic acid. Commercial humic acid was purified and then characterized by various analytical techniques. The stability constant determined by a radiochemical method has a worth of log βLa,AHA = 13.6. (Author)

  18. Anisotropy and micromagnetics in complex oxide thin films

    Wynn, Thomas Andrew

    Complex oxide perovskites are a class of material with a remarkably wide range of functional properties including magnetism, superconductivity, metal-to-insulator transitions, colossal magnetoresistance, and in some cases high magnetocrystalline anisotropy. Reduction in length scales through thin film deposition and nanopatterning results in altered properties from their bulk constituents. In this work, thin films of La0.7Sr0.3CoO3 (LSCO) and LSCO/La 0.7Sr0.3MnO3 (LSMO) bilayers of varying thicknesses were deposited onto (LaAlO3)0.3(Sr2TaAlO 6)0.7 (LSAT) substrates, and their anisotropic magnetic properties were measured along the in- plane [100] and [110] directions using superconducting quantum interference device (SQUID) magnetometry and soft x-ray magnetic spectroscopy. The LSCO showed thickness dependent magnetism, and films were non-magnetic below a critical thickness of 4 nm. Magnetic LSCO films showed unique anisotropic effects on the saturation magnetization (Ms), with a lower M s in the [110] direction than the [100] direction. This potentially indicates the existence of a hard component in the [110] direction that is not being switched at fields in the SQUID magnetometer (7 T). Normalized hysteresis loops indicate the LSCO films display little magnetocrystalline anisotropy within the plane of the film. LSCO/LSMO bilayers with a fixed LSMO layer of 6 nm in thickness showed cobalt magnetism at thicknesses where single layers were non-magnetic, suggesting that the substrate/film interface is not the cause of the non-magnetic layer in the LSCO thin films. Magnetic coupling occurs in bilayers with LSCO layer thicknesses of below 4 nm, and both LSCO and LSMO layers showed a [110] easy axis. When the layer thickness of LSCO was increased above 8 nm, the LSCO layer developed a soft component at the LSCO/LSMO interface. This soft LSCO component remained coupled with the LSMO, though the easy axis changed to the [100] direction, and the harder, non-interface LSCO

  19. Uranyl complexes of n-alkanediaminotetra-acetic acids

    The uranyl complexes of n-propanediaminetetra-acetic acid, n-butanediaminetetra-acetic acid and n-hexanediaminetetra-acetic acid have been studied by potentiometry, with computer evaluation of the titration data by the MINIQUAD program. Stability constants of the 1:1 and 2:1 metal:ligand chelates have been determined as well as the respective hydrolysis and polymerization constants at 25 deg in 0.10M and 1.00M KNO3. The influence of the length of the alkane chain of the ligands on the complexes formed is discussed. (author)

  20. Protection of NdFeB magnets by corrosion resistance phytic acid conversion film

    Nan, Haiyang; Zhu, Liqun; Liu, Huicong; Li, Weiping

    2015-11-01

    Phytic acid conversion film was prepared on NdFeB magnets by dipping the NdFeB into phytic acid solution. The morphology, composition, structure and corrosion resistance of the film were systematically investigated. The results showed that the phytic acid film was effective in improving the corrosion resistance of NdFeB magnets. XRD, TEM and FT-IR analyses revealed that the film was amorphous and had a strong peak of phosphate radical (PO43-). The formation mechanism of the film was also explored by XPS and the potential of zero charge (Epzc) measurement at the solution-metal interface.

  1. Investigation into neodymium complexes with methylmalonic acid by spectrography

    Complexes of neodymium with methylmalonic acid have been studied spectrographically. It has been shown that aquoion and three dimeric complexes of the composition approximately 1:1 coexist in the pH region 3.5-6.5 when the ratio between the components is equimolar. When there is an excess of the ligand, polymeric complexes of the composition 1:2 are found in the solution in addition to the complexes 1:1. The stability constants of the complexes have been determined and the data on their structure have been obtained

  2. Synthesis and characterization of acidic mesoporous borosilicate thin films.

    Xiu, Tongping; Liu, Qian; Wang, Jiacheng

    2009-02-01

    Work on the synthesis and characterization of acidic wormhole-like ordered mesoporous borosilicate thin films (MBSTFs) on silicon wafers is described in this paper. The MBSTFs coated by the dip-coating method were prepared through an evaporation-induced self-assembly (EISA) process using nonionic block copolymers as structure-directing agents. Fourier transform infrared (FT-IR) spectroscopy confirmed the formation of borosiloxane bonds (Si-O-B). High-resolution transmission electron microscopy (HRTEM) and N2 sorption evidenced a wormhole-like mesoporous structure in the MBSTFs obtained. Scanning electron microscopy (SEM) images of the cross sections and surfaces of the samples showed that MBSTFs on silicon wafers were continuous, homogeneous and did not crack. The acidic properties of the MBSTFs were characterized by FT-IR spectra of chemisorbed pyridine. The MBSTFs thus prepared may find their future applications in many fields including chemical sensors, catalysis, optical coating, molecule separation, etc. PMID:19441565

  3. Acrylic acid obtaining from methanol and acetic acid in the presence of complex oxide catalysts

    Небесний, Роман Володимирович; Піх, Зорян Григорович; Шпирка, Ірина Іванівна; Івасів, Володимир Васильович; Небесна, Юлія Віталіївна; Фуч, Уляна Василівна

    2015-01-01

    The purpose of this work is to research process of single-stage acrylic acid obtaining from methanol and acetic acid, namely: to develop effective catalysts for the process of methanol oxidation to formaldehyde with its further aldol condensation with acetic acid to acrylic acid, and to determine optimum conditions for the process. Complex oxide catalysts consisting of oxides of boron, phosphorus, tungsten and vanadium supported on the silica gel have been investigated. The effect of vanadium...

  4. Radiation grafting of acrylic acid onto polypropylene films

    A study has been made for the preparation of membranes by the direct radiation grafting of acrylic acid (AAc) onto polypropylene (PP) films. The appropriate reaction conditions were selected under which the graft polymerization was carried out successfully. The effect of different solvents such as benzene, methanol/water mixture, isopropanol/water mixture, dimethyl formamide and distilled water on the swelling and grafting process of AAc onto PP films was investigated. In this grafting system ammonium ferrous sulphate (Mohr's salt) and ferric chloride were used as inhibitors to minimize the homopolymerisation of AAc and the suitable concentration of the inhibitor was found to be 1.0 and 1.5 wt% for Mohr's salt and ferric chloride, respectively. Also, the effect of monomer concentration on the rate of grafting was investigated. The dependence of the grafting rate on monomer concentration was found to be 1.1 order. This grafting system proceeded by diffusion controlled process. Some selected properties of the grafted films such as swelling behaviour, gel determination, mechanical and electrical properties were also investigated. It was found that the grafted membranes possess good hydrophilic properties which may make them promising in some practical applications. (author)

  5. Laser-induced damage of sol-gel silica acid and basic thin films

    The sol-gel monolayer silica acid and basic thin films on K9 glass substrates were prepared with the dip method from acid and basic catalyzed silica sols, respectively. Both films have nearly similar optical thickness. The laser-induced damage thresholds(LIDT) of the two kinds of films were measured. Thermal absorption, porous ratio and surface morphologies of films were investigated by Stanford photo-thermal solutions, ellipsometer, atomic force microscope(AFM) and scanning electron micro-scope(SEM), respectively. Optical microscope was used to characterize the defects and impurities of films before laser irradiation and damage morphology after laser irradiation. The experimental results showed that compared with basic film, the silica acid film had larger absorption, smaller porous ratio, and smaller LIDT. Different damage morphologies of films were relative to their different absorption and microstructures. (authors)

  6. Photoconductivity study of acid on Zinc phthalocyanine pyridine thin films

    Singh, Sukhwinder; Saini, G. S. S.; Tripathi, S. K.

    2016-05-01

    The Metal Phthalocyanine (MPc) have attracted much interest because of chemical and high thermal stability. Molecules forming a crystal of MPc are held together by weak attractive Vander Waals forces. Organic semiconductors have π conjugate bonds which allow electrons to move via π-electron cloud overlaps. Conduction mechanisms for organic semiconductor are mainly through tunneling; hopping between localized states, mobility gaps, and phonon assisted hopping. The photo conductivity of thin films of these complexes changes when exposed to oxidizing and reducing gases. Arrhenius plot is used to find the thermal activation energy in the intrinsic region and impurity scattering region. Arrhenius plotsare used to find the thermal activation energy.

  7. Novel silk fibroin films prepared by formic acid/hydroxyapatite dissolution method

    Bombyx mori silk fibroin from the silkworm was firstly found to be soluble in formic acid/hydroxyapatite system. The rheological behavior of silk fibroin solution was significantly influenced by HAp contents in dissolved solution. At the same time, silk fibroin nanofibers were observed in dissolved solution with 103.6 ± 20.4 nm in diameter. Moreover, the structure behavior of SF films prepared by formic acid/hydroxyapatite dissolution method was examined. The secondary structure of silk fibroin films was attributed to silk II structure (β-sheet), indicating that the hydroxyapatite contents in dissolved solution were not significantly affected by the structure of silk fibroin. The X-ray diffraction results exhibited obviously hydroxyapatite crystalline nature existing in silk fibroin films; however, when the hydroxyapatite content was 5.0 wt.% in dissolved solution, some hydroxyapatite crystals were converted to calcium hydrogen phosphate dehydrate in silk fibroin dissolution process. This result was also confirmed by Fourier transform infrared analysis and DSC measurement. In addition, silk fibroin films prepared by this dissolution method had higher breaking strength and extension at break. Based on these analyses, an understanding of novel SF dissolution method may provide an additional tool for designing and synthesizing advanced materials with more complex structures, which should be helpful in different fields, including biomaterial applications. - Highlights: • SF fibers were firstly successfully dissolved in FA/HAp solution. • The rheological behavior of SF solution was significantly influenced by HAp contents. • SF nanofibrils were observed in FA/HAp solution with 103.6 ± 20.4 nm in diameter. • SF films prepared by FA/HAp dissolution method had higher mechanical properties

  8. Complex forming properties of natural organic acids. Pt. 2

    An ultrafiltration technique combined with ion-selective-electrode and atomic absorption methods have been employed to obtain information on the complex forming properties of fulvic acid with iron and calcium. A model for interpreting complexation of metal ions to fulvic acid at any pH, medium ionic strength and metal to fulvic acid ratio developed earlier has been used in an attempt to predict the nature of iron and calcium interaction to Armadale Horizon Bh fulvic acid. Binding of calcium to fulvic acid which is enhanced at pHs greater than 6.0 has reasonably been predicted by the model taking into consideration complications due to the polyelectrolyte nature and the heterogeneity of the fulvic acid. The lack of agreement observed between the model predicted binding behavior and the experimentally observed results for the fulvic acid-iron system has been attributed to the formation of metal-induced aggregation. Reduction of Fe(III) to Fe(II) by the fulvic acid as reported by other workers is corroborated. (orig.)

  9. NMR studies of the complexes of uramildiacetic acid

    Proton spectra of 1,3 dimethyluramildiacetic acid and its complexes with several lanthanide ions as well as titration curves of uramildiacetic and barbituric acids where 13C chemical shifts were followed as a function of pH, have enabled the establishment of the conformation in solution of the complexes of the uramildiacetate-type ligands and of the most probable mechanism of ionization of these compounds. It is definitely shown that uramildiacetic acid is tetradentate and that it coordinates to metal ions through the iminodiacetate group and one of the carboxyl groups in position 4,6 of the molecule. The pyrimidinic ring and one of the chelator rings are coplanar and the complexes have axial symmetry. (author)

  10. Phase Chemistry of the Complexes of RE Amino Acids

    2002-01-01

    Forty-three phase diagrams of ternary system concerning rare earth salts, α-amino acids and water, which were constructed by phase equilibrium methods, were expounded. The influences of the factors such as cations, anions, the structure of amino acids, temperature on the phase diagrams were discussed. Under the guidance of phase equilibrium results, over 150 new solid complexes were prepared. IR, reflecting, UV, FS, and Raman spectra for these complexes were investigated and the regularity of “tripartite effect”, “tetrad effect”, “Nephelanxetic effect”, “Oddo-Harkins” was observed. Thermal decomposition processes of the complexes were confirmed. Based on the comparison with the known crystal structures of rare earth-amino acid-complexes, an estimation method for predicting the crystal structure data of series complexes was founded. The constant volume combustion energies of the complexes were determined by RBC-1 type rotating bomb calorimeter. The standard enthalpies of combustion and standard enthalpies of formation were calculated for these complexes.

  11. Analyzing Freud's Oedipus Complex from the Perspective of the Films of Hamlet%Analyzing Freud's Oedipus Complex from the Perspective of the Films of Hamlet

    吴静

    2012-01-01

    Freud's Oedipus complex has an important influence on the performance of Shakespeare's Hamlet. Analyzing Freud's Oedipus complex from a visual perspective, which helps understand Hamlet's suffering from oedipal conflicts more easily and visibly. This paper mainly focuses on two popular films. One is the most classical, the black-and-white film produced, directed and starred by Laurence Oliver in 1948. with Eileen Heritee as Gertude. The other is the PBS version of 2010, lasting nearly three hours, directed by Gregory Doran.

  12. The Effects of plasticizers and palmitic acid toward the properties of the carrageenan Film

    Heru Wibowo, Atmanto; Listiyawati, Oktaviana; Purnawan, Candra

    2016-02-01

    Varied plasticizers and palmitic acid additive have been added in the carrageenan film. The film was made by mixing of the carrageenan and plasticizers (glycerol, polyethylene glycol, polyvinyl alcohol) with composition of 92:3, 90:6, 87:9, 84:12, 81:15(%w/w) and in the presence of palmitic acid as additive with 1%, 2%, 3%, 4%, 5% of total weight. Casting method was used for the film molding and drying at 60oC with the oven for 12 hours. To investigate the effects of plasticizers and additive, some mechanical tests on film were performed. The test result concludes that plasticizers in the film decreased the tensile strength and increased the elongation break of the carrageenan film. The additive of palmitic acid decreased the tensile strength of the carrageenan film and also decreased the-the water absorbance of the film. The highest tensile strength of films made was with the formulation of carrageenan: PEG with composition of 92:3 (% w/w). The highest elongation break of the film was for carrageenan:PVA with the composition of 81: 15 (%w/w) and carrageenan:palmitic acid:PEG with the composition of 92: 3: 1 (%w/w). The lowest water absorption of the film was achieved for carrageenan:PVA:palmitic acid with the composition of 87: 3: 5 (%w/w).

  13. Antimicrobial activity of nisin incorporated in pectin and polylactic acid composite films against Listeria monocytogenes

    Extruded composite films from 20% pectin and 80% polylactic acids (PLA) were developed and nisin was loaded into films by a diffusion post extrusion. Inhibitory activities of the films against Listeria monocytogenes were evaluated in brain heart infusion (BHI) broth, liquid egg white and orange juic...

  14. Formation constants of mixed ligand complexes of oxovanadium(IV) with salicylic acid/5-sulphosalicylic acid/8-hydroxyquinoline-5-sulphonic acid and hippuric acid

    Equilibrium studies are described on the interaction of oxovanadium(IV) with salicylic acid (SA)/5-sulphosalicylic acid (SSA)/8-hydroxyquinoline-5-sulphonic acid (HQSA) in presence of hippuric acid. The formation of 1:1:1 mixed ligand complexes and their hydroxo derivatives inferred from the pH-metric titration curves and formation constants of 1:1:1 ternary complexes have been evaluated at 30 +- 0.5deg (μ = 0.1 M KNO3). The order of stability of ternary complexes has been found to be the same as that of 1:1 binary complexes involving hydroxy acids. (author)

  15. Facile method to prepare silk fibroin/hyaluronic acid films for vascular endothelial growth factor release.

    Zhou, Juan; Zhang, Bin; Liu, Xunwei; Shi, Lijun; Zhu, Jun; Wei, Daixu; Zhong, Jian; Sun, Gang; He, Dannong

    2016-06-01

    A facile approach was proposed to prepare silk fibroin (SF) and hyaluronic acid (HA) composite films from aqueous solution without crosslinking or any post treatment. Only by controlling the HA content and film formation temperature during the film casting, the HA/SF films with different composition were prepared. The films were then characterized by structural characteristics, thermal stability, morphology, water stability, water absorption, mechanical properties. After immersing in water for 24h, all of the films showed good structural integrity. The degradation rate of the HA/SF films in protease XIV can be controlled by changing the film formation temperature and HA content. Decreasing the temperature and adding HA resulted in the rapid release of VEGF (vascular endothelial growth factor) from the HA/SF films. Overall, the 5% HA/SF films formed at 37°C with more rapid VEGF release exhibited great potential in drug delivery, especially when the rapid vascularization was needed. PMID:27083373

  16. Spectrographic investigation of neodymium complexing with hexamethylenediaminetetraacetic acid

    Complex formation between neodymium and hexamethylenediamine-tetraacetic acid (HMTA, H2L) in aqueous solution has been studied by high-resolution spectrography. Formation of NdHL, Hd(HL)23-, Nd(HL)36- complexes has been proved, their values of formation constants (lg Csub(form)) being equal to 5.63+-0.45, 4.20+-0.15, 2.63+-0.15, respectively

  17. A multivariant study of the absorption properties of poly(glutaric-acid-glycerol) films

    The solvent absorption into the matrix of poly(glutaric acid-glycerol) films made with or without either iminodiacetic acid, sugarcane bagasse, pectin, corn fiber gum or microcrystalline cellulose have been evaluated. The films were incubated in various solvent systems for 24h. The amounts of solve...

  18. Effects of swelling on the viscoelastic properties of polyester films made from glycerol and glutaric acid

    Viscoelastic properties have been determined for poly(glycerol-co-glutaric acid) films synthesized from Lewis acid-catalyzed polyesterifications. The polymers were prepared by synthesizing polymer gels that were subsequently cured at 125 degrees C to form polymer films. The polymers were evaluated ...

  19. Polypyrrole-polyvinyl sulphonate film based disposable nucleic acid biosensor

    Prabhakar, Nirmal [Biomolecular Electronics and Conducting Polymer Research Group, National Physical Laboratory, Dr. K.S. Krishnan Road, New Delhi 110012 (India); Centre for Biomedical Engineering, Indian Institute of Technology, Hauz Khas, New Delhi 110016 (India); Arora, Kavita [Biomolecular Electronics and Conducting Polymer Research Group, National Physical Laboratory, Dr. K.S. Krishnan Road, New Delhi 110012 (India); Singh, Surinder P. [Biomolecular Electronics and Conducting Polymer Research Group, National Physical Laboratory, Dr. K.S. Krishnan Road, New Delhi 110012 (India); Pandey, Manoj K. [Biomolecular Electronics and Conducting Polymer Research Group, National Physical Laboratory, Dr. K.S. Krishnan Road, New Delhi 110012 (India); Singh, Harpal [Centre for Biomedical Engineering, Indian Institute of Technology, Hauz Khas, New Delhi 110016 (India); Malhotra, Bansi D. [Biomolecular Electronics and Conducting Polymer Research Group, National Physical Laboratory, Dr. K.S. Krishnan Road, New Delhi 110012 (India)]. E-mail: bansi.malhotra@gmail.com

    2007-04-18

    Double stranded calf thymus deoxyribonucleic acid entrapped polypyrrole-polyvinyl sulphonate (dsCT-DNA-PPy-PVS) films fabricated onto indium-tin-oxide (ITO) coated glass plates have been used to detect organophosphates such as chlorpyrifos and malathion. These disposable dsCT-DNA-PPy-PVS/ITO bioelectrodes have been characterized using cyclic voltammetry, Fourier-transform-infra-red (FTIR) spectroscopy and atomic force microscopy (AFM), respectively. These biosensing electrodes have a response time of 30 s, are stable for about 5 months when stored in desiccated conditions at 25 deg. C and can be used to amperometrically detect chlorpyrifos (0.0016-0.025 ppm) and malathion (0.17-5.0), respectively. The additive effect of these pesticides on the amperometric response of the disposable dsCT-DNA-PPy-PVS/ITO bioelectrodes has also been investigated.

  20. Impact of acid and oxidative modifications, single or dual, of sorghum starch on biodegradable films.

    Biduski, Bárbara; Silva, Francine Tavares da; Silva, Wyller Max da; Halal, Shanise Lisie de Mello El; Pinto, Vania Zanella; Dias, Alvaro Renato Guerra; Zavareze, Elessandra da Rosa

    2017-01-01

    The objective of this study was to evaluate the effects of acid and oxidation modifications on sorghum starch, as well as the effect of dual modification of starch on the physical, morphological, mechanical, and barrier properties of biodegradable films. The acid modification was performed with 3% lactic acid and the oxidation was performed with 1.5% active chlorine. For dual modification, the acid modification was performed first, followed by oxidation under the same conditions as above. Both films of the oxidized starches, single and dual, had increased stiffness, providing a higher tensile strength and lower elongation when compared to films based on native and single acid modified starches. However, the dual modification increased the water vapor permeability of the films without changing their solubility. The increase in sorghum starch concentration in the filmogenic solution increased the thickness, water vapor permeability, and elongation of the films. PMID:27507447

  1. Diffusion coefficients of metals and metal complexes in hydrogels used in diffusive gradients in thin films

    Diffusion coefficients of metal ions and metal-ligand complexes in hydrogels were measured at ionic strengths of 0.1-100 mmol L-1 using a diffusion cell. The three different types of hydrogel were all based on polyacrylamide and have been commonly used in the technique of diffusive gradients in thin films (DGT), where accurate diffusion coefficients are essential for the assessment of the concentrations of labile metal in solution. There was little difference in the diffusion coefficients of either Cu and Cd measured in gels with thicknesses of 0.4, 0.8 and 1.6 mm, showing that any diffusion boundary layer in solution was negligibly small. The diffusion coefficients of Pb, Ni, Cu and Cd in simple inorganic solutions was independent of ionic strength (1-100 mmol L-1), except at very low ionic strengths (0.1 mmol L-1) where the value of D was 50% lower. This observation is consistent with the gel having a positive charge that creates a Donnan partitioning of cations at the gel surface. Diffusion coefficient of Pb complexes decreased with increasing size of the ligand, in the order of diglycolic acid (DGA), nitrilotriacetic acid (NTA), fulvic acid and humic acid. In freshwaters the contribution of fulvic acid species to measured DGT mass should be considered. No significant difference was found between the rate of diffusion of Cu and Cd through the mostly commonly used gel and the filter membrane at the face of the DGT device. Diffusion coefficients obtained using a gel with small pore size (restricted gel) plus filter membrane were higher than those obtained using the restricted gel alone. It may be necessary to modify the standard DGT equation for restricted gel deployments, to take into account the difference in diffusion between the gel and the filter membrane

  2. Effects of gas atmospheres on poly(lactic acid) film in acrylic acid plasma treatment

    Plasma polymerized acrylic acid (AA) coatings were deposited on poly(lactic acid) (PLA) films in various gas atmospheres during the pre-treatment of PLA and the deposition of AA, respectively. Therefore, this work was twofold: the argon pretreated PLA films followed by a deposition in argon were investigated against the mixture of argon and oxygen pretreated ones under the same deposition conditions; the plasma deposition of AA operating in different atmospheres (argon, oxygen and nitrogen) was employed to modify the pretreated PLA in oxygen. Chemical and physical changes on the plasma-treated surfaces were examined using contact angle, X-ray photoelectron spectroscopy (XPS), field emission scanning electron microscopy (FE-SEM) and attenuated total reflection infrared (ATR-FTIR) analysis. The results showed that the discharge gas can have a significant influence on the chemical composition of the PLA surfaces: oxygen plasmas introduced oxygen-containing groups in company with surface etching in pretreatment and deposition, while argon discharges was able to achieve much better hydrophilic behavior and high retention ratio of poly(acrylic acid) (PAA) coating before and after washing in water.

  3. Effects of gas atmospheres on poly(lactic acid) film in acrylic acid plasma treatment

    Zhao, Yun, E-mail: yun.zhaotju@yahoo.com [Dipartimento di Scienza Applicata e Tecnologia, Politecnico di Torino, C.so Duca degli Abruzzi 24, 10129 Turin (Italy); Fina, Alberto [Dipartimento di Scienza Applicata e Tecnologia, Politecnico di Torino – sede di Alessandria, V. T. Michel 5, 15121 Alessandria (Italy); Venturello, Alberto; Geobaldo, Francesco [Dipartimento di Scienza Applicata e Tecnologia, Politecnico di Torino, C.so Duca degli Abruzzi 24, 10129 Turin (Italy)

    2013-10-15

    Plasma polymerized acrylic acid (AA) coatings were deposited on poly(lactic acid) (PLA) films in various gas atmospheres during the pre-treatment of PLA and the deposition of AA, respectively. Therefore, this work was twofold: the argon pretreated PLA films followed by a deposition in argon were investigated against the mixture of argon and oxygen pretreated ones under the same deposition conditions; the plasma deposition of AA operating in different atmospheres (argon, oxygen and nitrogen) was employed to modify the pretreated PLA in oxygen. Chemical and physical changes on the plasma-treated surfaces were examined using contact angle, X-ray photoelectron spectroscopy (XPS), field emission scanning electron microscopy (FE-SEM) and attenuated total reflection infrared (ATR-FTIR) analysis. The results showed that the discharge gas can have a significant influence on the chemical composition of the PLA surfaces: oxygen plasmas introduced oxygen-containing groups in company with surface etching in pretreatment and deposition, while argon discharges was able to achieve much better hydrophilic behavior and high retention ratio of poly(acrylic acid) (PAA) coating before and after washing in water.

  4. Complexation of the uranyl ion with aquatic humic acid

    The complexation of the uranyl(VI) ion with aquatic humic acid from Gorleben groundwater (Gohy-573) is studied in 0.1 M NaClO4 at pH 4 under argon atmosphere. The concentration range investigated is from 1 x 10-7 to 1 x 10-5 mol/l for the uranyl ion and from 1 x 10-6 to 1.12 x 10-5 mol/l for the humic acid. Three different experimental methods are applied to separate the uncomplexed uranyl ion from the uranyl humate complex, using differences of the two species in size by ultrafiltration at the pore size of about 1 nm, in charge by anion exchange separation and in spectroscopic properties by time resolved laser fluorescence spectroscopy (TRLFS). No reduction of U(VI) to U(IV) is observed in the course of the humate complexation process. The experimental results confirm that the prevailing complexation reaction is charge neutralization of the UO2+2 ion with two proton exchanging sites of humic acid. At pH 4 in 0.1 M NaClO4, where the hydrolysis of the uranyl ion appears negligible, the fraction of proton exchanging sites of the humic acid that can be occupied by the uranyl ion (called the loading capacity (LC) of the uranyl ion) is determined to be 0.185±0.003. The complexation constant evaluated by taking the loading capacity into account is found to be logβ = 6.16±0.13, which is a grand average of all values determined by the three experimental procedures under consideration. This value is valid for the humate complexation of the non-hydrolyzed uranyl ion, being independent of pH and ionic strength. (orig.)

  5. Protactinium(V) complexation by oxalic and diethylenetriaminepentaacetic acids

    The present work is devoted to complexation of Pa(V) with oxalic acid and DTPA. Structural data on the limiting complex have been collected by combining X-ray absorption Spectroscopy, Capillary Electrophoresis (CE-ICP-MS) and DFT calculations. Thermodynamic data have been deduced from solvent extraction experiments. XAS data registered on samples of Pa(V) in oxalic acid have revealed the presence of one single Pa-O oxo bond and 3 oxalate in a bidentate mode in the complex of maximum order. The structure optimization, performed through DFT calculations indicate that 2 oxalate lie in the equatorial plane of the Pa=O bond, whereas one oxygen of the third oxalate goes in the prolongation of the oxo bond. Stability constants of the three successive complexes were determined by solvent extraction in the TTA/toluene/H2O/Pa(V)/NaClO4/HClO4/H2C2O4 system at different temperatures and 3M ionic strength. The stability of the complexes was proved to increase with their order. CE-ICP-MS measurements on Pa/DTPA samples have indicated the formation of a neutral (1:1)limiting complex. This complex can therefore be written as Pa(DTPA). The optimized structure determined by DFT calculations allowed one to conclude that all eight donor atoms (5 O and 3 N) of the DTPA ligand are involved in the coordination of protactinium. The formation constant of this complex has been determined for different values of ionic strength and temperature. The complexation reaction of Pa(V) with DTPA was proved to be entropy controlled. (author)

  6. Synthesis and properties of ZnS-EuS films grown from volatile complex compounds

    Bessergenev, V.G.; Ivanova, E.N.; Kovalevskaya, Y.A. [Siberian Branch of Russian Academy of Sciences, Novosibirsk (Russian Federation). Inst. of Inorganic Chemistry

    1997-10-01

    Deposition and characterization of films of ZnS, EuS and ZnS:Eu are described. The films have been prepared by chemical vapor deposition using new volatile complex compounds, dithiocarbamates of Zn and Eu, as precursors. Characterization includes X-ray diffraction, chemical analysis of the film composition, Raman spectroscopy, ellipsometry, and spectrophotometry. The spatial chemical homogeneity of the films has been determined using a recently developed method of differential dissolution and found to be uniform. Doping of ZnS by Eu with dopant concentration up to 0.3 at.% has been achieved. Effects of Eu doping on structural and optical properties of the films are presented.

  7. Synthesis ZnS:Sm thin films from volatile complex compounds

    Ivanova, Elena N.; Kovalevskaya, Yu. A.; Bessreguenev, Valentin G.

    2002-11-01

    Deposition and characterization of ZnS, Sm2S3 and ZnS:Sm films are described. The films have been prepared by chemical vapor deposition using new volatile complex compounds, dithiocarbamates of Zn and Sm, as precursors. Characterization includes X-ray diffraction, chemical analysis of the film composition, ellipsometry and spectrophotometry. It has been shown that at relatively low temperatures (about 380 °C) monophase crystalline Sm2S3 films can be fabricated. Doping of ZnS by Sm with dopant concentration up to 2 at. % has been achieved. Effects of Sm doping on structural and optical properties of the film are presented.

  8. Introduction of phosphoric acid group to polypropylene film by radiation grafting and its blood compatibility

    2,3-epoxypropyl methacrylate (EPMA) was grafted to polypropylene (PP) film by using a radiation grafting technique. The phosphoric acid group was introduced to the EPMA-grafted PP films with different grafting yields. The blood compatibility of the phosphoric acid group-introduced PP films was evaluated by the determination of platelet adsorption and thrombus formation. The EPMA grafting extent was found to be dependent on the absorbed dose, reaction time and temperature. The grafting and phosphonation reactions were confirmed by Fourier transform infrared spectroscopy in the attenuated total reflectance mode and electron spectroscopy for chemical analysis. The amount of thrombus and adherent platelet on modified PP film was evaluated by an in vitro method and scanning electron microscope, respectively. The phosphoric acid group-introduced PP film was found to have good blood compatibility, which increased with the content of the introduced phosphoric acid group

  9. Effect of complexing agent on the photoelectrochemical properties of bath deposited CdS thin films

    In the present paper photoelectrochemical (PEC) performance of bath deposited CdS thin films based on complexing agents i.e. ammonia and triethanolamine (TEA) has been discussed. Effect of annealing has also been analyzed. The as-deposited and annealed (at 523 K for 1 h in air) films were characterized by X-ray diffraction (XRD), ultraviolet-visible (UV-vis) absorption spectroscopy, SEM, electrochemical impedance spectroscopy (EIS), and PEC properties. XRD studies revealed that the films were nanocrystalline in nature with mixed hexagonal and cubic phases. TEA complex resulted in better crystallinity. Further improvement in the crystallinity of the films was observed after air annealing. The marigold flower-like structure, in addition to flakes morphology, was observed with TEA complex, whereas for ammonia complex only flakes morphology was observed. The UV-vis absorption studies revealed that the optical absorption edge for the films with ammonia and TEA complex was around 475 nm and 500 nm, respectively. Annealing of the films resulted in red shift in the UV-vis absorption. The PEC cell performance of CdS films was found to be strongly affected by crystallinity and morphology of the films resulted due to complexing agent and annealing. The air annealed film deposited using TEA complex showed maximum short circuit current density (Jsc) and open circuit voltage (Voc) i.e. 99 μA/cm2 and 376 mV respectively, under 10 mW/cm2 of illumination. The films deposited using TEA complex showed good stability under PEC cell conditions.

  10. The complexation behavior of neptunium and plutonium with nitrilotriacetic acid

    The first stability constant of NpO2+ with nitrilotriacetic acid (NTA) was determined at four ionic strengths (I = 0.5, 1.0, 2.0, 3.0 M) by using spectrophotometry. Nonlinear least-squares data fitting identified the complex as NpO2NTA2-. The specific ion interaction (SIT) theory approximation method was used to determine the stability constants at infinite dilution. In this paper first results on Pu4+ and PuO22+ complexation with NTA are reported. The stability constant for the Pu(NTA)+ complex at I = 0.1 M is given. From results for PuO22+ complexation with NTA (I = 1 M) at pH 2-NTA-. At pH > 3, NTA partially reduced PuO22+ to PuO2+

  11. Scandium and zirconium ion complexing with salicylic acid

    A study has been made of the extraction of complexes containing scandium and zirconium compounds and salicylic acid by using benzene, nitrobenzene, chloroform and isoamyl alcohol. It is shown that in the metal concentration range 10-5-10-3 mole/l scandium forms mononuclear complexes composed of Sc(HSal)3 (pH2 (pH>4), zirconium - polynuclear complexes Zrsub(x)(OH)sub(y)(HSal)sub(n), where the x:n ratio varies from 0.5 to 1.5. Stability constants have been calculated for the salicylate scandium complexes in aqueous solution, equal to β1=(3+-1)x102; β2=(5.0+-0.6)x104; β3=(5.3+-0.3)x106

  12. A study on antithrombogenic polymeric dialytic membrane. Irradiation grafting acrylic acid and styrene into polyethylene films

    A new type of antithrombogenic polymeric dialytic membrane with a hydrophilic-hydrophobic microphase structure was prepared by grafting acrylic acid and styrene into polyethylene films, using peroxidation pre-irradiation technique. Various ratios of monomers influencing on properties of the grafted films were examined. Experimental results showed that the grafted films have superior mechanic strength, and their antithrombogenicity and permeability were 30 and 10 times higher than that of the ungrafted films respectively on condition of the volume ratio 1:1 (styrene vs acrylic acid)

  13. Pharmacology of bile acid receptors: Evolution of bile acids from simple detergents to complex signaling molecules.

    Copple, Bryan L; Li, Tiangang

    2016-02-01

    For many years, bile acids were thought to only function as detergents which solubilize fats and facilitate the uptake of fat-soluble vitamins in the intestine. Many early observations; however, demonstrated that bile acids regulate more complex processes, such as bile acids synthesis and immune cell function through activation of signal transduction pathways. These studies were the first to suggest that receptors may exist for bile acids. Ultimately, seminal studies by many investigators led to the discovery of several bile acid-activated receptors including the farnesoid X receptor, the vitamin D receptor, the pregnane X receptor, TGR5, α5 β1 integrin, and sphingosine-1-phosphate receptor 2. Several of these receptors are expressed outside of the gastrointestinal system, indicating that bile acids may have diverse functions throughout the body. Characterization of the functions of these receptors over the last two decades has identified many important roles for these receptors in regulation of bile acid synthesis, transport, and detoxification; regulation of glucose utilization; regulation of fatty acid synthesis and oxidation; regulation of immune cell function; regulation of energy expenditure; and regulation of neural processes such as gastric motility. Through these many functions, bile acids regulate many aspects of digestion ranging from uptake of essential vitamins to proper utilization of nutrients. Accordingly, within a short time period, bile acids moved beyond simple detergents and into the realm of complex signaling molecules. Because of the important processes that bile acids regulate through activation of receptors, drugs that target these receptors are under development for the treatment of several diseases, including cholestatic liver disease and metabolic syndrome. In this review, we will describe the various bile acid receptors, the signal transduction pathways activated by these receptors, and briefly discuss the physiological processes that

  14. Controllably local gene delivery mediated by polyelectrolyte multilayer films assembled from gene-loaded nanopolymersomes and hyaluronic acid

    Teng W

    2014-10-01

    a complex form. In vitro cell experiments demonstrate that PEM films can enhance the adhesion and proliferation of MSCs and efficiently transfect MSCs in situ in vitro for at least 4 days. Our results suggest that a (pNPs/HAn system can mediate efficient transfection in stem cells in a spatially and temporally controllable pattern, highlighting its huge potential in local gene therapy. Keywords: localized gene delivery, layer-by-layer self-assembly, gene-loaded nanopolymersomes, hyaluronic acid, polyelectrolyte multilayer films, mesenchymal stem cells

  15. Corrosion Inhibition of Mild Steel in Hydrochloric Acid Solution by Amino Acid Complexes

    K. Kiruthikajothi; G. Chandramohan

    2015-01-01

    Using the amino acids methionine and serine reduced Schiff base and their copper(II) complexes were synthesized. The inhibition effect of these copper (II) complexes on the corrosion of mild steel in 1 M HCl solution was investigated. The corrosion inhibition action is studied through weight loss method. Among the tested complexes [CuCl(SMet)PPh3.H2O] exhibited better corrosion inhibition at 3 mmol concentration. The adsorption of the complexes on the metal surface obeys Langmuir’s adsorption...

  16. Photoelectrochemical properties of WO3 nanoparticulate thin films prepared by carboxylic acid-assisted electrodeposition

    Optimisation of particle sizes of WO3 films is important for photoelectrochemical applications. However, most of the developed size-controlled synthesis techniques involve complicated instruments or vacuum systems. The present work presents an alternative method using carboxylic acid-assisted electrodeposition where WO3 thin films were deposited from peroxotungstic acid (PTA) solution containing different carboxylic acids (formic, oxalic, citric). The effects of carboxylic acids on the electrodeposition and the resultant morphological, mineralogical, optical, and photoelectrochemical properties of the WO3 films were investigated. The analysis showed that the films consisted of equiaxed nanoparticulate monoclinic WO3. The deposition thicknesses and the average grain (individual particle and agglomerate) sizes of the films were dependent on the amount of hydronium ions and the molecular weight and associated sizes of the conjugate bases released upon the dissociation of carboxylic acids in the PTA solutions, which result in hydrogen bond formation and molecular dispersion. The photocurrent densities of the films deposited with carboxylic acids were greater than that of the film deposited from pure PTA. These differences were attributed to improvements in (1) grain size, which controls photogenerated electron-hole transport, and (2) effective grain boundary area, which controls the numbers of active reaction sites and electron-hole recombination sites. - Highlights: • Carboxylic acid-assisted electrodeposition of WO3 films from peroxotungstic acid. • The types of carboxylic acids control the deposition rates and microstructure. • WO3 grain sizes and effective grain boundary areas determine the photocurrents. • Maximal photocurrent measured in the smallest-aggregate films (∼ 83 nm)

  17. Nucleic Acid-Peptide Complex Phase Controlled by DNA Hybridization

    Vieregg, Jeffrey; Lueckheide, Michael; Leon, Lorraine; Marciel, Amanda; Tirrell, Matthew

    When polyanions and polycations are mixed, counterion release drives formation of polymer-rich complexes that can either be solid (precipitates) or liquid (coacervates) depending on the properties of the polyelectrolytes. These complexes are important in many fields, from encapsulation of industrial polymers to membrane-free segregation of biomolecules such as nucleic acids and proteins. Condensation of long double-stranded DNA has been studied for several decades, but comparatively little attention has been paid to the polyelectrolyte behavior of oligonucleotides. We report here studies of DNA oligonucleotides (10 - 88 nt) complexed with polylysine (10 - 100 aa). Unexpectedly, we find that the phase of the resulting complexes is controlled by the hybridization state of the nucleic acid, with double-stranded DNA forming precipitates and single-stranded DNA forming coacervates. Stability increases with polyelectrolyte length and decreases with solution salt concentration, with complexes of the longer double-stranded polymers undergoing precipitate/coacervate/soluble transitions as ionic strength is increased. Mixing coacervates formed by complementary single-stranded oligonucleotides results in precipitate formation, raising the possibility of stimulus-responsive material design.

  18. Thermochemical properties of rare earth complexes with salicylic acid

    Fourteen rare earth complexes with salicylic acid RE(HSal)3.nH2O (HSal = C7H5O3; RE = La-Sm, n = 2; RE = Eu-Lu, n = 1) were synthesized and characterized by elemental analysis, and their thermal decomposition mechanism were studied with TG-DTG technology. The constant-volume combustion energies of complexes, ΔcU, were determined by a precise rotating-bomb calorimeter at 298.15 K. Their standard molar enthalpies of combustion, ΔcHm0, and standard molar enthalpies of formation, ΔfHmo, were calculated

  19. Processing and Characterization of Cellulose Nanocrystals/Polylactic Acid Nanocomposite Films

    Erin M. Sullivan

    2015-12-01

    Full Text Available The focus of this study is to examine the effect of cellulose nanocrystals (CNC on the properties of polylactic acid (PLA films. The films are fabricated via melt compounding and melt fiber spinning followed by compression molding. Film fracture morphology, thermal properties, crystallization behavior, thermo-mechanical behavior, and mechanical behavior were determined as a function of CNC content using scanning electron microscopy, differential scanning calorimetry, X-ray diffraction, dynamic mechanical analysis, and tensile testing. Film crystallinity increases with increasing CNC content indicating CNC act as nucleating agents, promoting crystallization. Furthermore, the addition of CNC increased the film storage modulus and slightly broadened the glass transition region.

  20. Injectable hydrogels derived from phosphorylated alginic acid calcium complexes

    Phosphorylation of sodium alginate salt (NaAlg) was carried out using H3PO4/P2O5/Et3PO4 followed by acid–base reaction with Ca(OAc)2 to give phosphorylated alginic acid calcium complexes (CaPAlg), as a water dispersible alginic acid derivative. The modified alginate derivatives including phosphorylated alginic acid (PAlg) and CaPAlg were characterized by nuclear magnetic resonance spectroscopy for 1H, and 31P nuclei, high resolution inductively coupled plasma optical emission spectroscopy, Fourier transform infrared spectroscopy, and thermogravimetric analysis. CaPAlg hydrogels were prepared simply by mixing CaPAlg solution (2 w/v%) with NaAlg solution (2 w/v%) in various ratios (2:8, 4:6, 6:4, 8:2) of volume. No additional calcium salts such as CaSO4 or CaCl2 were added externally. The gelation was completed within about 3–40 min indicating a high potential of hydrogel delivery by injection in vivo. Their mechanical properties were tested to be ≤ 6.7 kPa for compressive strength at break and about 8.4 kPa/mm for elastic modulus. SEM analysis of the CaPAlg hydrogels showed highly porous morphology with interconnected pores of width in the range of 100–800 μm. Cell culture results showed that the injectable hydrogels exhibited comparable properties to the pure alginate hydrogel in terms of cytotoxicity and 3D encapsulation of cells for a short time period. The developed injectable hydrogels showed suitable physicochemical and mechanical properties for injection in vivo, and could therefore be beneficial for the field of soft tissue engineering. - Highlights: • Preparation of water-soluble alginic acid complexes with calcium phosphate • Self-assembly of the phosphorylated alginic acid calcium complexes with sodium alginate • Preparation of injectable hydrogels with diverse gelation times within about 3–40 min

  1. Ionic products of metal complexes with dithiocarbonic acid derivatives

    Ionic products of the complexes of certain sulfide-forming metal ions (In, Cd, Te, etc.) with alkyl derivates of dithiocarbonic acid have been defined. The possibility to use ionic products of alkyl xanthates for predicting the practicability of employing alkyl xanthates as analytic reagents in titrimetric methods of analysis, in extractional methods of separation and determination of elements, increase in the determination selectivity, is shown. 11 refs., 1 fig., 1 tab

  2. Technology of complex cleaning of mine acidic waters

    It is shown, that problem of complex use of mine waters includes two tasks: its cleaning and use of these waters in capacity of hydro-mineral raw. The floatation-extraction technology of mine acidic waters reprocessing is developed. The possibility of extraction processing of foam products of floatation with purpose of selective isolation of valuable components (Co, Ni, Sc, numerous of rare elements) is considered, optimum modes of metal extraction are defined. (author)

  3. Metallic Langmuir and Langmuir-Blodgett films based on TTF derivatives and fatty acid

    Recent progress in the metallic conducting Langmuir-Blodgett (LB) films built from TTF derivative and fatty acids is reported. A simple LB method of transferring the mixed Langmuir (L) film of BEDO-TTF (BO) and stearic acid (SA) onto substrates provided metallic conducting LB films. A homogeneous L film formation on the water surface observed by Brewster angle microscope (BAM) is an essential factor for the well-ordered LB films. In the L film, the carboxylate group of fatty acid forms anion layer bringing about a spontaneous formation of mixed valence state (MVS) of BO layer. Similar spontaneous formation was also found in the molecular combination of nonoxygen-substituted donor of EDT-TTF and octadecanesulfonic acid (OS). This type of reaction would be useful for obtaining conducting LB films. For the LB films of BEDO-TTF and stearic acid, we found a negative transverse magnetoresistance at low temperature that was interpreted in the weak localization of a two-dimensional (2D) electronic system based on the well-defined conducting layer

  4. Effect of inclusion complex on nitrous acid reaction with flavonoids

    Khalafi, Lida; Rafiee, Mohammad; Sedaghat, Sajjad

    2011-10-01

    The kinetic of the nitrous acid reactions with quercetin and catechin has been studied using spectrophotometric method in aqueous solution. The results show that these antioxidants participate in oxidation reactions with nitrous acid which is derived from protonation of nitrite ion in mild acidic conditions. Corresponding o-quinones as relatively stable products were detected by spectrophotometric techniques. pH dependence of the reactions has been examined and the rate constants of reactions were obtained by non-linear fitting of kinetic profiles. The effect of β-cyclodextrin on the oxidation pathway was another object of this study. It is shown that β-cyclodextrin has an inhibitory effect on the oxidation reaction. The rate constants of oxidation reactions for complexed forms and their stability constants were obtained based on changes in the reaction rates as a function of β-cyclodextrin concentration.

  5. Degradation and miscibility of poly(DL-lactic acid)/poly(glycolic acid) composite films: Effect of poly(DL-lactic-co-glycolic acid)

    Zhigang Ma; Na Zhao; Chengdong Xiong

    2012-08-01

    The in vitro degradation behaviour of poly(glycolic acid) (PGA) and its composite films containing poly(DL-lactic acid) (PDLLA) and poly(DL-lactic-co-glycolic acid) (PDLGA) were investigated via mass loss, scanning electron microscopy (SEM) and differential scanning calorimetry (DSC). All the films were prepared by solution casting, using 1,1,1,3,3,3-hexafluoro-2-propanol (HFIP) as the solvent. Since the degradation rate of PDLLA is lower than that of PGA, those of the PDLLA/PGA composite films decreased. As a compatibilizer, PDLGA improved the compatibility and hydrolytic stability of PDLLA/PGA composite films. Changes in the composite films indicate that this kind of PGA-based composite biomaterial may be applicable to device design for clinical application in the future.

  6. Estimating the acidity of transition metal hydride and dihydrogen complexes by adding ligand acidity constants.

    Morris, Robert H

    2014-02-01

    A simple equation (pKa(THF) = ∑AL + Ccharge + Cnd + Cd6) can be used to obtain an estimate of the pKa of diamagnetic transition metal hydride and dihydrogen complexes in tetrahydrofuran, and, by use of conversion equations, in other solvents. It involves adding acidity constants AL for each of the ligands in the 5-, 6-, 7-, or 8-coordinate conjugate base complex of the hydride or dihydrogen complex along with a correction for the charge (Ccharge = -15, 0 or 30 for x = +1, 0 or -1 charge, respectively) and the periodic row of the transition metal (Cnd = 0 for 3d or 4d metal, 2 for 5d metal) as well as a correction for d(6) octahedral acids (Cd6 = 6 for d(6) metal ion in the acid, 0 for others) that are not dihydrogen complexes. Constants AL are provided for 13 commonly occurring ligand types; of these, nine neutral ligands are correlated with Lever's electrochemical ligand parameters EL. This method gives good estimates of the over 170 literature pKa values that range from less than zero to 50 with a standard deviation of 3 pKa units for complexes of the metals chromium to nickel, molybdenum, ruthenium to palladium, and tungsten to platinum in the periodic table. This approach allows a quick assessment of the acidity of hydride complexes found in nature (e.g., hydrogenases) and in industry (e.g., catalysis and hydrogen energy applications). The pKa values calculated for acids that have bulky or large bite angle chelating ligands deviate the most from this correlation. The method also provides an estimate of the base strength of the deprotonated form of the complex. PMID:24410025

  7. Quantification of Acidic Compounds in Complex Biomass-Derived Streams

    Karp, Eric M.; Nimlos, Claire T.; Deutch, Steve; Salvachua, Davinia; Cywar, Robin M.; Beckham, Gregg T.

    2016-09-07

    Biomass-derived streams that contain acidic compounds from the degradation of lignin and polysaccharides (e.g. black liquor, pyrolysis oil, pyrolytic lignin, etc.) are chemically complex solutions prone to instability and degradation during analysis, making quantification of compounds within them challenging. Here we present a robust analytical method to quantify acidic compounds in complex biomass-derived mixtures using ion exchange, sample reconstitution in pyridine and derivatization with BSTFA. The procedure is based on an earlier method originally reported for kraft black liquors and, in this work, is applied to identify and quantify a large slate of acidic compounds in corn stover derived alkaline pretreatment liquor (APL) as a function of pretreatment severity. Analysis of the samples is conducted with GCxGC-TOFMS to achieve good resolution of the components within the complex mixture. The results reveal the dominant low molecular weight components and their concentrations as a function of pretreatment severity. Application of this method is also demonstrated in the context of lignin conversion technologies by applying it to track the microbial conversion of an APL substrate. Here too excellent results are achieved, and the appearance and disappearance of compounds is observed in agreement with the known metabolic pathways of two bacteria, indicating the sample integrity was maintained throughout analysis. Finally, it is shown that this method applies more generally to lignin-rich materials by demonstrating its usefulness in analysis of pyrolysis oil and pyrolytic lignin.

  8. Chloroform extraction of ethyl xanthate complexes from sulphuric acid media

    The chloroform extraction of 30 elements (Fe, Co, Ni, Zn, Cd, Ge, Sn, V, As, Sb, Bi, Cu, Ag, Au, Mn, Re, Ga, In, Tl, Se, Te, Cr, Mo, U, Pt, Pd, Rh, Ir, Ru and Ce) from 0.1 to 8 M sulphuric acid in the presence of potassium ethyl xanthate has been studied. Pd(II), Bi, As(III), Sb(III), Se(IV) and Te(IV) are completely extracted and Au(III) is largely extracted over the range of acid concentration investigated. Fe(II), Tl(I), Rh(III) and Cr(VI) are only slightly extracted and Se(VI), Te(VI), Ru(III), Cr(III), Mn(II), Zn, Ce(IV), Ir(IV) and Ge(IV) are not extracted at all. Depending on the acid concentration, the remaining elements are all partly extracted. Results are compared with those obtained in an earlier study of the extraction of xanthate complexes from hydrochloric acid media. The processes involved in the formation of some xanthate complexes and potential analytical separations are discussed. (author)

  9. complex formation of americium (III) with humic acid

    The presence of humic substances in natural waters will modify the migration behavior of actinides in the geosphere due to the strong reaction properties of these ligands with actinides. Therefore, the possible reactions of humic acid with actinides have been studied widely in recent years. The complex formation of Am(III) with humic acid is studied with solvent extraction technique. The experiments are performed in the pH range from 4.0 to 8.0 in 0.1 mol/kg NaClO4 solution at ambient temperature. Experimental results show that the complex formation constants of Am(III) with humic acid are varied with the variation of pH value in solution. 1:2 complex is obtained in the experiments and the complex formation constants determined at each pH are: lgβ1 = 6.56 +- 0.05, lgβ2 = 10.77 +- 0.31 at pH 4.0. lgβ1 = 7.94 +- 0.11, lgβ2 = 11.80 +- 0.21 at pH = 5.0. lgβ1 = 10.74 +- 0.28, lgβ2 = 12.88 +- 0.49 at pH = 6.0. lgβ1 = 12.85 +- 0.30, lgβ2 = 14.80 +- 0.62 at pH = 7.0. lgβ1 = 14.88 +- 0.48, lgβ2 = 15.65 +- 0.69 at pH = 8.0, respectively. The dependence of the complex formation constant on pH is: lgβ1 = 2.16 (+-0.98)pH-2.34(+-0.93),lgβ2 1.28(+-1.04)pH+5.52(+-1.21), respectively

  10. Synthesis of thin film containing 4-amino-1,2,4-triazole iron(II) complexes

    Onggo, Djulia, E-mail: djulia@Chem.itb.ac.id [Inorganic and Physical Chemistry Research Group, Faculty of Mathematics and Natural Sciences, Institut Teknologi Bandung, Jl. Ganesha 10 Bandung 40132 (Indonesia)

    2014-03-24

    The Iron(II) complex with 4-amino-1,2,4 triazole (NH{sub 2}-trz) ligand has potential applications as smart material since the compounds show a distinct color change from lilac at low temperature to colorless at high temperature. The lilac color of the complex represent the diamagnetic low spin state while the colorless correspond to the paramagnetic high spin state of iron(II). The transition between the two states could be tuned by changing the anionic group. Generally, the complex was synthesized directly from aqueous solution of iron(II) salt with considerable amounts of NH{sub 2}-trz solution produced solid powder compound. For application as an electronic molecular device, the complex should be obtained as a thin film. The transparent [Fe(NH{sub 2}trz){sub 3}]-Nafion film has been successfully obtained, however, no anion variation can be produced since the nafion is an anionic resin. In this work, the [Fe(NH{sub 2}trz){sub 3}]-complexes with several anions have been synthesized inside nata de coco membrane that commonly used as a medium for deposition metal nano-particles. After drying the membrane containing the complex became a thin film. At room temperature, the film containing iron(II) complexes of sulphate and nitrate salts show lilac color, similar to that of the original complexes in the powder form. On heating, the color of the complex film changed to colorless and this color change was observed reversibly. In contrast, the films containing perchlorate and tetrafluoroborate iron(II) complexes are colorless at room temperature and changed to lilac on cooling. The significant color changing of the iron(II)complexes in the nata de coco film can be used for demonstration thermo chromic effect of smart materials with relatively small amount of the compounds.

  11. Synthesis of thin film containing 4-amino-1,2,4-triazole iron(II) complexes

    The Iron(II) complex with 4-amino-1,2,4 triazole (NH2-trz) ligand has potential applications as smart material since the compounds show a distinct color change from lilac at low temperature to colorless at high temperature. The lilac color of the complex represent the diamagnetic low spin state while the colorless correspond to the paramagnetic high spin state of iron(II). The transition between the two states could be tuned by changing the anionic group. Generally, the complex was synthesized directly from aqueous solution of iron(II) salt with considerable amounts of NH2-trz solution produced solid powder compound. For application as an electronic molecular device, the complex should be obtained as a thin film. The transparent [Fe(NH2trz)3]-Nafion film has been successfully obtained, however, no anion variation can be produced since the nafion is an anionic resin. In this work, the [Fe(NH2trz)3]-complexes with several anions have been synthesized inside nata de coco membrane that commonly used as a medium for deposition metal nano-particles. After drying the membrane containing the complex became a thin film. At room temperature, the film containing iron(II) complexes of sulphate and nitrate salts show lilac color, similar to that of the original complexes in the powder form. On heating, the color of the complex film changed to colorless and this color change was observed reversibly. In contrast, the films containing perchlorate and tetrafluoroborate iron(II) complexes are colorless at room temperature and changed to lilac on cooling. The significant color changing of the iron(II)complexes in the nata de coco film can be used for demonstration thermo chromic effect of smart materials with relatively small amount of the compounds

  12. Tuning the properties of polyhydroxybutyrate films using acetic acid via solvent casting

    Anbukarasu, Preetam; Sauvageau, Dominic; Elias, Anastasia

    2015-12-01

    Biodegradable polyhydroxybutyrate (PHB) films were fabricated using acetic acid as an alternative to common solvents such as chloroform. The PHB films were prepared using a solvent casting process at temperatures ranging from 80 °C to 160 °C. The crystallinity, mechanical properties and surface morphology of the films cast at different temperatures were characterized and compared to PHB films cast using chloroform as a solvent. Results revealed that the properties of the PHB film varied considerably with solvent casting temperature. In general, samples processed with acetic acid at low temperatures had comparable mechanical properties to PHB cast using chloroform. This acetic acid based method is environmentally friendly, cost efficient and allows more flexible processing conditions and broader ranges of polymer properties than traditional methods.

  13. Ascorbic acid-containing whey protein film coatings for control of oxidation.

    Min, Seacheol; Krochta, John M

    2007-04-18

    A formulation for the whey protein isolate film or coating incorporating ascorbic acid (AA-WPI film or coating) was developed. Tensile and oxygen-barrier properties of the AA-WPI film were measured. Antioxidant effects of the AA-WPI coating on roasted peanuts were studied by comparing the values of peroxide (PO), thiobarbituric acid reactive substance (TBARS), and free-radical-scavenging activity, determined with noncoated peanuts and peanuts coated with WPI with and without ascorbic acid during storage at 21% relative humidity (RH) and 23, 35, and 50 degrees C. The incorporation of AA reduced elongation of WPI films. The oxygen-barrier property of the WPI film was significantly improved by incorporation of AA. The AA-WPI coating retarded lipid oxidation in peanuts significantly at 23, 35, and 50 degrees C. The AA-WPI coated peanuts were more red than noncoated peanuts at all storage temperatures. PMID:17367158

  14. Complex surfaces plated by thin-film deposition in one operation

    Buckley, D. H.; Przybyszewski, J. S.; Spalvins, T.

    1967-01-01

    Ion plating deposits thin film on complex surface in one operation. The ionized materials follow electric lines of force to all points on the objects, uniformly plating the surface from all sides simultaneously.

  15. Modification of hydrophobic polypeptide-based film by blending with hydrophilic poly(acrylic acid)

    Guoquan Zhu; Fagang Wang; Qiaochun Gao; Yuying Liu

    2013-01-01

    In this study, a series of poly(γ-benzyl L-glutamate)/poly(acrylic acid) (PBLG/PAA) polymer blend films were prepared by casting the polymer blend solution in dimethylsulfoxide (DMSO). The structure and morphology of the polymer blend film were investigated by Fourier Transform Infrared Spectroscopy (FT-IR) and Scanning Electron Microscopy (SEM). Thermal, mechanical, and chemical properties of PBLG/PAA polymer blend films were studied by Differential Scanning Calorimetry (DSC), Thermogra...

  16. Enhanced high temperature thermoelectric response of sulphuric acid treated conducting polymer thin films

    Kumar, Sarath

    2015-11-24

    We report the high temperature thermoelectric properties of solution processed pristine and sulphuric acid treated poly(3, 4-ethylenedioxythiophene):poly(4-styrenesulfonate) (or PEDOT:PSS) films. The acid treatment is shown to simultaneously enhance the electrical conductivity and Seebeck coefficient of the metal-like films, resulting in a five-fold increase in thermoelectric power factor (0.052 W/m. K ) at 460 K, compared to the pristine film. By using atomic force micrographs, Raman and impedance spectra and using a series heterogeneous model for electrical conductivity, we demonstrate that acid treatment results in the removal of PSS from the films, leading to the quenching of accumulated charge-induced energy barriers that prevent hopping conduction. The continuous removal of PSS with duration of acid treatment also alters the local band structure of PEDOT:PSS, resulting in simultaneous enhancement in Seebeck coefficient.

  17. Biodegradable films containing {alpha}-tocopherol/{beta}-cyclodextrin complex; Filmes biodegradaveis contendo {alpha}-tocoferol complexado em {beta}-ciclodextrina

    Motta, Caroline; Martelli, Silvia M.; Soldi, Valdir, E-mail: vsoldi@qmc.ufsc.br [Lab. de Materiais Polimericos (POLIMAT), Dept. de Quimica, Universidade Federal de Santa Catarina, Florianopolis, SC (Brazil); Barreto, Pedro L.M. [Lab. de Reologia (REOLAB), Dept. de Ciencia e Tecnologia de Alimentos, Universidade Federal de Santa Catarina, Florianopolis, SC (Brazil)

    2011-07-01

    The growing environmental concern about pollution and the need to reduce dependence of plastic industry in relation to non-renewable resources has increased the interest of both researchers and industry in the use of biopolymers. In this work {beta}-cyclodextrin/{alpha}-tocopherol complexes were prepared and characterized. In order to obtain polymeric active biofilms, the {beta}-cyclodextrin/{alpha}-tocopherol complex was incorporated into a polymeric matrix of carboxymethylcellulose. The {beta}-cyclodextrin/{alpha}-tocopherol complex was characterized through of X-ray diffraction and thermogravimetric analysis. The physicochemical properties of the films incorporated with the complex were evaluated through mechanical and colorimetric analysis and moisture sorption isotherm. (author)

  18. Preparation of poly(lactic acid) and pectin composite films intended for application in antimicrobial packaging

    Composite films of pectin and poly(lactic acid) (PLA) were compounded by extrusion. A model antimicrobial polypeptide, nisin, was loaded into the film by diffusion. The incorporation of pectin into PLA resulted in a heterogeneous biphasic structure as revealed by scanning electronic microscopy, co...

  19. Chemical modification of chitosan film via surface grafting of citric acid molecular to promote the biomineralization

    Liu, Yang; Shen, Xin; Zhou, Huan; Wang, Yingjun; Deng, Linhong

    2016-05-01

    We develop a novel chitosan-citric acid film (abbreviated as CS-CA) suitable for biomedical applications in this study. In this CS-CA film, the citric acid, which is a harmless organic acid has been extensively investigated as a modifying agent on carbohydrate polymers, was cross-linked by 1-Ethyl-3-(3-dimethyl aminopropyl) carbodiimide (EDC) and N-hydroxysuccinimide (NHS) onto the surface of chitosan (CS) film. Fourier transform infrared spectroscopy (FTIR) and X-ray photoelectron spectroscopy (XPS) confirms the graft copolymerization of the modified chitosan film (CS-CA). Surface wettability, moisturizing performance, the capacity of mineralization in vitro and biocompatibility of the films were characterized. After modification, this CS-CA film has good hydrophilicity. It is very evident that the citric acid grafting treatment significantly promotes the biomineralization of the chitosan based substrates. Cell experiments show that the MC3T3-E1 osteoblasts can adhere and proliferate well on the surface of CS-CA film. This CS-CA film, which can be prepared in large quantities and at low cost, should have potential application in bone tissue engineering.

  20. Multilayer Film Fabrication and Photoelectric Conversion Property of Two Pyrrolidinofullerene Carboxylic Acid Derivatives

    2000-01-01

    Two multilayer films of pyrrolidinofullerene carboxylic acid derivatives, which exhibit photoelectric conversion property, are reported here. The first monolayers were fabricated on hydrophilic indium-tin-oxide (ITO), quartz, and mica by esterification reaction. The multilayers were characterized by contact angle and UV spectrum. The photoelectric conversion properties of both multilayer films were studied.

  1. Poly(lactic acid) and Osage Orange Wood Fiber Composites for Agricultural Mulch Films

    Osage orange wood(OO)was combined with poly(lactic acid)(PLA)to form a polymer composite intended for use as an agricultural mulch film. The PLA-OO mechanical properties were comparable to existing mulch film products and had the advantage of being completely biodegradable through a single growing ...

  2. Preparation and acetone sensitive characteristics of nano-LaFeO3 semiconductor thin films by polymerization complex method

    Perovskite structure nano-LaFeO3 thin films were prepared by polymerization complex method using La(NO3)3.6H2O, FeCl3.6H2O as raw materials, citric acid (CA) as chelating agent and ethylene glycol (EG) as cross-linking agent. Nano-LaFeO3 thin films were fabricated on Al2O3 substrates by dip-coating, drying, pre-heating and sintering. The precursor and thin films were characterized by IR, AFM, XRD and SEM. The results revealed that the homogeneous LaFeO3 thin films with the grain size of about 37 nm and the thickness of approximately 2 μm were successfully synthesized at the sintering temperature of 650 deg. C. The nano-LaFeO3 semiconductor thin films have higher sensitive to acetone gas with lower concentration, which exposed to 80 ppm acetone gas show that sensitivity are 204, and response time are within 15 s at the testing temperature of 400 deg. C

  3. An iron(II) diketonate–diamine complex as precursor for thin film fabrication by atomic layer deposition

    Bratvold, Jon E., E-mail: j.e.bratvold@kjemi.uio.no [Centre for Materials Science and Nanotechnology (SMN)/Department of Chemistry, University of Oslo, PO Box 1033, Blindern, N-0315 Oslo (Norway); Carraro, Giorgio [Department of Chemistry, University of Padova and INSTM, via F. Marzolo 1, I-35131 Padova (Italy); Barreca, Davide [CNR-IENI and INSTM, Department of Chemistry, University of Padova, via F. Marzolo 1, I-35131 Padova (Italy); Nilsen, Ola [Centre for Materials Science and Nanotechnology (SMN)/Department of Chemistry, University of Oslo, PO Box 1033, Blindern, N-0315 Oslo (Norway)

    2015-08-30

    Highlights: • First report of Fe(hfa){sub 2}TMEDA as precursor in ALD and MLD. • Hybrid organic–inorganic films with oxalic acid as co-reactant between 125 and 350 °C. • Surface saturation evidenced by quartz crystal microbalance (QCM) analysis. • XPS confirms complete preservation of Fe(II) from precursor to film. • Deposition of α-Fe{sub 2}O{sub 3} when using ozone as co-reactant. - Abstract: A new divalent Fe precursor has been explored for deposition of iron-containing thin films by atomic layer deposition and molecular layer deposition (ALD/MLD). The Fe(II) β-diketonate-diamine complex, Fe(hfa){sub 2}TMEDA, (hfa = 1,1,1,5,5,5-hexafluoro-2,4-pentanedionate, TMEDA = N,N,N′,N′-tetramethylethylenediamine) can be handled in air, and sublimation at 60 °C ensures a satisfactory vaporization rate. The reactivity of the precursor does not allow for direct reaction with water as co-reactant. Nevertheless, it reacts with carboxylic acids, resulting in organic–inorganic hybrid materials, and with ozone, yielding α-Fe{sub 2}O{sub 3}. The divalent oxidation state of iron was maintained during deposition when oxalic acid was used as co-reactant, demonstrating the first preservation of Fe(II) from precursor to film during an MLD process. A self-saturating growth mode was proven by in situ quartz crystal microbalance (QCM) measurements, and the films were further characterized by grazing incidence X-ray diffraction (GIXRD), Fourier transform infrared spectroscopy (FTIR), and X-ray photoelectron spectroscopy (XPS)

  4. An iron(II) diketonate–diamine complex as precursor for thin film fabrication by atomic layer deposition

    Highlights: • First report of Fe(hfa)2TMEDA as precursor in ALD and MLD. • Hybrid organic–inorganic films with oxalic acid as co-reactant between 125 and 350 °C. • Surface saturation evidenced by quartz crystal microbalance (QCM) analysis. • XPS confirms complete preservation of Fe(II) from precursor to film. • Deposition of α-Fe2O3 when using ozone as co-reactant. - Abstract: A new divalent Fe precursor has been explored for deposition of iron-containing thin films by atomic layer deposition and molecular layer deposition (ALD/MLD). The Fe(II) β-diketonate-diamine complex, Fe(hfa)2TMEDA, (hfa = 1,1,1,5,5,5-hexafluoro-2,4-pentanedionate, TMEDA = N,N,N′,N′-tetramethylethylenediamine) can be handled in air, and sublimation at 60 °C ensures a satisfactory vaporization rate. The reactivity of the precursor does not allow for direct reaction with water as co-reactant. Nevertheless, it reacts with carboxylic acids, resulting in organic–inorganic hybrid materials, and with ozone, yielding α-Fe2O3. The divalent oxidation state of iron was maintained during deposition when oxalic acid was used as co-reactant, demonstrating the first preservation of Fe(II) from precursor to film during an MLD process. A self-saturating growth mode was proven by in situ quartz crystal microbalance (QCM) measurements, and the films were further characterized by grazing incidence X-ray diffraction (GIXRD), Fourier transform infrared spectroscopy (FTIR), and X-ray photoelectron spectroscopy (XPS)

  5. Electrophoretic deposition of composite halloysite nanotube–hydroxyapatite–hyaluronic acid films

    Deen, I. [Department of Materials Science and Engineering, McMaster University, 1280 Main Street West, Hamilton, Ontario, Canada L8S 4L7 (Canada); Zhitomirsky, I., E-mail: zhitom@mcmaster.ca [Department of Materials Science and Engineering, McMaster University, 1280 Main Street West, Hamilton, Ontario, Canada L8S 4L7 (Canada)

    2014-02-15

    Highlights: ► Composite halloysite nanotubes–hydroxyapatite–hyaluronic acid films were prepared. ► Electrophoretic deposition method was used for deposition. ► Natural hyaluronic acid was used as a dispersing, charging and film forming agent. ► Film composition and deposition yield can be varied. ► The films can be used for biomedical implants with controlled release of drugs. -- Abstract: Electrophoretic deposition method has been developed for the deposition of biocomposite films containing halloysite nanotubes (HNTs), hydroxyapatite (HA) and hyaluronic acid. The method is based on the use of natural hyaluronate biopolymer as a dispersing and charging agent for HNT and HA and film forming agent for the fabrication of the composite films. The deposition kinetics was studied by the quartz crystal microbalance method. The composite films were studied by X-ray diffraction, thermogravimetric analysis, differential thermal analysis and electron microscopy. The composite films are promising materials for the fabrication of biomedical implants with advanced functional properties.

  6. Electrophoretic deposition of composite halloysite nanotube–hydroxyapatite–hyaluronic acid films

    Highlights: ► Composite halloysite nanotubes–hydroxyapatite–hyaluronic acid films were prepared. ► Electrophoretic deposition method was used for deposition. ► Natural hyaluronic acid was used as a dispersing, charging and film forming agent. ► Film composition and deposition yield can be varied. ► The films can be used for biomedical implants with controlled release of drugs. -- Abstract: Electrophoretic deposition method has been developed for the deposition of biocomposite films containing halloysite nanotubes (HNTs), hydroxyapatite (HA) and hyaluronic acid. The method is based on the use of natural hyaluronate biopolymer as a dispersing and charging agent for HNT and HA and film forming agent for the fabrication of the composite films. The deposition kinetics was studied by the quartz crystal microbalance method. The composite films were studied by X-ray diffraction, thermogravimetric analysis, differential thermal analysis and electron microscopy. The composite films are promising materials for the fabrication of biomedical implants with advanced functional properties

  7. Sol-gel silica films embedding NIR- emitting Yb-quinolinolate complexes

    Sol-gel silica thin films embedding an ytterbium quinolinolato complex (YbClQ4) have been obtained using different alkoxides. Homogeneous, crack- and defect-free thin films of optical quality have been successfully deposited on glass substrate by dip-coating. The silica thin films have been characterized by time-resolved photoluminescence. The luminescence properties of the YbClQ4 are preserved in silica films prepared through an optimized sol-gel approach. The excited state lifetime of the lanthanide is comparable to those observed in bulk and longer than the corresponding ones in solution

  8. Self-assembled monolayer and multilayer formation using redox-active Ru complex with phosphonic acids on silicon oxide surface

    The formation of self-assembled monolayer and multilayer using redox-active Ru complex molecules with phosphonic acids on SiO2 surface has been examined using X-ray photoelectron spectroscopy (XPS), ellipsometry, and time of flight secondary mass-ion spectroscopy (TOF-SIMS). We found that an introduction of a Zr adlayer leads to higher surface molecular density of Ru complex SAMs on the SiO2 surface, compared to that of obtained from the direct adsorption of Ru complex monolayer on the SiO2 surface. We further tried to fabricate a multilayer film using this molecule with Zr(IV) ion acting as a chemical glue by a successive immersion process. The XPS data revealed that the molecular densities of the multilayers were also higher for the immobilization with Zr adlayer between Ru complex and SiO2 surface than those without the Zr adlayer, suggesting that Zr adlayer is effective in forming highly packed molecular layer of phosphonic acids on SiO2 surface. We found the film growth reached a saturation point after 6 layers on the SiO2 surface. The film growth saturation can be explained by a molecular domain boundary effect encountered due to the large tilt angle of the molecular layer.

  9. Complexes of carborane acids linked by strong hydrogen bonds: acidity scales.

    Grabowski, Sławomir J

    2016-06-28

    Carborane acids, currently known as the strongest acis, are analyzed and compared with other species classified as superacids as well as with selected mineral acids and carbocations. Calculations (B3LYP/6-311++G(d,p) level) on these moieties as well as on their conjugate bases were performed to evaluate corresponding proton affinities. In addition, the complexes of these species with the CHB11F11(-) anion and the complexes of the conjugate bases with the trimethylammonium cation were analyzed. The scales, based on spectroscopic results, DFT energies and on the topological QTAIM (Quantum Theory of Atoms in Molecules) parameters, are introduced and discussed to order the acidity of the species analyzed here. The properties of the bond critical points corresponding to the intermolecular contacts are discussed. The majority of the results show that HCHB11F11 carborane acid is the strongest in agreement with the previous experimental studies of Reed and coworkers. Very often the abovementioned acidity scales show that carborane acids are able to protonate hydrocarbons. PMID:27253195

  10. Characterization and Tribological Behavior of Octadecene, Dodecene and Undecenoic Acid Films on Si Substrate

    Jinfang ZHOU; Shengrong YANG

    2005-01-01

    The films of octadecene, dodecene, and undecenoic acid were prepared on H-terminated Si surface in the presence of ultraviolet irradiation. The resulted films were characterized with water-contact angle measurement and infrared spectroscopy. The friction-reducing behavior of the prepared films was examined on a static-dynamic friction coefficient measurement apparatus and on an atomic force microscope. It was found that all the reacted films on the Si substrate showed good friction-reducing ability; especially, the film of the octadecene exhibited the best frictionreducing ability. This was attributed to the transfer of the reacted films onto the counter face with formation of a transfer film on the counterpart surface, which led to the transformation of the sliding between the reacted films and the hard ceramic to that between the reacted films and its transfer film on the counterpart surface. The macroscopic and microscopic friction behaviors of the prepared films were dependent on their molecular chain lengths. Thus the octadecene reacted film with the highest degree of ordering arrangement showed the best friction-reducing and antiwear abilities in sliding against Si3 N4.

  11. Preparation and Properties of Moisture-absorbing Film Impregnated with Polyacrylic Acid Partial Sodium Salt Material

    Lee, Youn Suk; Park, Insik [Yonsei University, Wonju (Korea, Republic of); Choi, Hong Yeol [CJ Cheiljedang, Seoul (Korea, Republic of)

    2014-08-15

    Moisture is a major factor causing the deteriorative physical change, microbial growth, and chemical reaction of the products. In this study, the moisture absorbing composite films have been prepared with moisture absorbing material of polyacrylic acid partial sodium salt (PAPSS) impregnated on LLDPE polymer for the functional packaging applications. The results showed that PAPSS impregnated film illustrated uniformly dispersed PAPSS particles in the LLDPE polymer matrix. The transparency of the PAPSS impregnated film decreased slightly at higher PAPSS concentrations. An increase in the PAPSS content for moisture-absorbing films showed a similar decrease in tensile strength, percent elongation at break, and tear strength. Their values of films impregnated with PAPSS of 0.5, 1, and 2% showed no significant difference. Meanwhile, 4% PAPSS films significantly decreased the values of mechanical properties compared to the films impregnated with different PAPSS levels. Values of the oxygen permeability and water vapor permeability for PAPSS impregnated films decreased significantly with greater PAPSS. The results indicate that 4% PAPSS impregnated in LLDPE films had high affinity of moisture absorbencies compared to the other films. The mathematical equation that best described the moisture sorption isotherm of each film sample was the GAB equation at 25 .deg. C. The crystallization and melting temperatures of PAPSS films were influenced by the addition of PAPSS material, but showed good thermal stability.

  12. Enhancement of the wet properties of transparent chitosan-acetic-acid-salt films using microfibrillated cellulose.

    Nordqvist, David; Idermark, Johan; Hedenqvist, Mikael S; Gällstedt, Mikael; Ankerfors, Mikael; Lindström, Tom

    2007-08-01

    This report presents a new route to enhance the wet properties of chitosan-acetic-acid-salt films using microfibrillated cellulose (MFC). The enhancement makes it easier to form chitosan-acetic-acid-salt films into various shapes at room temperature in the wet state. Chitosan with MFC was compared with the well-known buffer treatment. It was observed that films containing 5 wt % MFC were visually identical to the buffered/unbuffered films without MFC. Field-emission scanning electron microscopy indicated that MFC formed a network with uniformly distributed fibrils and fibril bundles in the chitosan matrix. The addition of MFC reduced the risk of creases and deformation in the wet state because of a greater wet stiffness. The wet films containing MFC were also extensible. Although the stiffness, strength and extensibility were highest for the buffered films, the wet strength of the MFC-containing unbuffered films was sufficient for wet forming operations. The effects of MFC on the mechanical properties of the dry chitosan films were small or absent. It was concluded that the addition of MFC is an acceptable alternative to buffering for shaping chitosan films/products in the wet state. The advantages are that the "extra" processing step associated with buffering is unnecessary and that the film matrix remains more water-soluble. PMID:17645308

  13. Radiation-induced grafting of acrylic acid onto polypropylene film and its biodegradability

    Mandal, Dev K.; Bhunia, Haripada; Bajpai, Pramod K.; Chaudhari, C. V.; Dubey, K. A.; Varshney, L.

    2016-06-01

    Polypropylene based commodity polyolefins are widely used in packaging, manufacturing, electrical, pharmaceutical and other applications. The aim of the present work is to study the effect of grafting of acrylic acid on the biodegradability of acrylic acid grafted polypropylene. The effect of different conditions showed that grafting percentage increased with increase in monomer concentration, radiation dose and inhibitor concentration but decreased with increase in radiation dose rate. The maximum grafting of 159.4% could be achieved at optimum conditions. The structure of grafted polypropylene films at different degree of grafting was characterized by EDS, FTIR, TGA, DSC, SEM and XRD. EDS studies showed that the increase in acrylic acid grafting percentage increased the hydrophilicity of the grafted films. FTIR studies indicated the presence of acrylic acid on the surface of polypropylene film. TGA studies revealed that thermal stability decreased with increase in grafting percentage. DSC studies showed that melting temperature and crystallinity of the grafted polypropylene films lower than polypropylene film. SEM studies indicated that increase in acrylic acid grafting percentage increased the wrinkles in the grafted films. The maximum biodegradability could be achieved to 6.85% for 90.5% grafting. This suggested that microorganisms present in the compost could biodegrade acrylic acid grafted polypropylene.

  14. Enhanced surface coverage and conductivity of Cu complex ink-coated films by laser sintering

    We here show that highly conductive copper films are obtainable from Cu complex ink by laser sintering. The synthesized Cu formate ink was spin-coated onto polyimide substrate and the coated films were scanned by an ultraviolet laser beam at 355 nm. During the sintering process, N2 gas was blown into the irradiated area to prevent oxidation. Unlike the typical thermal process, laser sintering resulted in tightly packed, dense structures. This made it possible to produce highly conducting thin films with uniform thickness. A minimum resistivity of 1.92 × 10−5 Ω cm was obtained. - Highlights: • Highly conductive Cu films are obtainable by sintering Cu complex ink with laser. • Laser-sintered films exhibit very uniform and dense microstructure. • A minimum resistivity of 1.92 × 10−5 Ω cm is achieved

  15. Complex formation of americium (III) with humic acid

    The presence of humic substances in natural waters will modify the migration behavior of actinides in the geosphere due to the strong reaction properties of these ligands with actinides. Therefore, the possible reactions of humic acid with actinides have been studied widely in recent years. The complex formation of Am (III) with humic acid is studied with solvent extraction technique in this paper. The experiments are performed in the pH range from 4.0 to 8.0 in 0.1 M NaClO4 solution at ambient temperature. Experimental results show that the complex formation constants of Am (III) with humic acid are varied with the variation of pH value in solution. 1:2 complex is obtained in the experiments and the complex formation constants determined at each pH are: lgβ1=6.56±0.05, lgβ2=10.77±0.31 at pH=4.0; lgβ1=7.94±0.11, lgβ2=11.80±0.21 at pH=5.0; lgβ1=10.74±0.28, lgβ2=12.88±0.49 at pH=6.0; lgβ1=12.85±0.30, lgβ2=14.80±0.62 at pH=7.0; lgβ1=14.88±0.48, lgβ2=15.65±0.69 at pH=8.0, respectively. The dependence of the complex of the complex formation constant on pH is: lgβ1=2.16(±0.98)pH-2.34(±1.03), lgβ2=1.28(±1.04)pH+5.52(±1.21), respectively. (author)

  16. From ligand to complexes: inhibition of HIV-1 Integrase by beta-diketo acid metal complexes

    Sechi, Mario; BACCHI, Alessia; Carcelli, Mauro; Fisicaro, Emilia; Rogolino, Dominga; Gates, Paul; Derudas, Marco; Al-Mawsawi, Laith Q.; Neamati, Nouri

    2006-01-01

    Recently, a class of compounds bearing a β-diketo acid moiety have emerged as the most promising lead in anti-HIV-1 IN drug discovery. It is believed that the β-diketo acid pharmacophoric motif could be involved in a functional sequestration of one or both divalent metal ions, which are critical cofactors at the enzyme catalytic site. This would subsequently block the transition state of the IN-DNA complex. In this scenario, it is of paramount importance to acquire information ...

  17. Spectrophotometric study of lanthanoid complexes with antipyrine and salicylic acid

    The extraction-spectrophotometric method has been used to study lanthanoid ion complexing (Pr, Nd, Ho and Er) with antipyrine (Ant) and salicylic acid (Sal). The component relationship in different-ligand compounds Ln:Aut:Sal=2:3:6 and solvate number equal to 5 are determined; molar extinction coefficients of binary and different-ligand compounds are calculated. Oscillator strengths of absorption bands corresponding to supersensitive transitions of neodymium, holmium, erbium and some most intensive praseodymium bands are calculated. The study of IR spectra of investigated compounds allows to conclude on formation of coordination bonds of the central atom with the antipyrine molecule through the oxygen of the carbonyl group as well as on carboxyl group hydrogen substitution for metal and formation of coordination bond with OH group in salicylic acid molecules

  18. Chemical vapour deposition of amorphous Ru(P) thin films from Ru trialkylphosphite hydride complexes.

    McCarty, W Jeffrey; Yang, Xiaoping; DePue Anderson, Lauren J; Jones, Richard A

    2012-11-21

    The ruthenium phosphite hydride complexes H(2)Ru(P(OR)(3))(4) (R = Me (1), Et (2), (i)Pr (3)) were used as CVD precursors for the deposition of films of amorphous ruthenium-phosphorus alloys. The as-deposited films were X-ray amorphous and XPS analysis revealed that they were predominantly comprised of Ru and P in zero oxidation states. XPS analysis also showed the presence of small amounts of oxidized ruthenium and phosphorus. The composition of the films was found to depend on ligand chemistry as well as the deposition conditions. The use of H(2) as the carrier gas had the effect of increasing the relative concentrations of P and O for all films. Annealing films to 700 °C under vacuum produced films of polycrystalline hcp Ru while a flowing stream of H(2) resulted in polycrystalline hcp RuP. PMID:23018487

  19. Antibacterial poly(lactic acid) (PLA) films grafting electrospun PLA/Ally isothioscyanate (AITC) fibers for food packaging

    Poly(lactic acid) (PLA) fibers of submicron sizes encapsulating allyl isothiocyanate (AITC) (PfA) were made and electrospun onto the surfaces of PLA films (PfA-g-film). SEM examination confirmed that the fibers were grafted to the PLA film after the (PfA-g-film) underwent air blowing and water washi...

  20. Highly ordered thin films prepared with octabutoxy copper phthalocyanine complexes

    Langmuir-Blodgett (LB) films of copper (II) 1,4,8,11,15,18,22,25-octabutoxyphthalocyanine, nCuPc(OBu)8, (non-peripheral substitution) and copper (II) 2,3,9,10,16,17,23,24-octabutoxyphthalocyanine, pCuPc(OBu)8, (peripheral substitution), were fabricated and characterized by optical spectroscopy and scanning probe microscopy. The LB films were transferred onto hydrophilic substrates by vertical dipping. Although they posses relatively short polar substituents both compounds form smooth, uniform, dense, and highly stable LB monolayers composed of linear arrays of cofacial oligomers. The long range discotic assemblies of LB and spun cast films of pCuPc(OBu)8 and nCuPc(OBu)8 posses physical and chemical properties favorable for molecular electronic device application

  1. Highly ordered thin films prepared with octabutoxy copper phthalocyanine complexes.

    Stevenson, Kelly; Miyashita, Naoko; Smieja, Joanne; Mazur, Ursula

    2003-01-01

    Langmuir-Blodgett (LB) films of copper (II) 1,4,8,11,15,18,22,25-octabutoxyphthalocyanine, nCuPc(OBu)(8), (non-peripheral substitution) and copper (II) 2,3,9,10,16,17,23,24-octabutoxyphthalocyanine, pCuPc(OBu)(8), (peripheral substitution), were fabricated and characterized by optical spectroscopy and scanning probe microscopy. The LB films were transferred onto hydrophilic substrates by vertical dipping. Although they posses relatively short polar substituents both compounds form smooth, uniform, dense, and highly stable LB monolayers composed of linear arrays of cofacial oligomers. The long range discotic assemblies of LB and spun cast films of pCuPc(OBu)(8) and nCuPc(OBu)(8) posses physical and chemical properties favorable for molecular electronic device application. PMID:12801680

  2. Highly ordered thin films prepared with octabutoxy copper phthalocyanine complexes

    Stevenson, Kelly; Miyashita, Naoko; Smieja, Joanne; Mazur, Ursula

    2003-10-15

    Langmuir-Blodgett (LB) films of copper (II) 1,4,8,11,15,18,22,25-octabutoxyphthalocyanine, nCuPc(OBu){sub 8}, (non-peripheral substitution) and copper (II) 2,3,9,10,16,17,23,24-octabutoxyphthalocyanine, pCuPc(OBu){sub 8}, (peripheral substitution), were fabricated and characterized by optical spectroscopy and scanning probe microscopy. The LB films were transferred onto hydrophilic substrates by vertical dipping. Although they posses relatively short polar substituents both compounds form smooth, uniform, dense, and highly stable LB monolayers composed of linear arrays of cofacial oligomers. The long range discotic assemblies of LB and spun cast films of pCuPc(OBu){sub 8} and nCuPc(OBu){sub 8} posses physical and chemical properties favorable for molecular electronic device application.

  3. Injectable hydrogels derived from phosphorylated alginic acid calcium complexes

    Kim, Han-Sem; Song, Minsoo, E-mail: minsoosong00@gmail.com; Lee, Eun-Jung; Shin, Ueon Sang, E-mail: usshin12@dankook.ac.kr

    2015-06-01

    Phosphorylation of sodium alginate salt (NaAlg) was carried out using H{sub 3}PO{sub 4}/P{sub 2}O{sub 5}/Et{sub 3}PO{sub 4} followed by acid–base reaction with Ca(OAc){sub 2} to give phosphorylated alginic acid calcium complexes (CaPAlg), as a water dispersible alginic acid derivative. The modified alginate derivatives including phosphorylated alginic acid (PAlg) and CaPAlg were characterized by nuclear magnetic resonance spectroscopy for {sup 1}H, and {sup 31}P nuclei, high resolution inductively coupled plasma optical emission spectroscopy, Fourier transform infrared spectroscopy, and thermogravimetric analysis. CaPAlg hydrogels were prepared simply by mixing CaPAlg solution (2 w/v%) with NaAlg solution (2 w/v%) in various ratios (2:8, 4:6, 6:4, 8:2) of volume. No additional calcium salts such as CaSO{sub 4} or CaCl{sub 2} were added externally. The gelation was completed within about 3–40 min indicating a high potential of hydrogel delivery by injection in vivo. Their mechanical properties were tested to be ≤ 6.7 kPa for compressive strength at break and about 8.4 kPa/mm for elastic modulus. SEM analysis of the CaPAlg hydrogels showed highly porous morphology with interconnected pores of width in the range of 100–800 μm. Cell culture results showed that the injectable hydrogels exhibited comparable properties to the pure alginate hydrogel in terms of cytotoxicity and 3D encapsulation of cells for a short time period. The developed injectable hydrogels showed suitable physicochemical and mechanical properties for injection in vivo, and could therefore be beneficial for the field of soft tissue engineering. - Highlights: • Preparation of water-soluble alginic acid complexes with calcium phosphate • Self-assembly of the phosphorylated alginic acid calcium complexes with sodium alginate • Preparation of injectable hydrogels with diverse gelation times within about 3–40 min.

  4. Electrochemical behaviour of niobium and niobium passive films in nitric acid solutions

    Electrochemical behaviour of bare niobium and phosphoric acid anodized niobium electrodes is investigated in nitric acid solutions. Electrochemical impedance spectroscopy and polarisation techniques have been used to investigate the open-circuit growth of the passive film. The stability of the anodic oxide film has been studied as a function of the formation voltage, formation current density and concentration of the ambient electrolyte. The results show that the Nb-Nb2O5-1M HNO3 does not behave as a perfect dielectric. The flat band potential and donor concentration of the semiconducting anodic oxide film have been calculated from the Mott-Schottky plots. (author)

  5. Structure and function analysis of protein–nucleic acid complexes

    Kuznetsova, S. A.; Oretskaya, T. S.

    2016-05-01

    The review summarizes published data on the results and achievements in the field of structure and function analysis of protein–nucleic acid complexes by means of main physical and biochemical methods, including X-ray diffraction, nuclear magnetic resonance spectroscopy, electron and atomic force microscopy, small-angle X-ray and neutron scattering, footprinting and cross-linking. Special attention is given to combined approaches. The advantages and limitations of each method are considered, and the prospects of their application for wide-scale structural studies in vivo are discussed. The bibliography includes 145 references.

  6. Incorporation of europium III complex into nanoparticles and films obtained by the Sol-Gel methodology

    Faley Jean de Sousa

    2010-03-01

    Full Text Available The sol-gel process is very effective for the preparation of new materials with potential applications in optics, sensors, catalyst supports, coatings, and specialty inorganic polymers that can be used as hosts for the accommodation of organic molecules. The low temperature employed in the process is the main advantage of this methodology. In this work, the europium (III complex with 1,10-phenantroline was prepared, and this luminescent complex was incorporated into silica nanoparticles and films by the sol-gel process. The nanoparticles were obtained by the modified Stöber methodology. The films were obtained by the dip-coating technique, at different deposition rates and numbers of layers. The nanoparticles and films were characterized by photoluminescence, thermal analysis, and Raman and infrared spectroscopies. Characterization revealed that the europium (III complex was not affected upon incorporation into the nanoparticles and films, opening a new field for the application of these materials.

  7. A complex magnetic structure of ultrathin Fe films on Rh (001) surfaces

    Takada, Masaki [Max-Planck-Institut fuer Mikrostrukturphysik, Weinberg 2, 06120 Halle (Germany); Lana Gastelois, Pedro [Max-Planck-Institut fuer Mikrostrukturphysik, Weinberg 2, 06120 Halle (Germany); Servico de Nanotecnologia, Centro de Desenvolvimento da Tecnologia Nuclear, 31270-901 BeloHorizonte, MG (Brazil); Przybylski, Marek, E-mail: mprzybyl@mpi-halle.de [Max-Planck-Institut fuer Mikrostrukturphysik, Weinberg 2, 06120 Halle (Germany); Faculty of Physics and Applied Computer Science, AGH University of Science and Technology, 30-059 Krakow (Poland); Kirschner, Juergen [Max-Planck-Institut fuer Mikrostrukturphysik, Weinberg 2, 06120 Halle (Germany); Naturwissenschaftliche Fakultaet II, Martin-Luther-Universitaet Halle-Wittenberg, 06120 Halle (Germany)

    2013-03-15

    We conducted a structural and magnetic analysis of ultrathin Fe films on Rh (001) surfaces by using low electron energy diffraction (LEED), magneto-optical Kerr effects (MOKE) and spin-polarized scanning tunneling microscopy (SP-STM). The films in the investigated thickness range up to 6 monolayers (ML) are pseudomorphic to the Rh (001) substrate. While Fe films thinner than 3 ML grow layer-by-layer at room temperature (RT), Fe films thicker than 4 ML form islands. 1 ML Fe films do not show any hysteresis loops even at low temperature. Polar hysteresis loops for the 2 ML and 3 ML thick films appear at low temperatures. When 1 ML thick Fe films were studied by Cr- and Fe-coated W tips, a (2 Multiplication-Sign 3) and stripe structures were observed, respectively. The structures originate from a complex magnetic structure of 1 ML Fe. Based on the SP-STM results we propose a spin configuration model of a 1 ML Fe film. - Highlights: Black-Right-Pointing-Pointer We studied structural and magnetic properties of Fe films grown on an Rh (001). Black-Right-Pointing-Pointer MOKE measurements revealed that Fe films thicker than 2 ML are ferromagnetic at 5 K. Black-Right-Pointing-Pointer Fe films with thickness of 2 ML and 3 ML exhibit out-of-plane magnetization, those thicker than 4 ML show in-plane magnetization. Black-Right-Pointing-Pointer 1 ML Fe films have a complex magnetic configuration with zero net magnetization. Black-Right-Pointing-Pointer A spin configuration model of 1 ML Fe is proposed based on an SP-STM observation.

  8. Modification of hydrophobic polypeptide-based film by blending with hydrophilic poly(acrylic acid

    Guoquan Zhu

    2013-01-01

    Full Text Available In this study, a series of poly(γ-benzyl L-glutamate/poly(acrylic acid (PBLG/PAA polymer blend films were prepared by casting the polymer blend solution in dimethylsulfoxide (DMSO. The structure and morphology of the polymer blend film were investigated by Fourier Transform Infrared Spectroscopy (FT-IR and Scanning Electron Microscopy (SEM. Thermal, mechanical, and chemical properties of PBLG/PAA polymer blend films were studied by Differential Scanning Calorimetry (DSC, Thermogravimetric (TG Analysis, Tensile Tests, and measurements of Surface Contact Angles. The results revealed that the introduction of PAA could exert great effects on the structure and properties of the polypeptide films.

  9. Dynamics of the layer-by-layer assembly of a poly(acrylic acid)-lanthanide complex colloid and poly(diallyldimethyl ammonium).

    Xu, Jiali; Wang, Zhiliang; Wen, Lingang; Zhou, Xianju; Xu, Jian; Yang, Shuguang

    2016-01-21

    Poly(acrylic acid) (PAA) and lanthanide (Ln) ions, such as Ce(3+), Eu(3+), and Tb(3+), were prepared as dispersed complex colloidal particles through three different protocols with rigorous control of the pH value and mixing ratio. The negatively charged PAA-Ln complex particles were layer-by-layer (LbL) assembled with positively charged poly(diallyldimethyl ammonium) (PDDA) to prepare a thin film. The film thickness growth is much quicker than PDDA/PAA film. Due to the incorporation of Ln(3+) ions, the film exhibits fluorescence. During LbL assembly, PDDA-PAA association based on electrostatic force and PAA-Ce association based on coordination are in competition, which leads to the LbL assembly of PDDA and PAA-Ln complex colloidal particles being a complicated dynamic process. PMID:26549538

  10. A study on the performance of hyaluronic acid immobilized chitosan film

    Wang Yingjun; Guo Li; Ren Li; Yin Shiheng [Biomaterial Research Institute, College of Material Science and Engineering, South China University of Technology, Guangzhou, 510640 (China); Ge Jian; Gao Qianying [State Key Laboratory of Ophthalmology, Zhongshan Ophthalmic Center, Sun Yat-sen University, Guangzhou, 510060 (China); Luxbacher, Thomas; Luo Shijing, E-mail: imwangyj@scut.edu.c, E-mail: psliren@scut.edu.c [Anton Paar GmbH, Anton-Paar-Strasse 20, A-8054 Graz (Austria)

    2009-06-15

    In order to improve hydrophilicity and biocompatibility of chitosan, hyaluronic acid was immobilized onto the surface of chitosan film. The structure of films was characterized by Fourier transformed infrared spectroscopy with attenuated total reflectance (ATR-FTIR), x-ray photoelectron spectroscopy (XPS) and zeta potential. Results confirmed that hyaluronic acid was successfully immobilized on chitosan film. Transparency, water absorption percentage and contact angle of films were characterized. Results showed that there was no significant variation in transparency (p < 0.05) before and after immobilization, the maximum was up to 99% which was enough for corneal regeneration in clinical applications. After the immobilization, the time-dependent contact angle declined sharply (from 91.8 deg. to 67.7 deg. at 100 s). The hydrophilicity was significantly improved. The methylthiazol tetrazolium (MTT) (3-[4,5-dimethylthiazol-2-yl]-2,5-diphenyltetrazolium bromide) assay was used to assess cell viability and proliferation. Results showed that human cornea epithelial cells (HCEC) grew better on hyaluronic acid immobilized chitosan films than on chitosan films. The hyaluronic acid immobilized chitosan film could be a promising candidate material for corneal regeneration.

  11. A study on the performance of hyaluronic acid immobilized chitosan film

    In order to improve hydrophilicity and biocompatibility of chitosan, hyaluronic acid was immobilized onto the surface of chitosan film. The structure of films was characterized by Fourier transformed infrared spectroscopy with attenuated total reflectance (ATR-FTIR), x-ray photoelectron spectroscopy (XPS) and zeta potential. Results confirmed that hyaluronic acid was successfully immobilized on chitosan film. Transparency, water absorption percentage and contact angle of films were characterized. Results showed that there was no significant variation in transparency (p < 0.05) before and after immobilization, the maximum was up to 99% which was enough for corneal regeneration in clinical applications. After the immobilization, the time-dependent contact angle declined sharply (from 91.8 deg. to 67.7 deg. at 100 s). The hydrophilicity was significantly improved. The methylthiazol tetrazolium (MTT) (3-[4,5-dimethylthiazol-2-yl]-2,5-diphenyltetrazolium bromide) assay was used to assess cell viability and proliferation. Results showed that human cornea epithelial cells (HCEC) grew better on hyaluronic acid immobilized chitosan films than on chitosan films. The hyaluronic acid immobilized chitosan film could be a promising candidate material for corneal regeneration.

  12. Effect of acid and alkaline solubilization on the properties of surimi based film

    Thummanoon Prodpran

    2005-05-01

    Full Text Available The effect of acid and alkaline solubilizing processes on the properties of the protein based film from threadfin bream surimi was investigated. Surimi films prepared from both processes had the similar light transmission, tensile strength (TS and elongation at break (EAB (P<0.05. However, film with alkaline process had slightly lower water vapor permeability (WVP, compared to that prepared by acid solubilizing process. The protein concentration in the film-forming solution directly affected the properties of the film. Increase in protein concentration resulted in an increase in TS, EAB as well as WVP. The film prepared by acid solubilizing process had an increase in yellowish color as evidenced by the continuous increase in b* and E* values during the storage at r oom temperature. The acid and alkali solubilizing processes caused the degradation of muscle protein in surimi, especially with increasing exposure time. Therefore, solubilizing process had the influence on the properties of the protein film from threadfin bream surimi.

  13. Complexation behavior of Np(IV) and humic acid

    Complexation behavior between humic acid (HA), which is one of the natural organic matter in groundwater, and tetravalent neptunium (Np(IV)) was investigated by batch type complexation experiments and solvent extraction by TTA xylene, focused on the effect of concentration and molecular weight of HA. In addition, proton dissociation behavior from HA was evaluated by acid-base titration and its results was used for the calculation of stability constant of Np(IV) and HA complex. The results of titration of HA was analysed based on NICA-Donnan model and parameters used for evaluation of proton dissociation behavior were calculated. The charge density of HA in pH 8, which is necessary for calculation of stability constant, was evaluated as -4.35 meq/g. The complexation experiments were carried out under the conditions as follows; 1x10-5 mol/l of initial Np concentration, from 5 to 500 mg/l of HA concentration, pH 8, in the 0.1 mol/l NaClO4, and 0.05 mol/l Na2S2O4 as reductant to keep Np as tetravalent. As a result, in the presence of 5 mg/l of HA, total concentration of Np was increased at least one order of magnitude higher than in the case without HA. All added Np existed as soluble species in the presence of more than 50 mg/l of HA. Np in the solution was fractionated by solvent extraction using TTA-xylene as follows; 1) extractable Np into the organic phase, 2) non-extractable Np remained in the inorganic phase, and 3) precipitated Np. These were considered as 1) free Np(VI) or weakly binded Np(IV) and 3) strongly binded Np(IV), while 2) Np(IV)-fulvic acid complex could be suggested. Consequently, stability constant, log βα=26.31, was obtained. In addition, compared with Am(III) or Np(V), accessible site in the HA for Np(IV) seems to be quite limited. (author)

  14. Characterization of titanium thin films anodically grown in phosphoric acid; Caracterisation des films d'oxyde de titane obtenus anodiquement dans l'acide phosphorique

    Khadiri, M.E.; Benyaich [Faculte des Sciences Semlalia, Lab. d' Electrochimie et Chimie Analytique, Marakech (Morocco); Oueriagli, A.; Outzourhit, A.; Ameziane, E.L. [Faculte des Sciences Semlalia, Lab. de Physique du Solide et des Couches Minces, Marakech (Morocco)

    2004-08-01

    Ti-Cu(2%) alloy was anodized in a 5 M phosphoric acid solution under various voltages ranging from 10 to 35 V. The composition, the structural and optical properties of the as-grown oxide films were studied. It was found that the color of the anodized substrates varied from yellow to blue depending on the anodizing voltage. The films formed on the alloy are amorphous and the oxidation state of Ti on their surface is mainly +4. On the other hand it was found that the thickness of the films increases linearly with anodization voltage at rate of 1.94 nm/V, while the refractive index at the wavelength corresponding to the reflectance minimum was practically constant. These films were also found to have excellent protective properties for the examined alloy. (authors)

  15. Crosslinked collagen-gelatin-hyaluronic acid biomimetic film for cornea tissue engineering applications

    Liu, Yang; Ren, Li, E-mail: psliren@scut.edu.cn; Wang, Yingjun, E-mail: imwangyj@163.com

    2013-01-01

    Cornea disease may lead to blindness and keratoplasty is considered as an effective treatment method. However, there is a severe shortage of donor corneas worldwide. This paper presents the crosslinked collagen (Col)-gelatin (Gel)-hyaluronic acid (HA) films developed by making use of 1-ethyl-3-(3-dimethyl aminopropyl) carbodiimide (EDC) and N-hydroxysuccinimide (NHS) as the crosslinker. The test results on the physical and biological properties indicate that the CGH631 film (the mass ratio of Col:Gel:HA = 6:3:1) has appropriate optical performance, hydrophilicity and mechanical properties. The diffusion properties of the CGH631 film to NaCl and tryptophan are also satisfactory and the measured data are 2.43 Multiplication-Sign 10{sup -6} cm{sup 2}/s and 7.97 Multiplication-Sign 10{sup -7} cm{sup 2}/s, respectively. In addition, cell viability studies demonstrate that the CGH631 film has good biocompatibility, on which human corneal epithelial cells attached and proliferated well. This biocompatible film may have potential use in cornea tissue engineering. - Highlights: Black-Right-Pointing-Pointer Crosslinked collagen-gelatin-hyaluronic acid films were fabricated in this study. Black-Right-Pointing-Pointer The film had appropriate physical properties. Black-Right-Pointing-Pointer Diffusion coefficient of the film was comparable with the human cornea. Black-Right-Pointing-Pointer HCEC viability studies confirmed the biocompatibility of the film.

  16. Crosslinked collagen–gelatin–hyaluronic acid biomimetic film for cornea tissue engineering applications

    Cornea disease may lead to blindness and keratoplasty is considered as an effective treatment method. However, there is a severe shortage of donor corneas worldwide. This paper presents the crosslinked collagen (Col)–gelatin (Gel)–hyaluronic acid (HA) films developed by making use of 1-ethyl-3-(3-dimethyl aminopropyl) carbodiimide (EDC) and N-hydroxysuccinimide (NHS) as the crosslinker. The test results on the physical and biological properties indicate that the CGH631 film (the mass ratio of Col:Gel:HA = 6:3:1) has appropriate optical performance, hydrophilicity and mechanical properties. The diffusion properties of the CGH631 film to NaCl and tryptophan are also satisfactory and the measured data are 2.43 × 10−6 cm2/s and 7.97 × 10−7 cm2/s, respectively. In addition, cell viability studies demonstrate that the CGH631 film has good biocompatibility, on which human corneal epithelial cells attached and proliferated well. This biocompatible film may have potential use in cornea tissue engineering. - Highlights: ► Crosslinked collagen–gelatin–hyaluronic acid films were fabricated in this study. ► The film had appropriate physical properties. ► Diffusion coefficient of the film was comparable with the human cornea. ► HCEC viability studies confirmed the biocompatibility of the film.

  17. Thermally driven stability of octadecylphosphonic acid thin films grown on SS316L.

    Lim, Min Soo; Smiley, Katelyn J; Gawalt, Ellen S

    2010-01-01

    Stainless steel 316L is widely used as a biomedical implant material; however, there is concern about the corrosion of metallic implants in the physiological environment. The corrosion process can cause mechanical failure due to resulting cracks and cavities in the implant. Alkyl phosphonic acid forms a thin film by self-assembly on the stainless steel surface and this report conclusively shows that thermal treatment of the octadecylphosphonic acid (ODPA) film greatly enhances the stability of the ODPA molecules on the substrate surface. AFM images taken from the modified substrates revealed that thermally treated films remain intact after methanol, THF, and water flushes, whereas untreated films suffer substantial loss. Water contact angles also show that the hydrophobicity of thermally treated films does not diminish after being incubated in a dynamic flow of water for a 3-hour period, whereas the untreated film becomes increasingly hydrophilic due to loss of ODPA. IR spectra taken of both treated and untreated films after water and THF flushes show that the remaining film retains its initial crystallinity. A model is suggested to explain the stability of ODPA film enhanced by thermal treatment. An ODPA molecule is physisorbed to the surface weakly by hydrogen bonding. Heating drives away water molecules leading to the formation of strong monodentate or mixed mono/bi-dentate bonds of ODPA molecule to the surface. PMID:20648546

  18. Aggregation properties of tetrachloroperylene-tetracarboxylic acid in binary Langmuir and Langmuir–Blodgett films

    The Langmuir and Langmuir–Blodgett films formed of tetra-n-butyl-1,6,7,12-tetrachloroperylene-3,4,9,10-tetracarboxylate and its binary mixtures with 4-octyl-4′-cyanobiphenyl and arachidic acid have been studied. The Langmuir films were characterized by surface pressure versus mean molecular area isotherms and the films morphology observations were made by means of a Brewster angle microscope. The miscibility of the compounds was determined. Subsequently, the Langmuir films were transferred onto hydrophilic quartz substrates forming the monolayer Langmuir–Blodgett films. The electronic absorption and fluorescence spectra reveal aggregation of the chromophores in ground state driven by π–π molecular orbitals interactions. Perylene-like dye aggregation depends upon the dye concentration in the dye/liquid crystal mixed films and is concentration-independent in dye/arachidic acid one. -- Highlights: • A new perylene derivative with four chlorine atoms in the core was synthetized. • Langmuir films of pure dye and its binary mixtures were studied thermodynamically. • The miscibility of the components in the films changes the π–π stacking of the dye. • We describe the dye aggregation in the pure and mixed films deposited onto quartz

  19. Aggregation properties of tetrachloroperylene-tetracarboxylic acid in binary Langmuir and Langmuir–Blodgett films

    Modlińska, Anna; Piosik, Emilia [Faculty of Technical Physics, Poznan University of Technology, Poznan (Poland); Paluszkiewicz, Joanna [Institute of Polymers and Dyes Technology, Lodz University of Technology, Lodz (Poland); Martyński, Tomasz, E-mail: tomasz.martynski@put.poznan.pl [Faculty of Technical Physics, Poznan University of Technology, Poznan (Poland)

    2014-04-15

    The Langmuir and Langmuir–Blodgett films formed of tetra-n-butyl-1,6,7,12-tetrachloroperylene-3,4,9,10-tetracarboxylate and its binary mixtures with 4-octyl-4′-cyanobiphenyl and arachidic acid have been studied. The Langmuir films were characterized by surface pressure versus mean molecular area isotherms and the films morphology observations were made by means of a Brewster angle microscope. The miscibility of the compounds was determined. Subsequently, the Langmuir films were transferred onto hydrophilic quartz substrates forming the monolayer Langmuir–Blodgett films. The electronic absorption and fluorescence spectra reveal aggregation of the chromophores in ground state driven by π–π molecular orbitals interactions. Perylene-like dye aggregation depends upon the dye concentration in the dye/liquid crystal mixed films and is concentration-independent in dye/arachidic acid one. -- Highlights: • A new perylene derivative with four chlorine atoms in the core was synthetized. • Langmuir films of pure dye and its binary mixtures were studied thermodynamically. • The miscibility of the components in the films changes the π–π stacking of the dye. • We describe the dye aggregation in the pure and mixed films deposited onto quartz.

  20. Influencing of resorption and side-effects of salicylic acid by complexing with β-cyclodextrin

    After oral administration of 14C-labelled salicylic acid and its β-cyclodextrin complex to rats, the radioactivity level of the blood reached its maximum during the first 2 h. The blood level obtained with the complex is somewhat but not significantly lower than with free acid. Since the resorption of cyclodextrin is a considerably slower process, it is very likely that the resorption of salicylic acid takes place in the form of free acid after dissociation of the complex. The urinary excretion cumulative curves showed that the free salicylic acid was completely excreted, while about 10% of the salicylic acid administered in the form of complex is lost. The cyclodextrin complex formation increased the pK values of all hydroxybenzoic acids. Direct observations revealed that complex formation decreased the stomach-irritating effect of salicylic acid. The ratio of radioactivity was nearly the same in the organs of animals treated by both free salicylic and cyclodextrin complex. (author)

  1. Investigation of molecular interactions in the complex formation of tartaric acid derivatives with di(2-ethylhexyl) phosphoric acid

    2008-01-01

    The molecular interactions in the complex formation of two tartaric acid derivatives with di(2-ethylhexyl) phosphoric acid are investigated. The complex formation with a 1:1 stoichiometry between tartaric acid derivatives and D2EHPA can be obtained through UV-Vis titration, NMR chemical shifts and molecular dynamic simulations. Furthermore, the differences of the two complexes on the binding constants and strength of hydrogen bonds can also be determined. Such research will ideally provide insight into ways of regulating the complex forming properties of tartaric acid derivatives for composing or syn- thesizing new chiral resolving agents.

  2. Investigation of molecular interactions in the complex formation of tartaric acid derivatives with di(2-ethylhexyl) phosphoric acid

    TAN Bin; ZHAI Zheng; LUO GuangSheng; WANG JiaDing

    2008-01-01

    The molecular interactions in the complex formation of two tartaric acid derivatives with di(2-ethylhexyl) phosphoric acid are investigated. The complex formation with a 1:1 stoichiometry between tartaric acid derivatives and D2EHPA can be obtained through UV-Vis titration, NMR chemical shifts and molecular dynamic simulations. Furthermore, the differences of the two complexes on the binding constants and strength of hydrogen bonds can also be determined. Such research will ideally provide insight into ways of regulating the complex forming properties of tartaric acid derivatives for composing or syn-thesizing new chiral resolving agents.

  3. Effects of preirradiation graft polymerization of acrylic acid onto polyethylene film

    With the aid of preirradiation method of grafting onto low-density polyethylene film, a systematic investigation was made of grafting of aqueous acrylic acid under conditions such as monomer concentrations, irradiation dose, dose rate, reaction time, the effect of concentrations of Mohr's salt and sulphuric acid on the graft reaction. (author)

  4. α-Lactalbumin:Oleic Acid Complex Spontaneously Delivers Oleic Acid to Artificial and Erythrocyte Membranes.

    Wen, Hanzhen; Strømland, Øyvind; Halskau, Øyvind

    2015-09-25

    Human α-lactalbumin made lethal to tumor cells (HAMLET) is a tumoricidal complex consisting of human α-lactalbumin and multiple oleic acids (OAs). OA has been shown to play a key role in the activity of HAMLET and its related complexes, generally known as protein-fatty acid (PFA) complexes. In contrast to what is known about the fate of the protein component of such complexes, information about what happens to OA during their action is still lacking. We monitored the membrane, OA and protein components of bovine α-lactalbumin complexed with OA (BLAOA; a HAMLET-like substance) and how they associate with each other. Using ultracentrifugation, we found that the OA and lipid components follow each other closely. We then firmly identify a transfer of OA from BLAOA to both artificial and erythrocyte membranes, indicating that natural cells respond similarly to BLAOA treatment as artificial membranes. Uncomplexed OA is unable to similarly affect membranes at the conditions tested, even at elevated concentrations. Thus, BLAOA can spontaneously transfer OA to a lipid membrane. After the interaction with the membrane, the protein is likely to have lost most or all of its OA. We suggest a mechanism for passive import of mainly uncomplexed protein into cells, using existing models for OA's effect on membranes. Our results are consistent with a membrane destabilization mediated predominantly by OA insertion being a significant contribution to PFA cytotoxicity. PMID:26297199

  5. Properties of CdS films prepared from thiourea complexes of cadmium salts

    One studied the effect of chemical nature of cadmium salt thiourea complex on the optical, electrical and structural properties of cadmium sulfide films. It was shown that the effect of chemical nature of thiourea complexes was associated with changing of the material chemical history. One may conclude that the composition and point symmetry of coordination compounds dictate, defect character and space symmetry of a new solid phase. Simulating the internal coordination sphere of the complex one may govern the properties of cadmium sulfide semiconducting films

  6. Dual Fatty Acid Elongase Complex Interactions in Arabidopsis.

    Morineau, Céline; Gissot, Lionel; Bellec, Yannick; Hematy, Kian; Tellier, Frédérique; Renne, Charlotte; Haslam, Richard; Beaudoin, Frédéric; Napier, Johnathan; Faure, Jean-Denis

    2016-01-01

    Very long chain fatty acids (VLCFAs) are involved in plant development and particularly in several cellular processes such as membrane trafficking, cell division and cell differentiation. However, the precise role of VLCFAs in these different cellular processes is still poorly understood in plants. In order to identify new factors associated with the biosynthesis or function of VLCFAs, a yeast multicopy suppressor screen was carried out in a yeast mutant strain defective for fatty acid elongation. Loss of function of the elongase 3 hydroxyacyl-CoA dehydratase PHS1 in yeast and PASTICCINO2 in plants prevents growth and induces cytokinesis defects. PROTEIN TYROSIN PHOSPHATASE-LIKE (PTPLA) previously characterized as an inactive dehydratase was able to restore yeast phs1 growth and VLCFAs elongation but not the plant pas2-1 defects. PTPLA interacted with elongase subunits in the Endoplasmic Reticulum (ER) and its absence induced the accumulation of 3-hydroxyacyl-CoA as expected from a dehydratase involved in fatty acid (FA) elongation. However, loss of PTPLA function increased VLCFA levels, an effect that was dependent on the presence of PAS2 indicating that PTPLA activity repressed FA elongation. The two dehydratases have specific expression profiles in the root with PAS2, mostly restricted to the endodermis, while PTPLA was confined in the vascular tissue and pericycle cells. Comparative ectopic expression of PTPLA and PAS2 in their respective domains confirmed the existence of two independent elongase complexes based on PAS2 or PTPLA dehydratase that are functionally interacting. PMID:27583779

  7. Evaluation of biocompatibility and toxicity of biodegradable poly (DL-lactic acid) films.

    Li, Rui-Yun; Liu, Zhi-Gang; Liu, Huan-Qiu; Chen, Lei; Liu, Jian-Feng; Pan, Yue-Hai

    2015-01-01

    Regeneration and functional recovery of nerves after peripheral nerve injury is the key to peripheral nerve repair. One of the putative therapeutic strategies is to use anti-adhesion polymer films, made of polymeric biomaterials. Recently, a novel biodegradable poly (DL-lactic acid) (PDLLA) film has been prepared using a method of phase transformation with biodegradable polylactic acid polymer as the substrate. This novel, anti-adhesion film has a porous structure, which provides better mechanical properties, better flexibility, more complete diffusion through the polymer of tissue biologic factors like growth factors, and more controllable degradation compared to traditional non-porous films. Little is known, however, about the in vitro and in vivo biocompatibility and cytotoxicity of this type of PDLLA film. Therefore, our aim was to evaluate the biocompatibility and cytotoxicity of this novel PDLLA film using various experimental methods, including a skin irritation test, MTT analysis, and the mouse bone marrow cell micronucleus test, as well as hematology or clinical chemistry measurements in rats after receiving sciatic nerve transection and anastomosis with wrapping of the anastomosis with DLLA films. We demonstrated that exposure to PDLLA film extracts did not generate apparent erythema or edema in rabbit skin and had no effect on the proliferation of Vero cells. Additionally, treatment with PDLLA film extracts did not alter the incidence of micronucleated polychromatic erythrocytes as compared with saline Treated group. Furthermore, implantation of PDLLA film did not alter liver or renal function as measured by serum levels of ALT, AST, TP, A/G, Cr, and BUN, and pathologic examinations showed that implantation of PDLLA film did not cause pathologic changes to the rat liver, kidney, pancreas, or spleen. Taken together, these results suggest that PDLLA films have excellent biocompatibility and no obvious toxicity in vivo, and may be used to prevent nerve

  8. Fabrication of superhydrophobic surface of hierarchical ZnO thin films by using stearic acid

    Wang, Yanfen; Li, Benxia; Xu, Chuyang

    2012-01-01

    Flower-like hierarchical ZnO microspheres were successfully synthesized by a simple, template-free, and low-temperature aqueous solution route. The morphology and microstructure of the ZnO microspheres were examined by X-ray diffraction, scanning electron microscopy and transmission electron microscopy. The bionic films with hydrophobicity were fabricated by the hierarchical ZnO microspheres modified by stearic acid. It was found that the hydrophobicity of the thin films was very sensitive to the added amount of stearic acid. The thin films modified with 8% stearic acid took on strong superhydrophobicity with a water contact angle (CA) almost to be 178° and weak adhersion. The remarkable superhydrophobicity could be attributed to the synergistic effect of micro/nano hierarchical structure of ZnO and low surface energy of stearic acid.

  9. Cataluminescence sensor for gaseous acetic acid using a thin film of In2O3

    We report on a cataluminescence sensor for the determination of gaseous acetic acid. It is based on a 60-nm thick sol-gel film of In2O3 on a ceramic support. SEM, XPS and surface profiling were applied for its characterization. It is found that aluminum ions of the ceramic substrate penetrate into the film and produce a synergetic catalytic effect. The sensor displays high sensitivity and specificity for acetic acid, a low detection limit, a wide linear range and a fast response. No (or only very low) interference was observed by formic acid, ammonia, acrolein, benzene, formaldehyde, ethanol, and acetaldehyde. The sensor was successfully applied to the determination of acetic acid in spiked air samples. We also discuss a conceivable mechanism (based on the reaction products) for the cataluminescence resulting from the oxidation reaction on the surface of the sensor film. (author)

  10. Chitosan-gum arabic polyelectrolyte complex films: physicochemical, mechanical and mucoadhesive properties.

    Sakloetsakun, Duangkamon; Preechagoon, Detpon; Bernkop-Schnürch, Andreas; Pongjanyakul, Thaned

    2016-08-01

    By blending chitosan (CS) and gum arabic (GA), a powerful biomaterial complex might be obtained due to the unique properties of CS and the low viscosity and good emulsifying properties of GA. The objectives of this study were to prepare and examine the properties of dispersions and films of CS and GA as a function of the mixing weight ratio, pH value and molecular weight of CS. The dispersions were characterized by turbidity, zeta potential and cytotoxicity and then the dispersions were cast into films. Physicochemical properties of the film were performed. CS-GA dispersions exhibited higher turbidity and a lower zeta potential with an increase in the GA ratio. Continuous films of the CS-GA could be formed at all ratios. CS and GA could molecularly interact via electrostatic forces and intermolecular hydrogen bonding. The CS-GA (1:0.5) films exhibited relatively low water uptake, erosion, water vapor permeability and puncture strength compared to the CS films. Furthermore, the CS-GA films demonstrated good mucoadhesive properties, allowing for adhesion to the mucosal membrane. Based on these results, it could be advantageous to use CS-GA films as film formers for the formulation of coatings and drug delivery systems. PMID:25886079

  11. Biodegradation of poly(hydroxy butanoic acid) copolymer mulch films in soil

    Kukade, Pranav

    Agricultural mulch films that are used to cover soil of crop rows contribute to earlier maturation of crops and higher yield. Incineration and landfill disposals are the most common means of disposal of the incumbent polyethylene (PE) mulch films; however, these are not environment friendly options. Biodegradable mulch films that can be rototilled into the soil after crop harvest are a promising alternative to offset problems such as landfill disposal, film retrieval and disposal costs. In this study, an in-house laboratory scale test method was developed in which the rate of disintegration, as a result of biodegradation of films based on polyhydroxybutanoic acid (PHB) copolymers was investigated in a soil environment using the residual weight loss method. The influence of soil composition, moisture levels in the soil, and industry-standard anti-microbial additive in the film composition on the rate of disintegration of PHB copolymer films was investigated. The soil composition has significant effect on the disintegration kinetics of PHB copolymer films, since the increasing compost levels in the soil lowered the rate of disintegration of the film. Also, with the increase in moisture level up to a threshold limit, the microbial activity and, hence, the rate of disintegration increased. Lastly, the developed lab-scale test protocol was found to be sensitive to even small concentrations of industry-standard antimicrobial additive in the film composition.

  12. Synthesis of cadmium sulphide in pure and mixed Langmuir-Blodgett films of -octadecylsuccinic acid

    G Hemakanthi; Balachandran Unni Nair; Aruna Dhathathreyan

    2000-04-01

    Cadmium sulphide (CdS) nanoparticles were grown by the reaction of sodium sulphide (Na2S) with Langmuir-Blodgett (LB) films of cadmium salts of -octadecylsuccinic acid (ODSU) and with LB films of ODSU in mixtures of octadecylamine and octadecyl alcohol. The results indicate that heterogeneous nucleation and aggregation in the pure ODSU LB films due to processes like Ostwald ripening are destabilized by the presence of the long-chain amine and alcohol in mixed systems. CdS nanoparticles in the LB films were monitored by UV-visible absorption spectra, which allow an estimation of the size of the particles. The morphology, size and nature of the nanocrystallites formed depend on whether the sulphidation was done on the pure film or in the mixed films. It is seen that particles of size around 1.6 nm were formed in ODSU/octadecylalcohol and ODSU/octadecylamine mixed LB films while in pure ODSU films the size was about 2.7 nm. These films showed typical needle-shaped structures, as observed by the optical microscopic technique. Mean size and morphology were confirmed by transmission and scanning electron microscopy, while selective area electron diffraction patterns showed six-fold symmetry and indicated that the CdS crystals grow epitaxially with respect to the monolayer. Further, the crystallisation enhanced in the mixed LB films showed a characteristic zinc oxide (Wurtzite) structure compared with the pure ODSU matrix.

  13. Comparative study of electroless nickel film on different organic acids modified cuprammonium fabric (CF)

    Zhao, Hang; Lu, Yinxiang

    2016-01-01

    Nickel films were grown on citric acid (CA), malic acid (MA) and oxalic acid (OA) modified cuprammonium fabric (CF) substrates via electroless nickel deposition. The nickel films were examined using scanning electron microscopy (SEM) and X-ray diffraction (XRD). Their individual deposition rate and electromagnetic interference (EMI) shielding effectiveness (SE) were also investigated to compare the properties of electroless nickel films. SEM images illustrated that the nickel film on MA modified CF substrate was smooth and uniform, and the density of nickel nuclei was much higher. Compared with that of CA modified CF, the coverage of nickel nuclei on OA and MA modified CF substrate was very limited and the nickel particles size was too big. XRD analysis showed that the nickel films deposited on the different modified CF substrates had a structure with Ni (1 1 1) preferred orientation. All the nickel coatings via different acid modification were firmly adhered to the CF substrates, as demonstrated by an ultrasonic washing test. The result of tensile test indicated that the electroless nickel plating on CF has ability to strengthen the CF substrate while causes limited effect on tensile elongation. Moreover, the nickel film deposited on MA modified CF substrate showed more predominant in EMI SE than that deposited on CA or OA modified CF.

  14. Ultrafine nanoporous palladium-aluminum film fabricated by citric acid-assisted hot-water-treatment of aluminum-palladium alloy film

    Hot-water-treatment has been adapted to fabricate ultrafine nanoporous palladium-aluminum film from aluminum-palladium alloy film. Using citric acid as a chelating agent, a precipitation of boehmite (aluminum oxide hydroxide, AlOOH) on the nanoporous palladium-aluminum film was suppressed. According to cross-sectional scanning transmission electron microscopy observations, the ligament/pore sizes of the prepared nanoporous film were considerably small (on the order of 10 nm). Since this fabrication method only requires aluminum alloy film and hot-water with chelating agent, the ultrafine nanoporous film can be prepared simply and environmentally friendly

  15. Ultrafine nanoporous palladium-aluminum film fabricated by citric acid-assisted hot-water-treatment of aluminum-palladium alloy film

    Takashi Harumoto; Yohei Tamura; Takashi Ishiguro

    2015-01-01

    Hot-water-treatment has been adapted to fabricate ultrafine nanoporous palladium-aluminum film from aluminum-palladium alloy film. Using citric acid as a chelating agent, a precipitation of boehmite (aluminum oxide hydroxide, AlOOH) on the nanoporous palladium-aluminum film was suppressed. According to cross-sectional scanning transmission electron microscopy observations, the ligament/pore sizes of the prepared nanoporous film were considerably small (on the order of 10 nm). Since this fabri...

  16. Syntheses,characteristics,and fluorescence properties of complexes of europium with benzoic acid and its derivatives

    ZHOU Zhongcheng; SHU Wangen; RUAN Jianming; HUANG Boyun; LIU Younian

    2004-01-01

    The binary complexes of europium with benzoic acid and its derivatives (phthalic acid, m-phthalic acid,o-aminobenzoic acid, salicylic acid, and sulfosalicylic acid) were synthesized and their compositions were identified by elemental analyses. UV and IR of the complexes have been investigated. The UV spectra indicated that the complexes' ultraviolet absorption were mainly the ligands' absorption. The IR spectra showed that the IR spectra of complexes are different from those of free ligands. The fluorescence properties of them were investigated by using luminescence spectroscopy, the results showed that only three complexes appear as better luminescence, they were Eu-benzoic acid,Eu-m-phthalic acid and Eu-phthalic acid, while the others exhibited the ligands' wideband emission.

  17. The structure study of boron carbonitride films obtained by use of trimethylamine borane complex

    Kosinova, M L; Fainer, N I; Maximovski, E A; Kuznetsov, F A

    2001-01-01

    Diffraction of synchrotron radiation (SR) was used to investigate crystalline structure and phase composition of thin films (1500-5000 A) of boron carbonitride. These films were synthesized by plasma-enhanced chemical vapor deposition using nontraditional volatile single source precursor trimethylamine borane complex (CH sub 3) sub 3 N centre dot BH sub 3 and its mixture with ammonia. The effect of the gas ratio and substrate temperature on chemical and phase composition as well as the structure of the films were investigated. The XRD peculiarities of texture films and ways of increasing sensibility of measurements were considered. A possibility of the information density rise of the thin film XRD was shown due to application of different methods for recording diffraction patterns.

  18. The application of layered double hydroxide clay (LDH)-poly(lactide-co-glycolic acid) (PLGA) film composites for the controlled release of antibiotics

    Chakraborti, Michelle; Jackson, John K.; Plackett, David;

    2012-01-01

    complexes in poly(lactic-co-glycolic acid) films resulted in a reduced burst phase of release and a slow continuous release for many weeks with effective antimicrobial amounts of VAN and SF released at later time points. Layered double hydroxide clays may be useful for controlled release applications at...... quantitation of the unbound fraction by UV/Vis absorbance or HPLC analysis. Drug release from layered double hydroxide clay/drug complexes dispersed in polymeric films was measured by incubation in phosphate-buffered saline (pH 7.4) at 37 °C using absorbance or HPLC analysis. Antimicrobial activity of drug...... sites requiring long-term antibiotic exposure as they maintain the drug in a non-degraded state and release effective amounts of drug over long time periods. LDH clay/drug complexes are amenable to homogenous dispersion in polymeric films where implant coating may be optimal or required....

  19. The response of quartz crystals coated with thin fatty acid film to organic gases

    We tried to apply a quartz crystal as a sensor by using the resonant frequency and the resistance properties of quartz crystals. Four kinds of fatty acids that have the same head groups were coated on the surfaces of the quartz crystals, and the shift of the resonant frequency and the resistance were observed based on the lengths of the tail groups. Myristic acid (C14), palmitic acid (C16), stearic acid (C18), and arachidic acid (C20) were deposited on the surfaces of quartz crystals by using the Langmuir-Blodgett (LB) method. As a result, the resonant frequency change was more sensitive to high molecular-weight fatty acids than to low molecular-weight ones. We also observed the effect of temperature on stearic acid LB films, and the response properties of quartz crystals coated with stearic-acid LB films to organic gases were investigated. As a result, the sensitivity of quartz crystals to organic gases was higher for higher molecular-weight gas, and we found that quartz crystals coated with stearic-acid LB film were more sensitive to organic gas than bare quartz crystals at room temperature

  20. Graphene oxide supported mononuclear aquaruthenium complex ultrathin films with enhanced photoelectric conversion and electrocatalytic water oxidation

    Graphical abstract: A electrostatic film composed of GO nanosheets and a Ru(II) complex on ITO exhibited quasi-reversible redox behaviors with rapid heterogeneous electron transfer dynamics, and remarkably improved electrocatalytic water oxidation and photoelectric conversion properties as compared with the electrodes with polyanionic being the support for the Ru(II) complex. Display Omitted -- Abstract: A new Ru(II) complex of [Ru(tpy)(Htip)(H2O)]2+ {tpy = 2,2′,2″-terpyridine, Htip = 2-(thiophen-2-yl)-1H-imidazo[4,5-f][1,10]-phenanthroline} is synthesized and characterized. A layer-by-layer deposition of equal amounts of graphene oxide (GO) and the Ru(II) complex on hydrophilic substrates through electrostatic attraction of these two components was evidenced by X-ray photoelectron and UV–visible absorption spectroscopy. Permeability of the film to the redox probe [Fe(CN)6]3−/4− was studied by cyclic voltammetry and electrochemical impedance spectroscopy. The films showed stable electrochemical and photoelectrochemical properties with photocurrent densities of 6.6 μA/cm2 being found for a monolayer film and 9.7 μA/cm2 for a 4-layer film, which is much improved as compared to GO monolayer alone and the film by using a polyanion instead of the GO. The enhanced electrocatalytic water oxidation properties of this hybrid film have also been demonstrated. Preliminary results of electrocatalytic water oxidation by this hybrid film is also reported

  1. Complex Nonlinear Deformation of Nanometer Intergranular Glassy Films in βSi3N4

    Chen, Jun; Ouyang, Lizhi; Rulis, Paul; Misra, Anil; Ching, W. Y.

    2005-01-01

    The mechanical properties of a model of Y-doped intergranular glassy film in silicon nitride ceramics are studied by large-scale ab initio modeling. By linking directly to its electronic structure, it is shown that this microstructure has a complex nonlinear deformation under stress and Y doping significantly enhances the mechanical properties. The calculation of the electrostatic potential across the film supports the space charge model in ceramic microstructures.

  2. Complex nonlinear deformation of nanometer intergranular glassy films in beta-Si3N4.

    Chen, Jun; Ouyang, Lizhi; Rulis, Paul; Misra, Anil; Ching, W Y

    2005-12-16

    The mechanical properties of a model of Y-doped intergranular glassy film in silicon nitride ceramics are studied by large-scale ab initio modeling. By linking directly to its electronic structure, it is shown that this microstructure has a complex nonlinear deformation under stress and Y doping significantly enhances the mechanical properties. The calculation of the electrostatic potential across the film supports the space charge model in ceramic microstructures. PMID:16384476

  3. Glass Difractive Optical Elements (DOEs with complex modulation DLC thin film coated

    Marina Sparvoli

    2008-09-01

    Full Text Available We developed a complex (amplitude and phase modulation Diffractive Optical Element (DOE with four phase levels, which is based in a glass substrate coated with DLC (Diamond Like Carbon thin film as the amplitude modulator. The DLC film was deposited by magnetron reactive sputtering with a graphite target and methane gas in an optical glass surface. The glass and DLC film roughness were measured using non destructive methods, such as a high step meter, Atomic Force Microscopy and Diffuse Reflectance. Other properties, such as refractive index of both materials were measured. The DOEs were tested using 632.8 nm HeNe laser.

  4. Relaxation Kinetic Study of Eudragit® NM30D Film Based on Complex Modulus Formalism

    Penumetcha, Sai Sumana; Byrn, Stephen R.; Morris, Kenneth R.

    2015-01-01

    This study is aimed at resolving and characterizing the primary (α) and secondary relaxations (β) in Eudragit® NM30D film based on apparent activation energies derived from complex modulus formalism using dielectric analysis (DEA). The glass transition (Tg) of the film was determined using differential scanning calorimetry (DSC). The α relaxation corresponding to Tg and the β relaxations occurring below Tg were probed using DEA. The occurrence of α and β relaxations in Eudragit® NM30D film wa...

  5. CVD of pure copper films from novel iso-ureate complexes.

    Willcocks, Alexander M; Pugh, Thomas; Hamilton, Jeff A; Johnson, Andrew L; Richards, Stephen P; Kingsley, Andrew J

    2013-04-21

    We report the synthesis and characterisation of a new family of copper(i) metal precursors based around alkoxy-N,N'-di-alkyl-ureate ligands, and their subsequent application in the production of pure copper thin films. The molecular structure of the complexes bis-copper(i)(methoxy-N,N'-di-isopropylureate) (1) and bis-copper(i)(methoxy-N,N'-di-cyclohexylureate)(5) are described, as determined by single crystal X-ray diffraction analysis. Thermogravimetric analysis of the complexes highlighted complex 1 as a possible copper CVD precursor. Low pressure chemical vapour deposition (LP-CVD) was employed using precursor 1, to synthesise thin films of metallic copper on ruthenium substrates under an atmosphere of hydrogen (H2). Analysis of the thin films deposited at substrate temperatures of 225 °C, 250 °C and 300 °C, respectively, by SEM and AFM reveal the films to be continuous and pin hole free, and show the presence of temperature dependent growth features on the surface of the thin films. Energy dispersive X-ray spectroscopy (EDX), powder X-ray diffraction (PXRD) and X-ray photoelectron spectroscopy (XPS) all show the films to be high purity metallic copper. PMID:23425976

  6. Effects of humic acid-metal complexes on hepatic carnitine palmitoyltransferase, carnitine acetyltransferase and catalase activities

    Fungjou Lu; Youngshin Chen (National Taiwan Univ., Taipei (Taiwan, Province of China). Dept. of Biochemistry); Tienshang Huang (National Taiwan Univ., Taipei (Taiwan, Province of China). Dept. of Medicine)

    1994-03-01

    A significant increase in activities of hepatic carnitine palmitoyltransferase and carnitine acetyltransferase was observed in male Balb/c mice intraperitoneally injected for 40 d with 0.125 mg/0.1 ml/d humic acid-metal complexes. Among these complexes, the humic acid-As complex was relatively effective, whereas humic acid-25 metal complex was more effective, and humic acid-26 metal complex was most effective. However, humic acid or metal mixtures, or metal such as As alone, was not effective. Humic acid-metal complexes also significantly decreased hepatic catalase activity. A marked decrease of 60-kDa polypeptide in liver cytoplasm was also observed on SDS-polyacrylamide gel electrophoresis after the mice had been injected with the complexes. Morphological analysis of a histopathological biopsy of such treated mice revealed several changes in hepatocytes, including focal necrosis and cell infiltration, mild fatty changes, reactive nuclei, and hypertrophy. Humic acid-metal complexes affect activities of metabolic enzymes of fatty acids, and this results in accumulation of hydrogen peroxide and increase of the lipid peroxidation. The products of lipid peroxidation may be responsible for liver damage and possible carcinogenesis. Previous studies in this laboratory had shown that humic acid-metal complex altered the coagulation system and that humic acid, per se, caused vasculopathy. Therefore, humic acid-metal complexes may be main causal factors of not only so-called blackfoot disease, but also the liver cancer prevailing on the southwestern coast of Taiwan.

  7. Fabrication of TiO2 nanoparticles/surfactant polymer complex film on glassy carbon electrode and its application to sensing trace dopamine

    A novel method for the fabrication of a TiO2/Nafion nano-film on glassy carbon electrode (NTGCE) is described. In the presence of dispersant, TiO2 nanoparticles were dispersed into water to give a homogeneous and stable suspension. After the solvent evaporation, a porous and uniform TiO2 nano-film was obtained on the GCE surface. Further coated with Nafion, the complex film possesses remarkable stability in aqueous solution. This nano-film was characterized by scanning electron microscopy (SEM) and atomic force microscopy (AFM). The prepared electrode showed excellent electrocatalytic behavior of dopamine and high concentration of ascorbic acid does not interfere with the dopamine detection. Based on this, an electrochemical method is developed for the determination of dopamine with simplicity and high sensitivity

  8. Highly Sensitive Bisphenol-A Electrochemical Aptasensor Based on Poly(Pyrrole-Nitrilotriacetic Acid)-Aptamer Film.

    Kazane, Imen; Gorgy, Karine; Gondran, Chantal; Spinelli, Nicolas; Zazoua, Ali; Defrancq, E; Cosnier, Serge

    2016-07-19

    An electrochemical highly sensitive aptasensor was developed based on electropolymerized poly(pyrrole-nitrilotriacetic) acid film and a new aptamer functionalized by a pentahistidine peptide for the quantification of bisphenol A. A surface coverage of antibisphenol A aptamer of 1.84 × 10(-10) mol cm(-2) was estimated from the electrochemical signal of the [Ru(III)(NH3)6](3+) complex bound by electrostatic interactions onto the aptamer-modified electrode. The binding of bisphenol A onto the polymer film was successfully characterized by electrochemical methods as square wave voltammetry and electrochemical impedance spectroscopy measurements. The designed label-free impedimetric aptasensor displayed a wide linear range from 10(-11) to 10(-6) mol L(-1) with a sensitivity of 372 Ω per unit of log of concentration and an excellent specificity toward interfering agents such as 4,4'-dihydroxybiphenyl and bisphenol P. PMID:27332710

  9. Complex formation of Eu(III) with polyacrylic acid

    For the quantitative description of the interaction of metal ions with humic substances, it is necessary to clarify the effects of both polyelectrolyte and heterogeneous nature of humic substances. To estimate the polyelectrolyte effect separately, polyacrylic acid (MW = 90 000) has been selected as a representative of well-defined, homogeneous polymeric weak acids, and its interaction with Eu(III) has been investigated by a solvent extraction method using 152Eu (∝ 10-8 M) with TTA and TBP in xylene. By defining the apparent complex formation constant as βα = [ML]/([M][R]), where [M] = [Eu3+], [ML] is the concentration of Eu(III) associated with polyacrylic acid and [R] = CRα (CR is a total concentration of proton exchanging sites and α is a degree of dissociation determined by potentiometric titration), the apparent constants have been obtained at several pcH and ionic strength (0.1 M and 1.0 M NaClO4). The constants increased with pcH and decreased with an increase of ionic strength, that is, the values of log βα varied from 6.0 (at pcH = 4.7) to 7.6 (pcH = 5.5) at 0.1 M NaClO4 and from 4.8 (pcH = 4.4) to 6.5 (pcH = 5.4) at 1.0 M. The plots of log βα versus log α revealed almost linear relationship both at 0.1 and 1.0 M NaClO4. (orig.)

  10. Application of Lemongrass Oil-Containing Polylactic Acid Films to the Packaging of Pork Sausages

    2016-01-01

    Polylactic acid (PLA) is a biodegradable and renewable polymer, which represents a valuable alternative to plastic packaging films, often associated with environmental problems. In this study, we tested the suitability of PLA as a biodegradable packaging film and assessed the antimicrobial activity of lemongrass oil (LO), incorporated into the PLA film in different concentrations. To obtain the optimal physical properties for PLA films, tensile strength, elongation at break, and water vapor permeability were measured under different preparation conditions. In addition, the antimicrobial activity of the LO contained in the PLA film against Listeria monocytogenes was investigated by disc diffusion and viable cell count. Among all concentrations tested, 2% LO was the most suitable in terms of antimicrobial activity and physical properties of the PLA film. Based on these results, we used the PLA film containing 2% LO to pack pork sausages; after 12 d of storage at 4℃, the population of inoculated L. monocytogenes in the sausage samples wrapped with the PLA film containing 2% LO was reduced by 1.47 Log CFU/g compared with the control samples. Our data indicate that PLA films containing 2% LO represent a valuable means for antimicrobial sausage packaging. PMID:27433114

  11. Electrical properties of biodegradable poly(ε-caprolactone): lithium thiocyanate complexed polymer electrolyte films

    Graphical abstract: - Highlights: • The minimum Tm and χc values are observed in 15 wt% LiSCN complexed film. • The conductivity of PCL:LiSCN complexed films follows Johnscher's power law. • Conductivity and dielectric constant follows the same trend. • The charge carriers responsible for both conduction and relaxation are the same. - Abstract: Lithium ion conducting polymer electrolyte films based on biodegradable poly(ε-caprolactone) (PCL) complexed with lithium thiocyanate (LiSCN) salt were prepared by solution cast technique. Thermal and electrical properties of the polymer electrolyte films were studied using differential scanning calorimetry (DSC) and ac impedance spectroscopy. In order to investigate the ion conduction mechanism and relaxation behavior of complex polymer electrolyte films, the conductivity, dielectric constant, loss tangent and electric modulus were analyzed as a function of frequency and temperature. The variation of conductivity with frequency obeyed the Johnscher's power law. The dielectric constant exhibited a higher value at a lower frequency and increased with rising temperature due to the polar nature of host polymer. The activation energies for both dc conductivity and relaxation had the same value (∼0.87 eV), implying that the charge carriers responsible for both conduction and relaxation were the same

  12. Platinum thin film anodes for solid acid fuel cells

    Louie, Mary W.; Haile, Sossina M.

    2011-01-01

    Hydrogen electro-oxidation kinetics at the Pt | CsH_2PO_4 interface have been evaluated. Thin films of nanocrystalline platinum 7.5–375 nm thick and 1–19 mm in diameter were sputtered atop polycrystalline discs of the proton-conducting electrolyte, CsH_2PO_4, by shadow-masking. The resulting Pt | CsH_2PO_4 | Pt symmetric cells were studied under uniform H_2-H_2O-Ar atmospheres at temperatures of 225–250 °C using AC impedance spectroscopy. For thick platinum films (>50 nm), electro-oxidation o...

  13. Electrochromic iridium oxide films: Compatibility with propionic acid, potassium hydroxide, and lithium perchlorate in propylene carbonate

    Wen, Rui-Tao; Niklasson, Gunnar A.; Granqvist, Claes G.

    2013-01-01

    Porous thin films of It oxide were prepared by reactive dc magnetron sputtering onto unheated substrates. The crystallite size was similar to 5 nm, and a small amount of unoxidized Ir was present. The electrochromic performance was studied by optical transmittance measurements and cyclic voltammetry applied to films in aqueous and non-aqueous electrolytes, specifically being 1 M propionic acid, 1 M potassium hydroxide (KOH), and 1 M lithium perchlorate in propylene carbonate (Li-PC). Cyclic v...

  14. Synthesis and spectroscopic characterization of fluorescent solid rare earth complexes with hydroxamic acids

    2002-01-01

    The complexes RE2(DHYA)3 .nH2O in the title bar were synthesized through some reactions oftrivalent rareearth ions. In the process of synthesis, dihydroxamic acids were taken as ligands while the alcohol was taken as a solvent.The ligands included adipylhydroxamic acid (ADHA), p-phthalichydroxamic acid (PPHA), oxalohydroxamic acid (OXHA), butadihydroxamic acid (BDHA), o-phthalichydroxamic acid (OPHA), benzoylhydroxamic acid (BHA), etc.Measured at 25 ℃, the molar conductances in various modes are 13.00-21.05 S. cm2. mol-1, which shows that rare-earth complexes are nonelectrolytes and the hydroxamino groups of the complexes have taken part in bonding. Infrared spectra, ultraviolet spectra, nuclear magnetic resonance (1HNMR) spectra, and fluorescence spectra were used to investigate the complexes. Experiments have proved that the complexes of Eu3+ and Tb3+ with aromatic hydroxamic acids have good fluorescent characteristics.

  15. Photophysical characterization of layer-by-layer self-assembled films of deoxyribonucleic acid

    D Dey; S A Islam; S A Hussain; D Bhattacharjee

    2008-08-01

    This communication reports the photophysical characterization of self-assembled layer-by-layer (LbL) films of DNA (deoxyribonucleic acid) fabricated at different temperatures by electrostatic interaction with a polycation, poly(allylamine hydrochloride). It was observed that there was a successful incorporation of DNA molecules in DNA–PAH LbL films at room temperature as well as after melting temperature. An abrupt increase in intensity was observed in the absorption spectra of the films fabricated at high temperature which is an indication of the immobilization of unzipped DNA after melting of DNA. The films were observed to remain unaffected even after 250 h of film fabrication. The total electrostatic interaction time between DNA and PAH is about 15 min, that is, no PAH binding site is free.

  16. Microwave complex conductivity of the YBCO thin films as a function of static external magnetic field

    Krupka, J.; Judek, J.; Jastrzebski, C.; Ciuk, T.; Wosik, J.; Zdrojek, M.

    2014-03-01

    A sapphire rod resonator operating at microwave frequencies was used to determine the electric properties of 600 nm thick YBCO films in the superconducting state. The rigorous electromagnetic modelling was applied to transform the measured Q-factor and the resonant frequency to the complex conductivity of high accuracy, which was previously shown to describe the intrinsic properties of superconductor thin films in more precise manner than the complex impedance. Static external magnetic field induces typical transition to normal state due to introduction of magnetic vortices into the sample. Observed magnetic hysteresis has the origin in the strong temperature dependent pinning. Additional energy absorption at about 1.5 T was observed.

  17. Transition Metal–α-Amino Acid Complexes with Antibiotic Activity against Mycobacterium spp.

    Karpin, George W.; Merola, Joseph S.; Joseph O. Falkinham

    2013-01-01

    Synthetic iridium-, rhodium-, and ruthenium-amino acid complexes with hydrophobic l-amino acids have antibiotic activity against Mycobacterium spp., including Mycobacterium bovis BCG and the rapidly growing species Mycobacterium abscessus and Mycobacterium chelonae. Concentrations of transition metal-amino acid complexes demonstrating hemolysis or cytotoxicity were 10- to 25-fold higher than were the MICs.

  18. Investigations of corrosion films formed on API-X52 pipeline steel in acid sour media

    Hernandez-Espejel, A. [Instituto Politecnico Nacional, Departamento de Ingenieria Metalurgica, IPN-ESIQIE, UPALM Ed. 7, Zacatenco 07738, Mexico, D.F. (Mexico); Dominguez-Crespo, M.A. [Instituto Politecnico Nacional, CICATA-Unidad Altamira-Tamaulipas, km 14.5, Carretera Tampico-Puerto Industrial Altamira, 89600 Altamira, Tamps (Mexico); Cabrera-Sierra, R. [Instituto Politecnico Nacional, Departamento de Ingenieria Quimica Industrial, IPN-ESIQIE, UPALM Ed. 7, Zacatenco 07738, Mexico, D.F. (Mexico); Rodriguez-Meneses, C. [Instituto Politecnico Nacional, Departamento de Ingenieria Metalurgica, IPN-ESIQIE, UPALM Ed. 7, Zacatenco 07738, Mexico, D.F. (Mexico); Arce-Estrada, E.M., E-mail: earce@ipn.m [Instituto Politecnico Nacional, Departamento de Ingenieria Metalurgica, IPN-ESIQIE, UPALM Ed. 7, Zacatenco 07738, Mexico, D.F. (Mexico)

    2010-07-15

    Corrosion films formed by voltammetry using different switching potentials and by immersion on API-X52 pipeline steel in simulated acid sour media (NACE ID182) have been characterized using Scanning Electron Microscopy (SEM), X-ray Diffraction (XRD), Linear Polarization and Electrochemical Impedance Spectroscopy (EIS) techniques. XRD and EDS analysis showed that the films are mainly composed of sulphide compounds (mackinawite, troilite, marcasite and pyrite) as well as iron oxides, as steel damage increases. Across SEM micrographs the corrosion films formed by potentiodynamic and immersion tests are very similar, covering most of the steel. Polarization and EIS results corroborate poor behavior against corrosion.

  19. Investigations of corrosion films formed on API-X52 pipeline steel in acid sour media

    Corrosion films formed by voltammetry using different switching potentials and by immersion on API-X52 pipeline steel in simulated acid sour media (NACE ID182) have been characterized using Scanning Electron Microscopy (SEM), X-ray Diffraction (XRD), Linear Polarization and Electrochemical Impedance Spectroscopy (EIS) techniques. XRD and EDS analysis showed that the films are mainly composed of sulphide compounds (mackinawite, troilite, marcasite and pyrite) as well as iron oxides, as steel damage increases. Across SEM micrographs the corrosion films formed by potentiodynamic and immersion tests are very similar, covering most of the steel. Polarization and EIS results corroborate poor behavior against corrosion.

  20. Physicochemical Properties of Edible Chitosan/Hydroxypropyl Methylcellulose/Lysozyme Films Incorporated with Acidic Electrolyzed Water

    Ewa Brychcy

    2015-01-01

    Full Text Available The treatment with acidic electrolyzed water (AEW is a promising disinfection method due to its effectiveness in reducing microbial population. The aim of the study was to evaluate physicochemical properties of chitosan/HPMC films incorporated with lysozyme and acidic electrolyzed water. In the composite films, decreasing film solubility and increasing concentration of sodium chloride solution and prolongation of electrolysis time were observed. Electrolysis process with sodium chloride induces spongy network of film structure. The use of AEW has not changed chemical composition of films which was proved by 1H NMR, MALDI-TOF, and FT-IR spectroscopy. The research confirmed that electrolysis significantly improved thermomechanical properties of the examined films. The contact angle values of the films were quite similar and ranged between 56° and 73°. The increase of salt concentration used in the electrolysis process had an impact on increasing flexibility of samples. Application of electrolyzed water in commonly used food processing systems is possible. Fusion of AEW and biopolymers may provide better integration with coated food product and multidirectional protecting effect.

  1. Comparative evaluation on fatty acid and Matricaria recutita essential oil incorporated into casein-based film.

    Aliheidari, Nahal; Fazaeli, Mahboubeh; Ahmadi, Reza; Ghasemlou, Mehran; Emam-Djomeh, Zahra

    2013-05-01

    Sodium caseinate composite films containing lipids-oleic acid (OA), stearic acid (SA), or Matricaria recutita essential oil (MEO) - were prepared through emulsification and their physical, thermal, mechanical, and barrier properties were evaluated and compared. Furthermore, their antimicrobial effectiveness against Listeria monocytogenes, Staphylococcus aureus, and Escherichia coli was studied. Emulsified films were softer, less rigid, and more stretchable than pure films. The films' water vapor barrier properties were found to decrease upon the addition of lipid content; this effect was greatly reduced when MEO was added. The presence of OA/SA and MEO decreased tensile strength and elastic modulus but increased the elongation at break. Thermal analysis of all emulsified films showed two endothermic peaks; these results confirmed those obtained by SEM studies, where a partial separation of the two phases occurred. The films' antimicrobial activities were increased by incorporating lipids, particularly those containing MEO, which were more effective against the studied bacteria. This work showed that when taking all the studied variables into account, films formulated with MEO were found most suitable for various food applications. PMID:23415659

  2. The anodizing behavior of aluminum in malonic acid solution and morphology of the anodic films

    Ren, Jianjun; Zuo, Yu

    2012-11-01

    The anodizing behavior of aluminum in malonic acid solution and morphology of the anodic films were studied. The voltage-time response for galvanostatic anodization of aluminum in malonic acid solution exhibits a conventional three-stage feature but the formation voltage is much higher. With the increase of electrolyte concentration, the electrolyte viscosity increases simultaneously and the high viscosity decreases the film growth rate. With the concentration increase of the malonic acid electrolyte, the critical current density that initiates local "burning" on the sample surface decreases. For malonic acid anodization, the field-assisted dissolution on the oxide surface is relatively weak and the nucleation of pores is more difficult, which results in greater barrier layer thickness and larger cell dimension. The embryo of the porous structure of anodic film has been created within the linear region of the first transient stage, and the definite porous structure has been established before the end of the first transient stage. The self-ordering behavior of the porous film is influenced by the electrolyte concentration, film thickness and the applied current density. Great current density not only improves the cell arrangement order but also brings about larger cell dimension.

  3. Kinetics and mechanism of reduction of iron (III) kojic acid complex by ascorbic acid

    Kinetics of reduction of iron (III) kojic acid complex by ascorbic acid has been carried out using photodiode array spectrophotometer over the ranges: 4.0<=pH<=5.5 and 5.0<=T<=25.0 degree C at ionic strength 0.2 M under pseudo-first order conditions by stopped-flow technique. Rate of the reaction was found to be pH dependent. The redox reaction followed the saturation kinetics. The rate law is deduced as follows: Rate = (k/sub 3/k/sub eq(H/sup +/)(HAsc/sup -/)(Fe(KA)/sub 3/) / (HKA) + K/sub eq/(H/sup +/)(HAsc/sup -/) The activation parameters of this reaction were determined. A mechanism consistent with this rate law has been proposed. (author)

  4. Influence of the use of acids and films in post-harvest lychee conservation

    Danielle Fabíola Pereira da Silva

    2012-12-01

    Full Text Available Lychee (Litchi chinensis Sonn. has a high commercial value; however, it has a short shelf-life because of its rapid pericarp browning. The objective of this study was to evaluate the shelf-life of 'Bengal' lychee fruits stored after treatment with hydrochloric acid and citric acid, associated with cassava starch and plastic packaging. Uniformly red pericarp fruits were submitted to treatments: 1-(immersion in citric acid 100 mM for 5 minutes + cassava starch 30 g L-1 for 5 minutes, 2-(immersion in hydrochloric acid 1 M for 2 minutes + starch cassava 30 g L-1 for 5 minutes, 3-(immersion in citric acid 100 mM for 5 minutes + polyvinyl chloride film (PVC, 14 µm thick and 4-(immersion in hydrochloric acid 1 M for 2 minutes + PVC film. During 20 days, the fruits were evaluated for mass loss, pericarp color, pH, soluble solids and titratable acidity, vitamin C of the pulp and pericarp and activities of polyphenol oxidase and peroxidase of the pericarp. The treatment with hydrochloric acid associated with PVC was the most effective in maintaining the red color of the pericarp for a period of 20 days and best preservation of the fruit. The cassava starch associated with citric acid, and hydrochloric acid did not reduce the mass loss and did not prevent the browning of lychee fruit pericarp.

  5. Ultra-Thin Films of Poly(acrylic acid)/Silver Nanocomposite Coatings for Antimicrobial Applications

    Alaa Fahmy; Eisa, Wael H.; Mohamed Yosef; Ali Hassan

    2016-01-01

    In this work not only colloids of poly(acrylic acid) (PAA) embedded with silver nanoparticles (Ag-NPs) but thin films (10 nm) also were deposited using electrospray deposition technique (ESD). A mixture of sodium borohydride (NaBH4) and ascorbic acid (AA) were utilized to reduce the silver ions to generate Ag-NPs in the PAA matrix. Moreover, sodium tricitrate was used to stabilize the prepared colloids. The obtained colloids and films were characterized using UV-visible, transmission electron...

  6. Refractive index modulation in polymer film doped with diazo Meldrum's acid

    Zanutta, Alessio; Villa, Filippo; Bertarelli, Chiara; Bianco, Andrea

    2016-08-01

    Diazo Meldrum's acid undergoes a photoreaction induced by UV light and it is used as photosensitizer in photoresists. Upon photoreaction, a change in refractive index occurs, which makes this system interesting for volume holography. We report on the sublimation effect at room temperature and the effect of photoirradiation on the refractive index in thin films of CAB (Cellulose acetate butyrate) doped with different amount of diazo Meldrum's acid. A net modulation of the refractive index of 0.01 is achieved with 40% of doping ratio together with a reduction of the film thickness.

  7. Electrical Transport in Nanoscale Complex Oxide Thin Films: Strontium titanate and RNiO3

    Son, Junwoo

    Complex oxide thin films have attracted significant attention due to a wealth of physical phenomena, such as ferroelectricity and Mott transitions arising from strong interactions in d-bands. Moreover, the physical phenomena observed in these materials exhibit sensitivities, which are not found in conventional semiconductors and give rise to abrupt changes in their physical properties. The richness of electronic phases and unique functionalities of complex oxides are attractive for applications in next-generation electronic devices. To realize new electronic devices with complex oxides, it is essential to understand the mechanisms of the electrical transport and to control the transport properties of complex oxide thin films. In this dissertation, electrical transport phenomena and their electrical control are experimentally studied in two different complex oxide thin film systems, exhibiting resistive switching and Mott metal-insulator transitions. The first part will briefly discuss resistive switching in ultrathin SrTiO3 tunnel junctions in metal-insulator-metal (MIM) geometry. The current-voltage characteristics provide hints of the origin of the resistive switching phenomena in SrTiO3 tunnel barriers, which are also relevant for resistive switching in thicker films. The second part focuses on the control of metal-insulator transitions in RNiO3, where R = trivalent rare earth ion, using different strategies: band-width control and band-filling control. The electrical transport in low-dimensional, strongly correlated LaNiO3 is explored in terms of band-width control by strain and dimensionality. A new concept of band-filling control in nanoscale NdNiO3 thin films by modulation doping is discussed, and the experimental charge injection from high-quality La-doped SrTiO3 into NdNiO3 thin films is experimentally studied. The potential and limitations of a Modulation-doped Mott Field Effect Transistor (MM-FET) for future "Mott" electronic devices is discussed.

  8. Complex Formation of Selected Radionuclides with Ligands Commonly Found in Ground Water: Low Molecular Organic Acids

    Jensen, Bror Skytte; Jensen, H.

    1985-01-01

    A general approach to the analysis of potentiometric data on complex formation between cations and polybasic amphoteric acids is described. The method is used for the characterisation of complex formation between Cs+, Sr2+, Co2+, La 3+, and Eu3+ with a α-hydroxy acids, tartaric acid and citric acid......, and with the α-amino acids, aspartic acid and L-cysteine. The cations have been chosen as typical components of reactor waste, and the acids because they are often found as products of microbial activity in pits or wherever organic material decays...

  9. Zn/Al complex-SWCNT ink for transparent and conducting homogeneous films by scalable bar coating method

    Kukobat, Radovan; Hayashi, Takuya; Matsuda, Takafumi; Sunaga, Motoo; Sakai, Toshio; Futamura, Ryusuke; Kaneko, Katsumi

    2016-04-01

    It is shown that the viscosity of SWCNT inks is essential to produce highly homogeneous SWCNT films on the PET substrate with bar coating method. The Zn/Al complex-aided SWCNT ink has a viscosity threshold of 1.30 mPa s for the preparation of homogeneous films. The local flows of the film are suppressed above this viscosity, allowing homogeneous film formation. The Zn/Al complex dispersant can be easily removed from SWCNTs coated on PET by 1 M HNO3, giving a pure SWCNT film with the sheet resistance of 150 ohm/sq and transmittance of 90% at 550 nm immediately after HNO3 treatment.

  10. Preparation, characterization and evaluation of drug-delivery systems: Pectin and mefenamic acid films

    Moreira, R.B. [Universidade Federal de Mato Grosso, Rodovia MT-100, Km 3,5, Barra do Garças, MT CEP 78600-000 (Brazil); Teixeira, J.A. [Universidade Federal de Mato Grosso, Cuiabá, MT CEP 78060-900 (Brazil); Furuyama-Lima, A.M. [Universidade Estadual Paulista, IBILCE, São José do Rio Preto, SP CEP 15054-000 (Brazil); Souza, N.C. de [Universidade Federal de Mato Grosso, Rodovia MT-100, Km 3,5, Barra do Garças, MT CEP 78600-000 (Brazil); Siqueira, A.B., E-mail: buzutti@cpd.ufmt.br [Universidade Federal de Mato Grosso, Rodovia MT-100, Km 3,5, Barra do Garças, MT CEP 78600-000 (Brazil)

    2014-08-20

    Highlights: • The films were prepared and characterized by FTIR, TG–DSC/FTIR and AFM microscopy. • The results provided information on the composition, dehydration, thermal stability, thermal decomposition. • DSC results of CaHCl shows two overlapping endothermic peaks. • The AFM image shows great similarity for A5 and A6 films. • A5 and A6 films functioned well as a topical delivery system. - Abstract: Mefenamic acid (H-Mef) is a nonsteroidal anti-inflammatory drug (NSAID). Various adhesive dosage forms of NSAIDs have been developed, which include adhesive tablets, gels, ointments, patches and more recently, polymeric films. The objective of this study was the development of H-Mef adhesive films to be used as a drug-delivery system with different ratios of pectin and calcium chloride dihydrate by the casting technique. The materials were characterized by TG–DSC coupled FTIR, AFM (atomic force microscopy) and spectroscopic techniques. The results provided information about the dehydration, film roughness, surface morphology, thermal decomposition, as well as identification of gaseous products evolved during thermal decomposition. The characterizations indicated the A5 and A6 films functioned well, with 99% H-Mef released within 15 min at pH 5, suggesting these degradable films could be used as a topical delivery system.

  11. Preparation, characterization and evaluation of drug-delivery systems: Pectin and mefenamic acid films

    Highlights: • The films were prepared and characterized by FTIR, TG–DSC/FTIR and AFM microscopy. • The results provided information on the composition, dehydration, thermal stability, thermal decomposition. • DSC results of CaHCl shows two overlapping endothermic peaks. • The AFM image shows great similarity for A5 and A6 films. • A5 and A6 films functioned well as a topical delivery system. - Abstract: Mefenamic acid (H-Mef) is a nonsteroidal anti-inflammatory drug (NSAID). Various adhesive dosage forms of NSAIDs have been developed, which include adhesive tablets, gels, ointments, patches and more recently, polymeric films. The objective of this study was the development of H-Mef adhesive films to be used as a drug-delivery system with different ratios of pectin and calcium chloride dihydrate by the casting technique. The materials were characterized by TG–DSC coupled FTIR, AFM (atomic force microscopy) and spectroscopic techniques. The results provided information about the dehydration, film roughness, surface morphology, thermal decomposition, as well as identification of gaseous products evolved during thermal decomposition. The characterizations indicated the A5 and A6 films functioned well, with 99% H-Mef released within 15 min at pH 5, suggesting these degradable films could be used as a topical delivery system

  12. Porous poly(DL-lactic acid) matrix film with antimicrobial activities for wound dressing application.

    Chitrattha, Sasiprapa; Phaechamud, Thawatchai

    2016-01-01

    Poly(lactic acid) (PLA) is polymeric biomaterial that has been used for wound dressing due to its biodegradability and biocompatibility. However, PLA has some limitations including poor toughness, low degradation rate and high hydrophobicity. The aim of this study is to develop an antibiotic drug-loaded PLA porous film as wound dressing with antibacterial activity. PLA porous film was fabricated by temperature change technique using solvent casting method. Polyethylene glycol (PEG) 400 was added for improving the pore interconnectivity of film. Gentamicin sulfate (GS) or metronidazole (MZ) was incorporated into PLA porous films. PLA containing PEG 400 exhibited the more amorphous form than plain PLA film and contained 55.31 ± 2.85% porosity and 20 μm of the pore size which significantly improved the water vapor transmission rate, oxygen transmission rate, degradation rate and percentage of drug release, respectively. Drug-loaded porous films efficiently inhibited the bacteria growth. GS-loaded film inhibited Staphylococcus aureus, Proteus mirabilis, Pseudomonas aeruginosa, whereas MZ-loaded film inhibited Bacteroides fragilis and the sustainable antibacterial activity was attained for 7 days. PMID:26478412

  13. UV assisted photoelectrocatalytic oxidation of phthalic acid using spray deposited Al doped zinc oxide thin films

    Mahadik, M.A.; Shinde, S.S.; Hunge, Y.M.; Mohite, V.S.; Kumbhar, S.S.; Moholkar, A.V.; Rajpure, K.Y.; Bhosale, C.H., E-mail: chbhosale@gmail.com

    2014-10-25

    Highlights: • Nanostructured undoped and AZO thin films prepared by chemical spray pyrolysis. • Effect of Al doping on the structural, morphological and photoluminance properties. • Photocatalytic degradation of phthalic acid under UV light illumination. • Reaction kinetics and mineralization of phthalic acid. - Abstract: Undoped and Al doped ZnO (AZO) thin films are successfully prepared by spray pyrolysis technique at optimised substrate temperature of 400 °C onto amorphous and F:SnO{sub 2} coated glass substrates. Effect of Al doping on structural, morphological and optical properties of ZnO thin films is studied. Deposited films are polycrystalline with a hexagonal (wurtzite) crystal structure having (0 0 2) preferred orientation. The PEC characterization shows that, short circuit current (I{sub sc}) and open circuit voltage (V{sub oc}) are (I{sub sc} = 0.38 mA and V{sub oc} = 421 mV) relatively higher at the 3 at.% Al doping. SEM images show deposited thin films are compact and uniform with seed like grains. All films exhibit average transmittance of about 82% in the visible region and a sharp absorption onset at 375 nm corresponding to 3.3 eV. The photocatalytic activities of the large surface area (64 cm{sup 2}) Al-doped ZnO photocatalyst samples were evaluated by photoelectrocatalytic degradation of phthalic acid under UV light irradiation. The results show that the 3 at.% AZO thin film photocatalyst exhibited degradation of phthalic acid up to about 45% within 3 h with significant reduction in COD and TOC values.

  14. Complexation of metal ions with humic acid: metal ion charge neutralization model

    The humic acid complexation reaction presented in this work is based on the concept of metal ion charge neutralization upon complexation to humic acid functional groups. Experimental results from the complexation of UO22+, Am3+, and Cm3+ with humic acids of different origin are presented to demonstrate and validate the proposed model. By introducing the operational humic acid concentration and the loading capacity, the complexation constants are derived, which are independent of the metal ion concentration, pH, and origin of humic acid. The loading capacity is an operational term needed for the intercomparison of stability constants and is the mole fraction of the maximum available complexing sites of humic acid under a given set of experimental conditions. The metal ion charge neutralization model adequately describes the thermodynamic equilibrium reaction of metal ions with humic acid and allows a direct application of the resulting stability constants for geochemical modeling of actinide migration at an environmentally relevant pH. (orig.)

  15. Polyurethane films modified by antithrombin-heparin complex to enhance endothelialization: An original impedimetric analysis

    In this paper, polyurethane (PU) was deposited as a thin layer onto the surface of ITO (indium tin oxide) and was then modified with an antithrombin-heparin complex (ATH). The resulting films were characterized by ATR spectroscopy, contact angle measurements and electrochemical impedance spectroscopy (EIS). Physicochemical characterization confirmed the surface modifications. The obtained films were used as substrates for endothelial cell attachment and growth. These processes were characterized using electrochemical impedance spectroscopy (EIS). We observed that the addition of a small amount of heparin and AT additives onto the polymer surface resulted in a considerable change in the surface characteristics, and we found that PU films that were modified by the ATH complex were able to greatly enhance adhesion and proliferation of endothelial cells (ECs).

  16. Microscale and nanoscale hierarchical structured mesh films with superhydrophobic and superoleophilic properties induced by long-chain fatty acids

    Wang, Shutao; Song, Yanlin; Jiang, Lei

    2007-01-01

    Inspired by the lotus effect, we fabricate new microscale and nanoscale hierarchical structured copper mesh films by a simple electrochemical deposition. After modification of the long-chain fatty acid monolayer, these films show superhydrophobic and superoleophilic properties, which could be used for the effective separation of oil and water. The length of the fatty acid chain strongly influences the surface wettability of as-prepared films. It is confirmed that the cooperative effect of the hierarchical structure of the copper film and the nature of the long-chain fatty acid contribute to this unique surface wettability.

  17. Microscale and nanoscale hierarchical structured mesh films with superhydrophobic and superoleophilic properties induced by long-chain fatty acids

    Wang Shutao [Center for Molecular Science, Institute of Chemistry, Beijing 100080 (China); Song Yanlin [Center for Molecular Science, Institute of Chemistry, Beijing 100080 (China); Jiang Lei [Center for Molecular Science, Institute of Chemistry, Beijing 100080 (China)

    2007-01-10

    Inspired by the lotus effect, we fabricate new microscale and nanoscale hierarchical structured copper mesh films by a simple electrochemical deposition. After modification of the long-chain fatty acid monolayer, these films show superhydrophobic and superoleophilic properties, which could be used for the effective separation of oil and water. The length of the fatty acid chain strongly influences the surface wettability of as-prepared films. It is confirmed that the cooperative effect of the hierarchical structure of the copper film and the nature of the long-chain fatty acid contribute to this unique surface wettability.

  18. Microscale and nanoscale hierarchical structured mesh films with superhydrophobic and superoleophilic properties induced by long-chain fatty acids

    Inspired by the lotus effect, we fabricate new microscale and nanoscale hierarchical structured copper mesh films by a simple electrochemical deposition. After modification of the long-chain fatty acid monolayer, these films show superhydrophobic and superoleophilic properties, which could be used for the effective separation of oil and water. The length of the fatty acid chain strongly influences the surface wettability of as-prepared films. It is confirmed that the cooperative effect of the hierarchical structure of the copper film and the nature of the long-chain fatty acid contribute to this unique surface wettability

  19. Complex formation of Eu(III) with humic acid and polyacrylic acid

    With the intention of estimating the effect of the heterogeneous composition in the humic acid separately from its polyelectrolyte effect, comparative study on the interaction of Eu(III) with humic acid and polyacrylic acid has been carried out by the solvent extraction method with 10-3 M TTA and 10-3 M TBP in xylene at various total concentrations of Eu(III) (10-8 M to 10-5 M), pcH (5.0 to 5.5) and ionic strengths (0.02 to 1.0 M NaClO4). The interaction has been discussed in terms of the apparent complex formation constants, βα = [ML]/([M][R]), where [M] and [ML] are the concentrations of free and bound Eu3+ ion and [R] is the concentration of dissociated proton exchanging site. For both humate and polyacrylate, log βα increased with pcH or the degree of ionization and decreased with ionic strength. The Eu3+ ion concentration had no appreciable influence on the complex formation of Eu(III)-polyacrylate, and the values of log βα were obtained to be 7.57 ± 0.05 (I = 0.1, pcH = 5.53), 7.13 ± 0.04 (I = 0.1, pcH = 5.20), 6.68 ± 0.04 (I = 1.0, pcH = 5.54) and 5.61 ± 0.09 (I = 1.0, pcH = 4.73). On the other hand, log βα of humate remarkably decreased with the Eu3+ ion concentration; from 9.32 ([Eu3+] = 10-11.9 M) to 7.20 ([Eu3+] = 10-7.5 M) at pcH = 5.53 in 0.02 M NaClO4, from 8.63 ([Eu3+] = 10-12.5 M) to 6.35 ([Eu3+] = 10-7.2 M) at pcH = 5.53 in 0.1 M and from 7.59 ([Eu3+] = 10-10.7 M) to 5.20 ([Eu3+] = 10-7.0 M) at pcH = 5.52 in 1.0 M. The observed dependence of log βα of humate on the concentration of metal ion strongly suggests the heterogeneity of the complexing sites (the coexistence of weak and strong binding sites) in the humic acid. (orig.)

  20. Preparation and Characterization of Films Extruded of Polyethylene/Chitosan Modified with Poly(lactic acid

    Jesús Manuel Quiroz-Castillo

    2014-12-01

    Full Text Available The use of mixtures of synthetic and natural polymers is a potential option to reduce the pollution by plastic waste. In this work, the method for the chemical modification of chitosan with poly(lactic acid was developed; then, the preparation of films of blends of polyethylene and chitosan-poly(lactic acid produced by an extrusion method using polyethylene-graft maleic anhydride as a compatibilizer. It was possible to obtain films with a maximum content of 20 wt% and 30 wt%, chitosan, with and without compatibilizer, respectively. Scanning electron microscope (SEM analysis showed a homogeneous surface on all films. The addition of the compatibilizer had a significant effect on the mechanical properties of the films, such as an increase in Young’s modulus and a decrease in the elongation at break; additionally, the compatibilizer promotes thermal degradation in a single step and gives the film a slight increase in thermal resistance. These results are attributed to an improved interaction in the interface of polyethylene and chitosan-poly(lactic acid, promoted by the compatibilizer.

  1. Enhanced charge transport in highly conducting PEDOT-PSS films after acid treatment

    Shiva, V. Akshaya; Bhatia, Ravi; Menon, Reghu

    The high electrical conductivity, good stability, high strength, flexibility and good transparency of poly(3,4-ethylenedioxythiophene)-poly(styrenesulfonate) (PEDOT-PSS), make it useful for many applications including polymeric anodes for organic photovoltaics, light-emitting diodes, flexible electrodes, supercapacitors, electrochromic devices, field-effect transistors and antistatic-coatings. However, the electrical conductivity of PEDOT-PSS has to be increased significantly for replacement of indium tin oxide (ITO) as the transparent electrode in optoelectronic devices. The as prepared (pristine) PEDOT-PSS film prepared from the PEDOT-PSS aqueous solution usually has conductivity below 1Scm-1, remarkably lower than ITO. Significant conductivity enhancement has been observed on transparent and conductive PEDOT-PSS films after a treatment with inorganic acids. Our study investigates the charge transport in pristine and H2SO4, HNO3, HCl treated PEDOT-PSS films. We have treated the films with various concentrations of acids to probe the effect of the acid treatment on the conduction mechanism. The study includes the measurement of dc and electric field dependent conductivity of films in the temperature range of 4.2K-300K. We have also performed magneto-resistance measurements in the range of 0-5T. An enhancement by a factor of~103 has been observed in the room temperature conductivity. The detailed magneto-transport studies explain the various mechanisms for the conductivity enhancement observed.

  2. Exceptionally crystalline and conducting acid doped polyaniline films by level surface assisted solution casting approach

    Puthirath, Anand B.; Methattel Raman, Shijeesh; Varma, Sreekanth J.; Jayalekshmi, S.

    2016-04-01

    Emeraldine salt form of polyaniline (PANI) was synthesized by chemical oxidative polymerisation method using ammonium persulfate as oxidant. Resultant emeraldine salt form of PANI was dedoped using ammonia solution and then re-doped with camphor sulphonic acid (CSA), naphthaline sulphonic acid (NSA), hydrochloric acid (HCl), and m-cresol. Thin films of these doped PANI samples were deposited on glass substrates using solution casting method with m-cresol as solvent. A level surface was employed to get homogeneous thin films of uniform thickness. Detailed X-ray diffraction studies have shown that the films are exceptionally crystalline. The crystalline peaks observed in the XRD spectra can be indexed to simple monoclinic structure. FTIR and Raman spectroscopy studies provide convincing explanation for the exceptional crystallinity observed in these polymer films. FESEM and AFM images give better details of surface morphology of doped PANI films. The DC electrical conductivity of the samples was measured using four point probe technique. It is seen that the samples also exhibit quite high DC electrical conductivity, about 287 S/cm for CSA doped PANI, 67 S/cm for NSA doped PANI 65 S/cm for HCl doped PANI, and just below 1 S/cm for m-cresol doped PANI. Effect of using the level surface for solution casting is studied and correlated with the observed crystallinity.

  3. Stretchability of Silver Films on Thin Acid-Etched Rough Polydimethylsiloxane Substrates Fabricated by Electrospray Deposition

    Mehdi, S. M.; Cho, K. H.; Kang, C. N.; Choi, K. H.

    2015-07-01

    This paper investigates the fabrication of Ag films through the electrospray deposition (ESD) technique on sub-millimeter-thick acid-etched rough polydimethylsiloxane (PDMS) substrates having both low and high modulus of elasticity. The main focus of the study is on the stretchable behavior of ESD-deposited Ag nanoparticles-based thin films on these substrates when subjected to axial strains. Experimental results suggest that the as-fabricated films on thin acid-etched rough low modulus PDMS has an average stretchability of 5.6% with an average increase in the resistance that is 23 times that of the initial resistance at electrical failure (complete rupture of the films). Comparatively, the stretchability of Ag films on the high modulus PDMS was found to be 3 times higher with 4.65 times increase in the resistance at electrical failure. Also, a high positive value of the piezoresistive coefficient for these films suggests that the resistivity changes during stretching, and thus deviation from the simplified models is inevitable. Based on these results, new models are presented that quantify the changes in resistance with strain.

  4. Synthesis and characterization of rough electrochromic phosphotungstic acid films obtained by spray-gel process

    Rough electrochromic phosphotungstic acid (PWA) films were fabricated by spraying a gel of phosphotungstate anions with a molar ratio of P:W = 1:12 onto glass substrates precoated with transparent and electrically conducting SnO2:F at 300 oC. The analysis by X-ray photoelectron spectroscopy (XPS) determined that the P:W molar ratio in the films was approximately 1:14. Infrared spectroscopy (IR) and X-ray diffraction (XRD) showed that the film is a polycrystalline phosphotungstic acid. SEM micrographs showed that the films present a rough morphology based on fiber-shape bridges. Optoelectrochemical measurements demonstrated pronounced electrochromism in the PWA films upon H+ intercalation/deintercalation with a high diffuse reflectance (Rd) and transmittance (Td). We found for as-deposited films that Rd/total reflectance (Rt) and Td/total transmittance (Tt) at 550 nm was around 0.83 and 0.68, respectively. This ratio decreases at bleached state to 0.74 and 0.41 for Rd/Rt and Td/Tt, respectively. (authors)

  5. Effects of deposition time in chemically deposited ZnS films in acidic solution

    Haddad, H.; Chelouche, A., E-mail: azeddinechelouche@gmail.com; Talantikite, D.; Merzouk, H.; Boudjouan, F.; Djouadi, D.

    2015-08-31

    We report an experimental study on the synthesis and characterization of zinc sulfide (ZnS) single layer thin films deposited on glass substrates by chemical bath deposition technique in acidic solution. The effect of deposition time on the microstructure, surface morphology, optical absorption, transmittance, and photoluminescence (PL) was investigated by X-ray diffraction (XRD), scanning electronic microscopy (SEM), UV-Vis–NIR spectrophotometry and photoluminescence (PL) spectroscopy. The results showed that the samples exhibit wurtzite structure and their crystal quality is improved by increasing deposition time. The latter, was found to affect the morphology of the thin films as showed by SEM micrographs. The optical measurements revealed a high transparency in the visible range and a dependence of absorption edge and band gap on deposition time. The room temperature PL spectra indicated that all ZnS grown thin films emit a UV and blue light, while the band intensities are found to be dependent on deposition times. - Highlights: • Single layer ZnS thin films were deposited by CBD in acidic solution at 95 °C. • The effect of deposition time was investigated. • Coexistence of ZnS and ZnO hexagonal structures for time deposition below 2 h • Thicker ZnS films were achieved after monolayer deposition for 5 h. • The highest UV-blue emission observed in thin film deposited at 5 h.

  6. Effects of deposition time in chemically deposited ZnS films in acidic solution

    We report an experimental study on the synthesis and characterization of zinc sulfide (ZnS) single layer thin films deposited on glass substrates by chemical bath deposition technique in acidic solution. The effect of deposition time on the microstructure, surface morphology, optical absorption, transmittance, and photoluminescence (PL) was investigated by X-ray diffraction (XRD), scanning electronic microscopy (SEM), UV-Vis–NIR spectrophotometry and photoluminescence (PL) spectroscopy. The results showed that the samples exhibit wurtzite structure and their crystal quality is improved by increasing deposition time. The latter, was found to affect the morphology of the thin films as showed by SEM micrographs. The optical measurements revealed a high transparency in the visible range and a dependence of absorption edge and band gap on deposition time. The room temperature PL spectra indicated that all ZnS grown thin films emit a UV and blue light, while the band intensities are found to be dependent on deposition times. - Highlights: • Single layer ZnS thin films were deposited by CBD in acidic solution at 95 °C. • The effect of deposition time was investigated. • Coexistence of ZnS and ZnO hexagonal structures for time deposition below 2 h • Thicker ZnS films were achieved after monolayer deposition for 5 h. • The highest UV-blue emission observed in thin film deposited at 5 h

  7. Optical Absorption, Stability and Structure of NpO2+ Complexes with Dicarboxylic Acids

    Complexation of NpO2+ with oxalic acid (OX),2,2'-oxydiacetic acid (ODA), 2,2'-iminodiacetic acid (IDA) and 2,2'-thiodiacetic acid (TDA), has been studied using spectrophotometry in1 M NaClO4. Both the position and the intensity of the absorption band of NpO2+ at 980 nm are affected by the formation of NpO2+/dicarboxylate complexes, providing useful information on the complexation strength, the coordination mode and the structure of the complexes

  8. Quantum chemical prediction of paramagnetic NMR spectra of lanthanide complexes with salicylic acid in water solution

    17O and 13C paramagnetic NMR (PNMR) shifts have been calculated for Gd complexes with salicylic acid in water solution. These complexes served us as model compounds for simulation of more complicated lanthanide complexes with humic acids. The obtained data demonstrate that paramagnetic NMR spectra are very sensitive to the bonding details of the ligand. Our calculations suggest that formation of Gd(III) complex with salicylic acid in water solution via carboxyl group with uni-dentate coordination is preferable. New experimental studies with the enriched 17O and 13C nuclei of carboxylate groups of the salicylic and humic acids are extremely desirable

  9. Influence of humic acid size on actinide complexation

    The complexation of Am(III) and Eu(III) with humic acid of different molecular sizes was measured and the data for the ≥300kD and ≥10kD sized HA at pcH 4.0 and 6.0 was analyzed by the Charge Neutralization Model (CNM) and the Polyelectrolyte Model (PM). For the PM, solvent extraction was used to obtain the stability constants of 241Am at tracer concentration. For the CNM, ultrafiltration was used to determine the loading capacity and the stability constants for Eu(III) at macro concentrations. There was a difference of 1-2 orders of magnitude in the stability constants from the two models. The 5D0-7F0 excitation spectra of Eu(III) as a function of loading of HA was found to have a shift in wavenumbers of the peak maximum, indicating that the coordination environment of Eu(III) varied with pH, presumably due to variation in the number of functional groups of the humate bound to the metal ion

  10. Complex modulation of androgen responsive gene expression by methoxyacetic acid

    Stanley Kerri A

    2011-03-01

    Full Text Available Abstract Background Optimal androgen signaling is critical for testicular development and spermatogenesis. Methoxyacetic acid (MAA, the primary active metabolite of the industrial chemical ethylene glycol monomethyl ether, disrupts spermatogenesis and causes testicular atrophy. Transcriptional trans-activation studies have indicated that MAA can enhance androgen receptor activity, however, whether MAA actually impacts the expression of androgen-responsive genes in vivo, and which genes might be affected is not known. Methods A mouse TM3 Leydig cell line that stably expresses androgen receptor (TM3-AR was prepared and analyzed by transcriptional profiling to identify target gene interactions between MAA and testosterone on a global scale. Results MAA is shown to have widespread effects on androgen-responsive genes, affecting processes ranging from apoptosis to ion transport, cell adhesion, phosphorylation and transcription, with MAA able to enhance, as well as antagonize, androgenic responses. Moreover, testosterone is shown to exert both positive and negative effects on MAA gene responses. Motif analysis indicated that binding sites for FOX, HOX, LEF/TCF, STAT5 and MEF2 family transcription factors are among the most highly enriched in genes regulated by testosterone and MAA. Notably, 65 FOXO targets were repressed by testosterone or showed repression enhanced by MAA with testosterone; these include 16 genes associated with developmental processes, six of which are Hox genes. Conclusions These findings highlight the complex interactions between testosterone and MAA, and provide insight into the effects of MAA exposure on androgen-dependent processes in a Leydig cell model.

  11. Characterization of Active Packaging Films Made from Poly(Lactic Acid)/Poly(Trimethylene Carbonate) Incorporated with Oregano Essential Oil

    Dong Liu; Hongli Li; Lin Jiang; Yongming Chuan; Minglong Yuan; Haiyun Chen

    2016-01-01

    Antimicromial and antioxidant bioactive films based on poly(lactic acid)/poly(trimenthylene carbonate) films incorporated with different concentrations of oregano essential oil (OEO) were prepared by solvent casting. The antimicrobial, antioxidant, physical, thermal, microstructural, and mechanical properties of the resulting films were examined. Scanning electron microscopy analysis revealed that the cross-section of films became rougher when OEO was incorporated into PLA/PTMC blends. Differ...

  12. Friction reducing behavior of stearic acid film on a textured aluminum substrate

    Zhang, Quan [School of Mechanical Engineering, Qingdao Technological University, Qingdao 266033 (China); Wan, Yong, E-mail: wanyong@qtech.edu.cn [School of Mechanical Engineering, Qingdao Technological University, Qingdao 266033 (China); Li, Yang; Yang, Shuyan [School of Mechanical Engineering, Qingdao Technological University, Qingdao 266033 (China); Yao, Wenqing [Analysis Center of Tsinghua University, Beijing 100084 (China)

    2013-09-01

    A simple two-step process was developed to render the aluminum hydrophobicity with lower friction. The textured aluminum substrate was firstly fabricated by immersed in a sodium hydroxide solution at 100 °C for 1 h. Stearic acid film was then deposited to acquire high hydrophobicity. Scanning electron microscopy, IR spectroscopy and water contact angle measurements were used to analyze the morphological features, chemical structure and hydrophobicity of prepared samples, respectively. Moreover, the friction reducing behavior of the organic–inorganic composite film on aluminum sliding against steel was evaluated in a ball-on-plate configuration. It was found that the stearic acid film on the textured aluminum led to decreased friction with significantly extended life.

  13. Micromachined dense palladium electrodes for thin-film solid acid fuel cells

    Unnikrishnan, Sandeep

    2009-01-01

    This thesis paves the way towards the microfabrication of a solid acid electrolyte based fuel cell (µSAFC), which has a membrane electrode assembly (MEA) consisting of a thin-film of water soluble electrolyte encapsulated between two dense palladium electrode membranes. This project work investigate

  14. Physicochemical properties of poly(lactic acid-co-glycolic acid film modified via blending with poly(butyl acrylate-co-methyl methacrylate

    Guoquan Zhu

    2013-01-01

    Full Text Available A series of poly(lactic acid-co-glycolic acid (PLGA/poly(butyl acrylate-co-methyl methacrylate (P(BA-co-MMA blend films with different P(BA-co-MMA mole contents were prepared by casting the polymer blend solution in chloroform. Surface morphologies of the PLGAP(BA-co-MMA blend films were studied by scanning electron microscopy (SEM. Thermal, mechanical, and chemical properties of PLGAP(BA-co-MMA blend films were investigated by differential scanning calorimeter (DSC, thermogravimetric analysis (TGA, tensile tests, and surface contact angle tests. The introduction of P(BA-co-MMA could modify the properties of PLGA films.

  15. Graft copolymers obtained by radiation grafting of methacrylic acid onto polypropylene films

    Direct radiation grafting of methacrylic acid (MAA) onto polypropylene films (PP) was studied. The effect of different solvents such as benzene, distilled water, dimethyl formamide, isopropanol, isopropanol/water-mixture, on the swelling and the grafting process of MAA onto (PP) films was investigated. It was found that the grafting process was enhanced under vacuum irradiation in benzene as a diluent for MAA as compared with other solvents examined. The dependence of the grafting rate on such monomer concentrations was found to be 1.2 order. The relationship between the grafting rate and film thickness gave a negative first order dependence. This grafting system proceeded by a diffusion controlled process. Some selected properties of the grafted films such as mechanical and electrical properties, swelling behaviour, and gel determination, were also investigated. (author)

  16. Development and Characterization of Novel Polyurethane Films Impregnated with Tolfenamic Acid for Therapeutic Applications

    Hilal Istanbullu

    2013-01-01

    Full Text Available The present study deals with the preparation of polyurethane (PU films impregnated with a nonsteroidal anti-inflammatory drug, tolfenamic acid (TA. Solvent evaporation technique has been employed for the preparation of TA-PU films in two different ratios of 1 : 2 and 1 : 5 in Tetrahydrofuran (THF or THF-ethanol mixtures. The prepared films were characterized using X-Ray Diffraction (XRD, Differential Scanning Calorimetry (DSC, Fourier Transform Infrared Spectroscopy (FTIR, Scanning Electron Microscopy (SEM, and release studies. The results indicate transformation of crystalline TA to its amorphous form. The degree of crystallinity changes both by increasing the polymer concentration and solvent used for the film preparations. The release profiles of TA were also found to be affected, showing a decrease from approximately 50% to 25% from 1 : 2 to 1 : 5 ratios, respectively.

  17. Formation of Porous Anodic Oxide Film on Titanium in Phosphoric Acid Electrolyte

    Liu, Z.; Thompson, G. E.

    2015-01-01

    A sequential breakdown anodizing conditions on cp-Ti in phosphoric acid has been investigated in the present study. Anodic oxide films were formed at 100, 150, and 200 V, examined by scanning electron microscopy, Raman spectroscopy, glow discharge optical emission spectrometry, and electrochemical impedance spectroscopy. A porous oxide texture was formed at each voltage. The thickness of anodic porous oxide increased with the increase of anodic voltage. Nano-particulates were formed around and within the pores, and the size of pores increased with increased voltage due to the expansion of particulates. The amorphous-to-crystalline transition was initiated during the film growth. The degree of crystallinity in the anodic oxide film fabricated at 200 V is more abundant than 150 and 100 V. Increased content of the phosphorus species was incorporated into the porous film with the increase of anodic voltage, stabilizing for the nanocrystals developed within the oxide.

  18. The response of quartz crystals coated with thin fatty acid film to organic gases

    Jin, C N; Kim, K H; Kwon, Y S

    1999-01-01

    We tried to apply a quartz crystal as a sensor by using the resonant frequency and the resistance properties of quartz crystals. Four kinds of fatty acids that have the same head groups were coated on the surfaces of the quartz crystals, and the shift of the resonant frequency and the resistance were observed based on the lengths of the tail groups. Myristic acid (C sub 1 sub 4), palmitic acid (C sub 1 sub 6), stearic acid (C sub 1 sub 8), and arachidic acid (C sub 2 sub 0) were deposited on the surfaces of quartz crystals by using the Langmuir-Blodgett (LB) method. As a result, the resonant frequency change was more sensitive to high molecular-weight fatty acids than to low molecular-weight ones. We also observed the effect of temperature on stearic acid LB films, and the response properties of quartz crystals coated with stearic-acid LB films to organic gases were investigated. As a result, the sensitivity of quartz crystals to organic gases was higher for higher molecular-weight gas, and we found that quar...

  19. Investigation of chemical bath deposition of CdO thin films using three different complexing agents

    Khallaf, Hani [Department of Physics, University of Central Florida, Orlando, FL 32816 (United States); Chen, Chia-Ta; Chang, Liann-Be [Graduate Institute of Electro-Optical Engineering, Chang Gung University, Kweishan, Taoyuan 333, Taiwan (China); Green Technology Research Center, Chang Gung University, Kweishan, Taoyuan 333, Taiwan (China); Lupan, Oleg [Department of Physics, University of Central Florida, Orlando, FL 32816 (United States); Department of Microelectronics and Semiconductor Devices, Technical University of Moldova, 168 Stefan cel Mare Boulevard, MD-2004 Chisinau, Republic of Moldova (Moldova, Republic of); Dutta, Aniruddha; Heinrich, Helge [Department of Physics, University of Central Florida, Orlando, FL 32816 (United States); Advanced Materials Processing and Analysis Centre, Department of Mechanical, Materials, and Aerospace Engineering, University of Central Florida, Orlando, FL 32816 (United States); Shenouda, A. [Central Metallurgical R and D Institute (CMRDI), Tebbin, P.O. Box 87, Helwan (Egypt); Chow, Lee, E-mail: Lee.Chow@ucf.edu [Department of Physics, University of Central Florida, Orlando, FL 32816 (United States); Advanced Materials Processing and Analysis Centre, Department of Mechanical, Materials, and Aerospace Engineering, University of Central Florida, Orlando, FL 32816 (United States)

    2011-09-01

    Chemical bath deposition of CdO thin films using three different complexing agents, namely ammonia, ethanolamine, and methylamine is investigated. CdSO{sub 4} is used as Cd precursor, while H{sub 2}O{sub 2} is used as an oxidation agent. As-grown films are mainly cubic CdO{sub 2}, with some Cd(OH){sub 2} as well as CdO phases being detected. Annealing at 400 deg. C in air for 1 h transforms films into cubic CdO. The calculated optical band gap of as-grown films is in the range of 3.37-4.64 eV. Annealed films have a band gap of about 2.53 eV. Rutherford backscattering spectroscopy of as-grown films reveals cadmium to oxygen ratio of 1.00:1.74 {+-} 0.01 while much better stoichiometry is obtained after annealing, in accordance with the X-ray diffraction results. A carrier density as high as 1.89 x 10{sup 20} cm{sup -3} and a resistivity as low as 1.04 x 10{sup -2} {Omega}-cm are obtained.

  20. Complex coacervation for the development of composite edible films based on LM pectin and sodium caseinate.

    Eghbal, Noushin; Yarmand, Mohammad Saeid; Mousavi, Mohammad; Degraeve, Pascal; Oulahal, Nadia; Gharsallaoui, Adem

    2016-10-20

    Coacervation between sodium caseinate (CAS) and low methoxyl pectin (LMP) at pH 3 was investigated as a function of protein/polysaccharide ratio. The highest amount of complex coacervates was formed at a CAS/LMP ratio of 2 at which the ζ-potential value was zero and the turbidity reached its highest value. Then, the properties of films based on these complex coacervates were studied. Coacervation resulted in decreasing water content and water sorption of films as the protein concentration increased. The mechanical properties of films were highly influenced by the formation of electrostatic complexes. The highest values of Young's modulus (182.97± 6.48MPa) and tensile strength (15.64±1.74MPa) with a slight increase of elongation at break (9.35±0.10%) were obtained for films prepared at a CAS/LMP ratio equal to 0.05. These findings show that interactions between LMP and CAS can be used to develop innovative packaging containing active molecules. PMID:27474643

  1. Indium tin oxide thin films elaborated by sol-gel routes: The effect of oxalic acid addition on optoelectronic properties

    Single layer indium tin oxide (ITO) thin films were deposited on glass using modified sol-gel formulations. The coating sols were prepared using indium (InCl3∙ 4H2O) and tin salts (SnCl4∙ 5H2O). The stable sols were obtained using ethanol (C2H5OH) and acetylacetone (C5H8O2) as solvents and by the addition of oxalic acid dihydrate (C2H2O4∙ 2H2O) in different amounts. The effect of oxalic acid content in the sol formulation and post-coating calcination treatment (in air at 300–600 °C) on electrical/optical properties of ITO films have been reported. It was shown that film formation efficiency, surface coverage and homogeneity were all enhanced with oxalic acid addition. Oxalic acid modification also leads to a significant improvement in electrical conductivity without affecting the film thickness (45 ± 3 nm). ITO films exhibiting high transparency (≈ 93%, visible region) with a sheet resistance as low as 3.8 ± 0.4 kΩ/sqr have been formed by employing coating sols with optimized oxalic acid amount. The mechanisms and factors affecting the functional performance of oxalic acid-modified films have been thoroughly discussed and related to the microstructural and chemical characteristic of the films achieved by oxalic acid addition. - Highlights: • A solution-based method for processing indium tin oxide (ITO) thin film is reported. • Oxalic acid (OAD) modification leads to a highly compacted film microstructure. • Bulk resistivity of a single layer OAD-modified ITO film was determined as 0.02 Ωcm. • Thin films with transparency values higher than 90% were produced

  2. Cadmium sulfate complexing with thiourea during preparation of cadmium sulfide films

    Composition of complexes deposited from cadmium sulfate and thiourea(TU) aqueous solution is studied. Its influence on cadmium sulfide film deposition during solution spraying is ascertained. It is shown that with increase of TU concentration in aqueous solution gradual substitution of TU molecules for the first sphere SO42- ions takes place. As a result CdS deposition from these solutions is initiated when the ratio of CdSO4:TU concentrations is 1:2 and for prepartation of uniform films a five-fold TU excess as a minimum is necessary

  3. Research Update: New possibilities for the nanoscale engineering of complex oxide thin films

    McMitchell, S. R. C.

    2015-06-01

    Complex oxides are becoming engrained into modern technology. Understanding the growth and properties of these materials is extremely important for development of novel devices and optimization of existing technologies. Control of the growth of thin film oxides is essential to facilitate the fine-tuning of properties needed for device optimization. In this article, some recent advances in nanoscale engineering of functional oxides are summarized. Control of film structure through manipulation of growth kinetics and substrate considerations is discussed. The construction of composites and artificial materials is also considered. Furthermore, a future outlook is investigated including a route to industrial scale application.

  4. Suberin fatty acids isolated from outer birch bark improve moisture barrier properties of cellulose ether films intended for tablet coatings.

    Heinämäki, Jyrki; Halenius, Anna; Paavo, Maaja; Alakurtti, Sami; Pitkänen, Pauliina; Pirttimaa, Minni; Paaver, Urve; Kirsimäe, Kalle; Kogermann, Karin; Yliruusi, Jouko

    2015-07-15

    We showed that the addition of suberin fatty acids (SFAs) even at small concentrations significantly improves the water vapor barrier properties of hydroxypropyl methylcellulose (HPMC) films. SFAs were isolated from the outer birch bark using extractive hydrolysis. The effects of SFAs on the film formation of aqueous HPMC were investigated with free films plasticized with polyethylene glycol (PEG 400). Special attention was paid on the physical solid-state, moisture barrier and mechanical stress-strain properties of films intended for tablet film coatings. Topography and surface morphology, glass transition temperature (Tg), tensile strength, Young's modulus, and water vapor permeation (WVP) of films were studied. The addition of SFAs lowered the Tg of films suggesting partial enhancement in film plasticization. The WVP of films decreased with increasing SFAs concentration up to 15% (calculated as a % w/w from a polymer weight). The WVP value for a non-suberized reference film and suberized film plasticized with PEG 400 was 2.13×10(-6) and 0.69[×10(-6) g/(mm(2)×h)×mm/Pa], respectively. The addition of SFAs impaired the mechanical stress-strain properties of HPMC films by reducing the deformation capacity of film. In conclusion, the film properties and performance of aqueous HPMC can be modified by including SFAs in the films. PMID:25936623

  5. Quartz crystal microbalance and spectroscopy measurements for acid doping in polyaniline films

    Mohamad M Ayad and Eman A Zaki

    2008-01-01

    Full Text Available We investigated the doping of thin polyaniline (PANI films, prepared by the chemical oxidation of aniline, with different acids. The initial step in the investigation is the preparation of PANI films from aqueous hydrochloric acid solution. This is followed by dedoping with ammonia to obtain a PANI base, which is subsequently doped with strong acids (e.g. hydrochloric, sulfuric, phosphoric and trichloroacetic acids and with a weak acid (acetic acid. The dopant weight fraction (w, which is connected with the gain of mass during the doping of PANI, was determined in situ using a quartz crystal microbalance (QCM. The behavior of PANI upon doping with different anions derived from strong acids indicates that both proton and the anion uptake into the polymer chains occur sharply, rapidly, completely, and reversibly. However the uptake in the case in acetic acid is characterized by slow diffusion. The doping was studied at different concentrations of acetic acid. A second cycle of dedoping–redoping was also performed. The kinetics of the doping reaction is dominated by Fickian diffusion kinetics. The diffusion coefficients (D of the dopant ions into the PANI chains were determined using the QCM and by UV–Vis absorption spectroscopy in the range of (0.076–1.64× 10−15 cm2 s−1. It was found that D in the second cycle of doping is larger than that evaluated from the first cycle of doping for high concentrations of acetic acid. D for the diffusion and for the dopant ion expulsion from the PANI chains was also determined during the redoping process. It was found that D for acetic acid ions in the doping process is larger than that calculated for the dedoping process.

  6. Synthesis, Characterization of α-Oxopentanedioic Acid-Isonicotinoyl Hydrazone Rare Earth-Complexes and Relaxivity of Gd-complex

    杨正银; 杨汝栋

    2004-01-01

    α-Oxopentanedioic acid isonicotinoyl hydrazone (H2L) and its five rare earth complexes were synthesized with a view to further investigating MRI activities of the polycarboxylic Schiff base complexes. The complexes were characterized on the basis of elemental analyses, IR, UV, 1H NMR spectra and thermal analyses. The general formula of the complexes is [Ln(HL)(H2O)2]Cl2·H2O (where Ln(Ⅲ)=La, Pr, Nd, Eu and Gd). In addition, the relaxivity (R1) of the Gd-complex was determined by INVREC Au program.

  7. Study of Complexes of Lanthanum with Amino Acids by Titration Calorimeter

    2000-01-01

    The stability constants and thermodynamic functions for complexes of lanthanum with eight kind of amino acids according to 1:1 and 1:2 in proportion have been determined by titration calorimeter at 298. 15 K. The enthalpy change makes a predominant contribution to the stability of these complexes. The ring in amino acid associated with lanthanum ion helps to enhance the stability of complexes. Steric effectsbetween rings in complexes leads to that the equilibrium constants of reaction of the complexes (1:2) ismuch less than that of the complexes (l:1).

  8. Preliminary characterization of dexamethasone-loaded cross-linked hyaluronic acid films for topical ocular therapy.

    Calles, J A; López-García, A; Vallés, E M; Palma, S D; Diebold, Y

    2016-07-25

    The aim of this work was to design and characterize cross-linked hyaluronic acid (HA)-itaconic acid (IT) films loaded with dexamethasone sodium phosphate salt (DEX) for topical therapy of inflammatory ocular surface diseases. Films were chemically cross-linked with polyethylene glycol diglycidyl ether (PEGDE), then physical and mechanical characterization by stress-strain, X-ray diffraction, X-ray fluorescence spectrometry and swelling assays was conducted. A sequential in vitro therapeutic efficacy model was designed to assess changes in interleukin (IL)-6 production in an inflamed human corneal epithelial (HCE) cell line after film exposure. Changes in cell proliferation after film exposure were assessed using the alamarBlue(®) proliferation assay. Experimental findings showed desirable mechanical properties and in vitro efficacy to reduce cell inflammation. A moderately decreased proliferation rate was induced in HCE cells by DEX-loaded films, compared to commercial DEX eye drops. These results suggest that DEX and HA have opposite effects. The sequential in vitro therapeutic efficacy model arises as an efficient tool to study drug release from delivery systems by indirect measurement of a biological response. PMID:27242313

  9. Peptide Nucleic Acids Complexes of Two Peptide Nucleic Acid Strands and One

    1999-01-01

    Peptide nucleic acids and analogues of peptide nucleic acids are used to form duplex, triplex, and other structures with nucleic acids and to modify nucleic acids. The peptide nucleic acids and analogues thereof also are used to modulate protein activity through, for example, transcription arrest...

  10. Investigation of lanthanum and lutetium complexing with 5-sulfosalicylic acid by the NMR method

    The study of the lanthanum-5-sulfosalicylic acid and lutetium-5-sulfosalicylic acid systems is carried out using the method of NMR spectroscopy. Participation of ionized phenol hydroxyl and carboxylic group of 5-sulfosalicylic acid in complexing with lanthanum and lutetium is shown. pH value at which phenol proton splitting out occurs is found and the constant of acid dissociation of phenol hydroxyl in the complex, pK of which has the value 6.82+-0.04, is calculated dissociation of phenol hydroxyl in the complex, pK of which has the value 6.82+-0.04, is calculated dissociation of phen

  11. Spectrophotometric study into complexing of vanadium(3) with salicylic acid derivatives

    Complexing of vanadium (3) with 5 amino-salicylic acid and amide of salicylhydroxamic acid has been studied. It has been shown that in acidic medium V3+ forms yellow complexes of the composition 1:1 with instability constants 2.2x10-19, 7.8x10-11, and 2.2x10-12, respectively. Complexes of V3+ with derivatives of salicylic acid can be used for determining V(3) content in the presence of V(4)

  12. Syntheses and characterizations of three acid-base supramolecular complexes

    Three acid-base compounds with supramolecular architectures, namely, (1,2-H2bdc)(dmt) (1), (trans-1,4-H2ccdc)0.5(phdat) (2) and (1,3-H2bdc)(phdat) (3) (1,2-H2bdc = 1,2-benzenedicarboxylic acid, trans-1, 4-H2ccdc = trans-1, 4-cyclohexanedicarboxylic acid, 1,3-H2bdc = 1,3-benzenedicarboxylic acid, dmt = 2,4-diamino-6-methyl-s-triazine, phdat = 2,4-diamino-6-phenyl-s-triazine) have been synthesized and characterized by IR spectra, elemental analyses, single-crystal X-ray diffractions and TGA. (author)

  13. Study on complex formation of cadmium (II) ions, 9. Formation constants on cadmium (II) complexes with dicarboxylic acids

    Matsui, Haruo (Government Industrial Research Inst., Nagoya (Japan))

    1984-03-01

    Formation constants of cadmium (11) complexes with dicarboxylic acids such as oxalic, malonic, methylmalonic, succinic, and glutaric acids were determined in aqueous solutions containing 3 mol.dm/sup -3/ LiClO/sub 4/ as a constant ionic medium at 25/sup 0/C by potentiometric titrations. It was reported in the previous works that cadmium (11)- aspartic acid complexes contained two chelate rings. However, a problem remained whether the second chelate ring could be formed by six membered-ring containing -O-Cd-N- bond or by seven membered-ring containing -O-Cd-O- bond. The results of the present work suggested that it would be formed by a six membered ring. Cadmium (11) ions were coordinated with a carboxylic group of the dicarboxylic acids studied, and formed no chelate ring within the complexes. The white precipitate appeared in the solution containing cadmium (11) ion and oxalic acid, in the pH range below 3.0, therefore, the chelate formation was not ascertained in this case. The formation constants, log ..beta..sub(pr)= log((Cdsub(p)Lsub(r)sup((2p-2r)+))/((Cd/sup 2 +/)sup(p)(L/sup 2 -/)sup(r))), of the complexes were: log ..beta../sub 11/ = 1.98, log ..beta../sub 12/ = 3.05 for cadmium (11)-malonic acid; log ..beta../sub 11/ = 2.28, log ..beta../sub 12/ = 3.06 for cadmium (11)-methylmalonic acid; log ..beta../sub 11/ = 1.78, log ..beta../sub 12/ = 3.08 for cadmium (11)-succinic acid; log ..beta../sub 11/ = 1.85, log ..beta../sub 12/ = 3.28 for cadmium (11)-glutaric acid complexes.

  14. Chemical sporulation and germination: cytoprotective nanocoating of individual mammalian cells with a degradable tannic acid-FeIII complex

    Lee, Juno; Cho, Hyeoncheol; Choi, Jinsu; Kim, Doyeon; Hong, Daewha; Park, Ji Hun; Yang, Sung Ho; Choi, Insung S.

    2015-11-01

    Individual mammalian cells were coated with cytoprotective and degradable films by cytocompatible processes maintaining the cell viability. Three types of mammalian cells (HeLa, NIH 3T3, and Jurkat cells) were coated with a metal-organic complex of tannic acid (TA) and ferric ion, and the TA-FeIII nanocoat effectively protected the coated mammalian cells against UV-C irradiation and a toxic compound. More importantly, the cell proliferation was controlled by programmed formation and degradation of the TA-FeIII nanocoat, mimicking the sporulation and germination processes found in nature.Individual mammalian cells were coated with cytoprotective and degradable films by cytocompatible processes maintaining the cell viability. Three types of mammalian cells (HeLa, NIH 3T3, and Jurkat cells) were coated with a metal-organic complex of tannic acid (TA) and ferric ion, and the TA-FeIII nanocoat effectively protected the coated mammalian cells against UV-C irradiation and a toxic compound. More importantly, the cell proliferation was controlled by programmed formation and degradation of the TA-FeIII nanocoat, mimicking the sporulation and germination processes found in nature. Electronic supplementary information (ESI) available: Experimental details, LSCM images, and SEM and TEM images. See DOI: 10.1039/c5nr05573c

  15. Photoactive layer-by-layer films of cellulose phosphate and titanium dioxide containing phosphotungstic acid

    Ullah, Sajjad; Acuña, José Javier Sáez; Pasa, André Avelino; Bilmes, Sara A.; Vela, Maria Elena; Benitez, Guillermo; Rodrigues-Filho, Ubirajara Pereira

    2013-07-01

    A versatile layer-by-layer (LbL) procedure for the preparation of highly dispersed, adherent and porous multilayer films of TiO2 nanoparticles (NPs) and phosphotungstic acid (HPW) on a variety of substrates at room temperature was developed based on the use of cellulose phosphate (CP) as an efficient and non-conventional polyelectrolyte. UV/vis absorption spectroscopy confirmed the linear and regular growth of the films with the number of immersion cycles and a strong adsorption ability of CP towards TiO2 NPs. FTIR spectroscopy showed that HPW binds to the surface of TiO2 through the oxygen atom at the corner of the Keggin structure. XPS results showed that the interaction between TiO2 and CP is through Ti-O-P linkage. A model is proposed for the TiO2-HPW interaction based on XPS and FTIR results. FEG/SEM study of the surface morphology revealed a porous film structure with a homogenous distribution of the TiO2 NPs induced by CP. HRTEM studies showed that the resulting composite films consist of crystalline anatase and rutile phases and poly-nano-crystalline HPW with a semi-crystalline TiO2-HPW interface. These CP/TiO2 and CP/TiO2/HPW LbL films showed good photoactivity against both saturated and unsaturated species, for instance, stearic acid (SA), crystal violet (CV) and methylene blue (MB) under UV irradiation. The CP/HPW films formed on bacterial cellulose (BC) showed good photochromic response which is enhanced in presence of TiO2 due to an interfacial electron transfer from TiO2 to HPW. This simple and environmentally safe method can be used to form coatings on a variety of surfaces with photoactive TiO2 and TiO2/HPW films.

  16. Photoactive layer-by-layer films of cellulose phosphate and titanium dioxide containing phosphotungstic acid

    A versatile layer-by-layer (LbL) procedure for the preparation of highly dispersed, adherent and porous multilayer films of TiO2 nanoparticles (NPs) and phosphotungstic acid (HPW) on a variety of substrates at room temperature was developed based on the use of cellulose phosphate (CP) as an efficient and non-conventional polyelectrolyte. UV/vis absorption spectroscopy confirmed the linear and regular growth of the films with the number of immersion cycles and a strong adsorption ability of CP towards TiO2 NPs. FTIR spectroscopy showed that HPW binds to the surface of TiO2 through the oxygen atom at the corner of the Keggin structure. XPS results showed that the interaction between TiO2 and CP is through Ti–O–P linkage. A model is proposed for the TiO2–HPW interaction based on XPS and FTIR results. FEG/SEM study of the surface morphology revealed a porous film structure with a homogenous distribution of the TiO2 NPs induced by CP. HRTEM studies showed that the resulting composite films consist of crystalline anatase and rutile phases and poly-nano-crystalline HPW with a semi-crystalline TiO2–HPW interface. These CP/TiO2 and CP/TiO2/HPW LbL films showed good photoactivity against both saturated and unsaturated species, for instance, stearic acid (SA), crystal violet (CV) and methylene blue (MB) under UV irradiation. The CP/HPW films formed on bacterial cellulose (BC) showed good photochromic response which is enhanced in presence of TiO2 due to an interfacial electron transfer from TiO2 to HPW. This simple and environmentally safe method can be used to form coatings on a variety of surfaces with photoactive TiO2 and TiO2/HPW films.

  17. Fluorescence of complexes of Eu( Ⅱ ) with aromatic carboxylic acid-1, 1O-phenanthroline

    2001-01-01

    The 1, 10-phenanthroline-aromatic carboxylic acid (benzoic acid and o-phthalic acid) binary and ternary complexes of europium were synthesized. The fluorescence and FT-IR spectroscopy, elemental analysis, UV spectroscopic studies on these complexes were also performed. These complexes can emit strong red fluorescence of Eu( m ) excited by UV light. At the same excited wavelength, the fluorescence spectra of the complexes were also studied. The results indi cated that the fluorescence intensities of ternary complexes are stronger than that of binary complexes. The reason is that phenanthroline has higher electron density and higher orbit scope in the conjugated system and consequently an easier ener gy transfer to the europium ion, which makes the fluorescence intensity of ternary complexes be stronger than that of bi nary complexes.

  18. Influence of heterogeneity of binding sites of humic acid on its complexation with actinyl ions

    The influence of heterogeneity of binding sites of humic acid was investigated using three different experimental approaches. 1) Complexation with UO22+ was studied by fluorescence spectroscopy. Considering the quenching phenomena, the apparent stability constants of complexation of humic acid with UO22+ were evaluated and compared with the values reported in the literature. 2) Complexation kinetics of NpO2+ with humic acid and fulvic acid was investigated by kinetic spectra. The complexation kinetics was found to be controlled by the heterogeneity of binding sites. 3) The migration of humic acid-NpO2+ complexes was discussed experimentally by column experiments and analytically by a migration model. The concentration profile of NpO2+ in the column was qualitatively simulated. (author)

  19. Influence of Oxide Film to Stress Corrosion Cracking of Zirconium in Boiling Nitric Acid Solution

    Nuclear fuel reprocessing process acts an important role of nuclear energy cycle. In Japan, a commercial reprocessing plant has been operating at the Rokkasho reprocessing plant. Purex process that is used nitric acid and dodecane with tributyl phosphate for solvent has been adopted in the plant. Boiling nitric acid is applied to dissolve oxide spent nuclear fuel. In the boiling nitric acid solution, plant material corrodes severely and intergranular corrosion is observed in stainless steels. In order to avoid corrosion in such severe environment, some equipment in the plants has been made of zirconium, which has excellent corrosion resistance in nitric acid solutions. However, it has been known that zirconium has stress corrosion cracking (SCC) susceptibility in concentrated HNO3 with nobler corrosion potential. Nobler corrosion potential causes breakdowns of passive film having excellent protective performance and raises SCC susceptibility of zirconium in nitric acid solutions. Therefore, it is important to clarify the relationship among potential, growth and the breakdown of oxide film for the SCC initiation mechanism. In this study, we investigated the oxide film growth of zirconium with various potentials in boiling nitric acid solutions. Electrochemical tests and immersion tests with various applied potentials conducted in boiling 3. 6 and 9 mol.dm-3 HNO3. The potentials in the immersion tests were set at 1.3, 1.4 and 1.5 V vs. sat. KCl-Ag/AgCl electrode (SSE). These were in the region of trans-passive state of zirconium in boiling nitric acid solution. The test durations were 10, 100 and 500 h. After the corrosion tests, cross-sectional observations of oxide films were conducted. From the results of anodic polarization curves of zirconium in boiling nitric acid, passivity region was observed through rest potential to about 1.5 V in boiling 6 mol.dm-3 HNO3. Rapid increase of current density was observed at the potential attributed to transition from passivity

  20. Characterization of biodegradable film based on zein and oleic acid added with nanocarbonate

    Wanessa Ximenes Ribeiro

    2015-10-01

    Full Text Available Zein oleic acid films added with 1, 2 and 3 % (w/w of nanocarbonate and 30 % glycerol as plasticizer, were produced and evaluated according to their structure and functional properties. Structural characteristics were analyzed by optical and scanning electron microscopy (SEM. Water solubility and mechanical properties were determined according to ASTM methods. The increase of nanocarbonate concentration increased water solubility and influenced the color and mechanical properties. Optical and SEM of film samples added with nanocarbonate, shown low amount of pores and great fat globules size.

  1. Electrochemical and electrochromic response of poly(thiophene-3-acetic acid) films

    Giglioti, M.; Trivinho-Strixino, F.; Matsushima, J.T.; Bulhoes, L.O.S.; Pereira, E.C. [Laboratorio Interdisciplinar de Eletroquimica e Ceramica, Departamento de Quimica, Universidade Federal de Sao Carlos, Caixa Postal 676, Sao Carlos SP 13565-905 (Brazil)

    2004-05-15

    Thiophene-3-acetic acid has been polymerized in chloroform by a chemical method using FeCl{sub 3} as oxidant. The films were prepared casting the solubilized polymer on ITO electrodes and studied using cyclic voltammetry, chronoamperometry and spectroelectrochemistry. During the potential sweep, an electrochromic process is observed in which the film color changes from red to black. High electrochromic efficiency was observed for more than 600 cycles, although it decreases to 73% of the initial value. Until 264 cycles, the electrochromic efficiency at 750nm is stable and the value is 242cm{sup 2}C{sup -1}.

  2. Photoluminescence emission of nanoporous anodic aluminum oxide films prepared in phosphoric acid

    Nourmohammadi, Abolghasem; Asadabadi, Saeid Jalali; Yousefi, Mohammad Hasan; Ghasemzadeh, Majid

    2012-12-01

    The photoluminescence emission of nanoporous anodic aluminum oxide films formed in phosphoric acid is studied in order to explore their defect-based subband electronic structure. Different excitation wavelengths are used to identify most of the details of the subband states. The films are produced under different anodizing conditions to optimize their emission in the visible range. Scanning electron microscopy investigations confirm pore formation in the produced layers. Gaussian analysis of the emission data indicates that subband states change with anodizing parameters, and various point defects can be formed both in the bulk and on the surface of these nanoporous layers during anodizing.

  3. Development and characterization of sugar palm starch and poly(lactic acid) bilayer films.

    Sanyang, M L; Sapuan, S M; Jawaid, M; Ishak, M R; Sahari, J

    2016-08-01

    The development and characterization of environmentally friendly bilayer films from sugar palm starch (SPS) and poly(lactic acid) (PLA) were conducted in this study. The SPS-PLA bilayer films and their individual components were characterized for their physical, mechanical, thermal and water barrier properties. Addition of 50% PLA layer onto 50% SPS layer (SPS50-PLA50) increased the tensile strength of neat SPS film from 7.74 to 13.65MPa but reduced their elongation at break from 46.66 to 15.53%. The incorporation of PLA layer significantly reduced the water vapor permeability as well as the water uptake and solubility of bilayer films which was attributed to the hydrophobic characteristic of the PLA layer. Furthermore, scanning electron microscopy (SEM) image of SPS50-PLA50 revealed lack of strong interfacial adhesion between the SPS and PLA. Overall, the incorporation of PLA layer onto SPS films enhances the suitability of SPS based films for food packaging. PMID:27112848

  4. Sorption of small quantities of silver on silicic acid under the conditions of complex formation

    Present article is devoted to sorption of small quantities of silver on silicic acid under the conditions of complex formation. Study of precipitation of small quantities of silver (4.2·10-5mg/l) from the solutions of oxalic, tartaric and citric acids depending on ph showed that under these conditions the precipitation does not occur. This is due to formation of stable and soluble in the water silver complex compounds with oxalic, tartaric and citric acids.

  5. Grain growth and complex stress evolution during Volmer–Weber growth of polycrystalline thin films

    Volmer–Weber growth of polycrystalline thin films involves poorly understood kinetic processes that occur far from equilibrium and lead to complex co-evolution of the surface, microstructure and intrinsic stress of the films. Here we present a comprehensive study consisting of in situ stress measurements, microstructure characterization and analytical modeling for various metallic films that grow by the Volmer–Weber mechanism. We find that, under conditions of intermediate atomic mobility, stress evolution after coalescence involves a turnaround from a compressive to a tensile stress state. The thickness at which the stress turnaround is observed increases as the substrate temperature increases or the deposition rate decreases. We show that this phenomenon is associated with two competing mechanisms: grain growth during deposition (at homologous temperatures as low as 0.17) and adatom attachment to surface sites at grain boundaries. Grain growth during film deposition not only causes a tensile component of the intrinsic stress, but also leads to changes in the magnitude of the compressive stresses, from being independent of, to scaling with, the inverse of the grain size. Analyses of these phenomena lead to insights into stress evolution under conditions of low and high atomic mobility, as well as intermediate mobility, and are general for stress evolution during Volmer–Weber growth of polycrystalline films

  6. Biodegradable polyester films from renewable aleuritic acid: surface modifications induced by melt-polycondensation in air

    Jesús Benítez, José; Alejandro Heredia-Guerrero, José; Inmaculada de Vargas-Parody, María; Cruz-Carrillo, Miguel Antonio; Morales-Flórez, Victor; de la Rosa-Fox, Nicolás; Heredia, Antonio

    2016-05-01

    Good water barrier properties and biocompatibility of long-chain biopolyesters like cutin and suberin have inspired the design of synthetic mimetic materials. Most of these biopolymers are made from esterified mid-chain functionalized ω-long chain hydroxyacids. Aleuritic (9,10,16-trihydroxypalmitic) acid is such a polyhydroxylated fatty acid and is also the major constituent of natural lac resin, a relatively abundant and renewable resource. Insoluble and thermostable films have been prepared from aleuritic acid by melt-condensation polymerization in air without catalysts, an easy and attractive procedure for large scale production. Intended to be used as a protective coating, the barrier's performance is expected to be conditioned by physical and chemical modifications induced by oxygen on the air-exposed side. Hence, the chemical composition, texture, mechanical behavior, hydrophobicity, chemical resistance and biodegradation of the film surface have been studied by attenuated total reflection–Fourier transform infrared spectroscopy (ATR–FTIR), atomic force microscopy (AFM), nanoindentation and water contact angle (WCA). It has been demonstrated that the occurrence of side oxidation reactions conditions the surface physical and chemical properties of these polyhydroxyester films. Additionally, the addition of palmitic acid to reduce the presence of hydrophilic free hydroxyl groups was found to have a strong influence on these parameters.

  7. Biocatalyzed approach for the surface functionalization of poly(L-lactic acid) films using hydrolytic enzymes.

    Pellis, Alessandro; Acero, Enrique Herrero; Weber, Hansjoerg; Obersriebnig, Michael; Breinbauer, Rolf; Srebotnik, Ewald; Guebitz, Georg M

    2015-09-01

    Poly(lactic acid) as a biodegradable thermoplastic polyester has received increasing attention. This renewable polyester has found applications in a wide range of products such as food packaging, textiles and biomedical devices. Its major drawbacks are poor toughness, slow degradation rate and lack of reactive side-chain groups. An enzymatic process for the grafting of carboxylic acids onto the surface of poly(L-lactic acid) (PLLA) films was developed using Candida antarctica lipase B as a catalyst. Enzymatic hydrolysis of the PLLA film using Humicola insolens cutinase in order to increase the number of hydroxyl and carboxylic groups on the outer polymer chains for grafting was also assessed and showed a change of water contact angle from 74.6 to 33.1° while the roughness and waviness were an order of magnitude higher in comparison to the blank. Surface functionalization was demonstrated using two different techniques, (14) C-radiochemical analysis and X-ray photoelectron spectroscopy (XPS) using (14) C-butyric acid sodium salt and 4,4,4-trifluorobutyric acid as model molecules, respectively. XPS analysis showed that 4,4,4-trifluorobutyric acid was enzymatically coupled based on an increase of the fluor content from 0.19 to 0.40%. The presented (14) C-radiochemical analyses are consistent with the XPS data indicating the potential of enzymatic functionalization in different reaction conditions. PMID:25963883

  8. Sub-monolayer film growth of a volatile lanthanide complex on metallic surfaces

    Hironari Isshiki

    2015-12-01

    Full Text Available We deposited a volatile lanthanide complex, tris(2,2,6,6-tetramethyl-3,5-heptanedionatoterbium(III, onto metal surfaces of Cu(111, Ag(111 and Au(111 in vacuum and observed well-ordered sub-monolayer films with low temperature (5 K scanning tunneling microscopy. The films show a distorted three-fold symmetry with a commensurate structure. Scanning tunneling spectroscopy reveals molecular orbitals delocalized on the ligands of the molecule. Our results imply that this complex can be transferred onto the metal substrates without molecular decomposition or contamination of the surface. This new rare-earth-based class of molecules broadens the choice of molecular magnets to study with scanning tunneling microscopy.

  9. Effects of Acid Vapor, Basic Vapor and Heat Treatments on the Properties of Langmuir-Blodgett Films of Divalent Metal Salts of Fatty Acids

    Saito, Mitsuyoshi; Sugi, Michio; Ikegami, Keiichi; Yoneyama, Mitsuru; Iizima, Sigeru

    1986-06-01

    When LB films are exposed to the atmosphere vaporized from acid at room temperature, the X-ray diffraction peaks attributed to the lamellar structure disappear and new peaks appear depending on the metal ion species of the salt, whereas such noticeable change is not observed by basic vapor treatment and heat treatment. Diffraction patterns for LB films of free fatty acids are not influenced by these three treatments.

  10. Mediated participation: Using filmed narratives in complex multi-stakeholder settings

    Witteveen, L.M.; Enserink, B.; Lie, R

    2009-01-01

    Mediated participation aims to bring `distanced¿ or `overlooked¿ stakeholders in a mediated way to the doorstep of decision makers. It promotes inclusion of their stories, concerns and proposals in decision-making processes because it allows policy and decision makers to `learn¿ in mediated interaction with distant stakeholders. Visual Problem Appraisal (VPA) is a film-based methodology for analysis and social learning, which is produced and used in settings of complex problems and sustainabl...

  11. Chemical deposition in CdSe thin films using cadmium trithanolamine complex

    Eid, A.H.; Mahmoud, S. (National Research centre, Dokki, Cairo (EG). Dept. of Electron Microscopy and Thin Films)

    1992-07-01

    Thin layers of metal chalcogenides are important for photovoltaic cells, photoconductors and other electro-optical devices. These materials can be obtained in thin-layer form by sputtering, spray pyrolysis, vacuum deposition and sintering. Chemical deposition is the simplest way of obtaining thin layers of high quality and good reproducibility. In the recent work the triethanolamine (TEA) complex of Cd{sup 2+} ion was used for CdSe thin-film deposition. (author).

  12. Characterization of the effects of lignin and lignin complex particles as filler on a polystyrene film

    Highlights: ► We have studied the use of Co(II) to form a complex with the lignin. We use first vanillin as the lignin model and we observed a change in color for the produced complex depending on the light wavelength. The use of other transition metals does not give the same observation. ► The use of the transition metal with the lignin precipitated from the black liquor after pulping of agricultural residues, gave a fluorescent color under fluorescent microscope. ► We applied the resulted lignin complex to prepare polymer film that can be used as special polymer packaging which can be color changed under different wavelengths. - Abstract: The work in this research outlines the use of lignin precipitated from lignocellulosic substrate as fillers after modified with transition metal cations, Fe(III), Ni(II) and Co(II), in the production of a polystyrene based composite for polymer packaging applications. Virgin polystyrene was compared with lignin and lignin complex filled composites with loading of 5% by weight prepared using twin screw extrusion. The lignin complexes were first characterized by the UV spectra to identify the new absorption bands occurred due to the complex formation. Moreover, lignin model, namely vanillin, was used to notify the geometric structure of the resulting complexes applying the GC mass spectra. Scanning electron microscopy was used to indicate the change in the morphological structure of the filler particles. On the other hand, the mechanical and thermal analysis for the resulting polymer composites was studied and it was noticed that the type of lignin or lignin complex plays a roll in the results. The inclusion of the Co(II)–lignin complex was observed to increase the tensile strength of the resulting polymer composite and a decrease of the glass transition temperature. Furthermore, light wave lengths and UV fluorescent microscope were used to identify the change of color for the resulting polymer film.

  13. Characterization of the effects of lignin and lignin complex particles as filler on a polystyrene film

    El-Zawawy, Waleed K., E-mail: wkzawawy@yahoo.com [Cellulose and Paper Department, National Research Center, El-Tahrir St., Giza (Egypt); Ibrahim, Maha M. [Cellulose and Paper Department, National Research Center, El-Tahrir St., Giza (Egypt); Belgacem, Mohamed Naceur; Dufresne, Alain [Grenoble Institute of Technology (INP) - The International School of Paper, Print Media and Biomaterials (PAGORA), BP 65, 38402 Saint Martin d' Heres cedex, Grenoble (France)

    2011-12-15

    Highlights: Black-Right-Pointing-Pointer We have studied the use of Co(II) to form a complex with the lignin. We use first vanillin as the lignin model and we observed a change in color for the produced complex depending on the light wavelength. The use of other transition metals does not give the same observation. Black-Right-Pointing-Pointer The use of the transition metal with the lignin precipitated from the black liquor after pulping of agricultural residues, gave a fluorescent color under fluorescent microscope. Black-Right-Pointing-Pointer We applied the resulted lignin complex to prepare polymer film that can be used as special polymer packaging which can be color changed under different wavelengths. - Abstract: The work in this research outlines the use of lignin precipitated from lignocellulosic substrate as fillers after modified with transition metal cations, Fe(III), Ni(II) and Co(II), in the production of a polystyrene based composite for polymer packaging applications. Virgin polystyrene was compared with lignin and lignin complex filled composites with loading of 5% by weight prepared using twin screw extrusion. The lignin complexes were first characterized by the UV spectra to identify the new absorption bands occurred due to the complex formation. Moreover, lignin model, namely vanillin, was used to notify the geometric structure of the resulting complexes applying the GC mass spectra. Scanning electron microscopy was used to indicate the change in the morphological structure of the filler particles. On the other hand, the mechanical and thermal analysis for the resulting polymer composites was studied and it was noticed that the type of lignin or lignin complex plays a roll in the results. The inclusion of the Co(II)-lignin complex was observed to increase the tensile strength of the resulting polymer composite and a decrease of the glass transition temperature. Furthermore, light wave lengths and UV fluorescent microscope were used to identify

  14. Phase transitions via selective elemental vacancy engineering in complex oxide thin films

    Lee, Sang A.; Jeong, Hoidong; Woo, Sungmin; Hwang, Jae-Yeol; Choi, Si-Young; Kim, Sung-Dae; Choi, Minseok; Roh, Seulki; Yu, Hosung; Hwang, Jungseek; Kim, Sung Wng; Choi, Woo Seok

    2016-04-01

    Defect engineering has brought about a unique level of control for Si-based semiconductors, leading to the optimization of various opto-electronic properties and devices. With regard to perovskite transition metal oxides, O vacancies have been a key ingredient in defect engineering, as they play a central role in determining the crystal field and consequent electronic structure, leading to important electronic and magnetic phase transitions. Therefore, experimental approaches toward understanding the role of defects in complex oxides have been largely limited to controlling O vacancies. In this study, we report on the selective formation of different types of elemental vacancies and their individual roles in determining the atomic and electronic structures of perovskite SrTiO3 (STO) homoepitaxial thin films fabricated by pulsed laser epitaxy. Structural and electronic transitions have been achieved via selective control of the Sr and O vacancy concentrations, respectively, indicating a decoupling between the two phase transitions. In particular, O vacancies were responsible for metal-insulator transitions, but did not influence the Sr vacancy induced cubic-to-tetragonal structural transition in epitaxial STO thin film. The independent control of multiple phase transitions in complex oxides by exploiting selective vacancy engineering opens up an unprecedented opportunity toward understanding and customizing complex oxide thin films.

  15. Effect of Fermented Chitin Nano whiskers on Properties of Polylactic Acid Bio composite Films

    The fermented chitin nano whiskers (FCNW) filled polylactic acid (PLA) bio composite films were successfully produced using solution casting method. The bio composite films were characterized in terms of tensile properties. The Young's modulus increased with increasing FCNW content while the tensile strength increased and reached the maximum value at 4 phr FCNW loading. Therefore it can be concluded that the optimum loading of FCNW is at 4 phr and further addition of FCNW may lead to agglomeration resulting in a decrease in tensile strength. The elongation at break of the bio composite films decreased rapidly upon addition of FCNW into PLA. From the Atomic Force Microscopy, the surface morphology of the PLA changed upon addition of FCNW and tendency for agglomeration of FCNW at high loading was observed. (author)

  16. Stability of cadmium complex with octaphenyltetrazaporphin and its solvoprotolytic dissociation in pyridine-acetic acid medium

    Berezin, B.D.; Khelevina, O.G. (Ivanovskij Khimiko-Tekhnologicheskij Inst. (USSR))

    1982-01-01

    Solvoprotolytic dissociation of octaphenyltetrazaporphin cadmium complex in acetic acid solutions in pyridine is investigated. It is stated that its dissociation is obeyed submitted the first order by the complex and the second order by solvated proton. Comparison with cadmium complexes of other porphyrins is carried out.

  17. Preparation and characteristics of chemical bath deposited ZnS thin films: Effects of different complexing agents

    Shin, Seung Wook [Department of Materials Science and Engineering, KAIST, Daejeon 305-701 (Korea, Republic of); Agawane, G.L.; Gang, Myeng Gil [Photonics Technology Research Institute, Department of Materials Science Engineering, Chonnam National University, Gwangju 500-757 (Korea, Republic of); Moholkar, A.V. [Department of Physics, Shivaji University, Kolhapur 416-004 (India); Moon, Jong-Ha [Photonics Technology Research Institute, Department of Materials Science Engineering, Chonnam National University, Gwangju 500-757 (Korea, Republic of); Kim, Jin Hyeok, E-mail: jinhyeok@chonnam.ac.kr [Photonics Technology Research Institute, Department of Materials Science Engineering, Chonnam National University, Gwangju 500-757 (Korea, Republic of); Lee, Jeong Yong, E-mail: j.y.lee@kaist.ac.kr [Department of Materials Science and Engineering, KAIST, Daejeon 305-701 (Korea, Republic of)

    2012-06-15

    Highlights: Black-Right-Pointing-Pointer Thick ZnS thin films were successfully prepared by chemical bath deposition in a basic medium using less toxic complexing agents. Black-Right-Pointing-Pointer Effect of different complexing agents such as no complexing agent, Na{sub 3}-citrate and a mixture of Na{sub 3}-citrate and EDTA on the properties of ZnS thin films was investigated. Black-Right-Pointing-Pointer ZnS thin film deposited using two complexing agent showed the outstanding characteristics as compared to those using no and one complexing agent. - Abstract: Zinc sulfide (ZnS) thin films were prepared on glass substrates by a chemical bath deposition technique using aqueous zinc acetate and thiourea solutions in a basic medium (pH {approx} 10) at 80 Degree-Sign C. The effects of different complexing agents, such as a non-complexing agent, Na{sub 3}-citrate, and a mixture of Na{sub 3}-citrate and ethylenediamine tetra-acetate (EDTA), on the structural, chemical, morphological, optical, and electrical properties of ZnS thin films were investigated. X-ray diffraction pattern showed that the ZnS thin film deposited without any complexing agent was grown on an amorphous phase. However, the ZnS thin films deposited with one or two complexing agents showed a polycrystalline hexagonal structure. No secondary phase (ZnO) was observed. X-ray photoelectron spectroscopy showed that all ZnS thin films exhibited both Zn-S and Zn-OH bindings. Field emission scanning electron microscopy (FE-SEM) images showed that ZnS thin films deposited with complexing agents had thicker thicknesses than that deposited without a complexing agent. The electrical resistivity of ZnS thin films was over 10{sup 5} {Omega} cm regardless of complexing agents. The average transmittance of the ZnS thin films deposited without a complexing agent, those with Na{sub 3}-citrate, and those with a mixture of Na{sub 3}-citrate and EDTA was approximately 85%, 65%, and 70%, respectively, while the band gap

  18. Fabrication of carbon nanotube films from alkyne-transition metal complexes

    Iyer, Vivekanantan S.; Vollhardt, K. Peter C.

    2007-08-28

    A simple method for the production or synthesis of carbon nanotubes as free-standing films or nanotube mats by the thermal decomposition of transition metal complexed alkynes with aryl, alkyl, alkenyl, or alkynyl substituents. In particular, transition metal (e.g. Co, Ni, Fe, Mo) complexes of diarylacetylenes, e.g. diphenylacetylene, and solid mixtures of these complexes with suitable, additional carbon sources are heated in a vessel. More specifically, the heating of the transition metal complex is completed at a temperature between 400-800.degree. C. and more particularly 550-700.degree. C. for between 0.1 to 24 hours and more particularly 0.5-3 hours in a sealed vessel under a partial pressure of argon or helium.

  19. Syntheses,characteristics and fluorescence properties of complexes of terbium with benzoic acid and its derivatives

    ZHOU Zhong-cheng; SHU Wan-gen; RUAN Jian-ming; HUANG Bai-yun; LIU You-nian

    2005-01-01

    The binary complexes of terbium with benzoic acid and its derivatives (phthalic acid,iso-phthalic acid,oaminobenzoic acid,salicylic acid,sulfosalicylic acid) were synthesized and their compositions were identified by elemental analyses.UV,IR of the complexes were investigated.The UV spectra indicate that the complexes'ultraviolet absorption is mainly the ligands' absorption,but the location of peak drifts.The IR spectra show that the IR spectra of complexes are different from those of free ligands,and the band at 400-500 cm-1,due to the stretching vibration of Tb-O,is absent for free ligands.The fluorescence properties were investigated by using luminescence spectroscope,the results show that all the six complexes of terbium exhibit excellent luminescence,due to the transition from the lowest excited state 5D4 to 7F ground state manifold,the complexes of terbium with sulfosalicylic acid have the strongest fluorescence intensity,and is stronger than o-aminobenzoic acid-terbium,whose fluorescence intensity is regarded as the strongest one in the literature,and even stronger than some phosphor of terbium.

  20. Features of photopolymerization of Langmiur-Blodgett thin films of acetylenic acids

    UV-induced polymerization of thin (1-4 monolayers) Langmuir-Blodgett films of acetylenic carboxylic acids with triple bonds in different positions (terminal: 23-tetracosinic acid HC≡C(CH2)21COOH, and internal: 2-docosinic CH3(CH2)18C≡CCOOH) and their lead salts is investigated. It is shown by means of IR spectroscopy that the topochemical reaction proceeds with the participation of carboxylic groups. The differences in the structure of mono- and bilayers are demonstrated. The mechanism of the topochemical reaction depends on the method of film transfer onto the substrate. It is shown by means of UV spectroscopy that short conjugated polyenes (containing 7 to 9 carbon atoms) are formed as the product of polymerization. The mechanism of the formation of these polyene chains is proposed on the basis of the experimental data and semi-empirical calculations.

  1. Features of photopolymerization of Langmiur-Blodgett thin films of acetylenic acids

    Dultsev, F.N., E-mail: fdultsev@thermo.isp.nsc.r [Institute of Semiconductor Physics SB RAS, Novosibisrk, 630090, Lavrentiev Ave., 13 (Russian Federation); Badmaeva, I.A. [Institute of Semiconductor Physics SB RAS, Novosibisrk, 630090, Lavrentiev Ave., 13 (Russian Federation)

    2009-11-02

    UV-induced polymerization of thin (1-4 monolayers) Langmuir-Blodgett films of acetylenic carboxylic acids with triple bonds in different positions (terminal: 23-tetracosinic acid HC{identical_to}C(CH2)21COOH, and internal: 2-docosinic CH3(CH2)18C{identical_to}CCOOH) and their lead salts is investigated. It is shown by means of IR spectroscopy that the topochemical reaction proceeds with the participation of carboxylic groups. The differences in the structure of mono- and bilayers are demonstrated. The mechanism of the topochemical reaction depends on the method of film transfer onto the substrate. It is shown by means of UV spectroscopy that short conjugated polyenes (containing 7 to 9 carbon atoms) are formed as the product of polymerization. The mechanism of the formation of these polyene chains is proposed on the basis of the experimental data and semi-empirical calculations.

  2. Neodymium(3) complexing with bischloromethylphosphinic acid in aqueous solution

    High resolution spectrography is used to study Nd3+ complexing with (ClCH2)2POOH(HL) in aqueous solution. NdL2+ complex (lg Kstab = 0.44±0.04) with the corresponding absorption band with a maximum at λ=4283 A is formed in a system

  3. Design of stereoelectronically promoted super lewis acids and unprecedented chemistry of their complexes.

    Foroutan-Nejad, Cina; Vicha, Jan; Marek, Radek

    2014-09-01

    A new family of stereoelectronically promoted aluminum and scandium super Lewis acids is introduced on the basis of state-of-the-art computations. Structures of these molecules are designed to minimize resonance electron donation to central metal atoms in the Lewis acids. Acidity of these species is evaluated on the basis of their fluoride-ion affinities relative to the antimony pentafluoride reference system. It is demonstrated that introduced changes in the stereochemistry of the designed ligands increase acidity considerably relative to Al and Sc complexes with analogous monodentate ligands. The high stability of fluoride complexes of these species makes them ideal candidates to be used as weakly coordinating anions in combination with highly reactive cations instead of conventional Lewis acid-fluoride complexes. Further, the interaction of all designed molecules with methane is investigated. All studied acids form stable pentavalent-carbon complexes with methane. In addition, interactions of the strongest acid of this family with very weak bases, namely, H2, N2, carbon oxides, and noble gases were investigated; it is demonstrated that this compound can form considerably stable complexes with the aforementioned molecules. To the best of our knowledge, carbonyl and nitrogen complexes of this species are the first hypothetical four-coordinated carbonyl and nitrogen complexes of aluminum. The nature of bonding in these systems is studied in detail by various bonding analysis approaches. PMID:25055748

  4. Starch-based Antimicrobial Films Incorporated with Lauric Acid and Chitosan

    Salleh, E.; Muhamad, I. I.

    2010-03-01

    Antimicrobial (AM) packaging is one of the most promising active packaging systems. Starch-based film is considered an economical material for antimicrobial packaging. This study aimed at the development of food packaging based on wheat starch incorporated with lauric acid and chitosan as antimicrobial agents. The purpose is to restrain or inhibit the growth of spoilage and/or pathogenic microorganisms that are contaminating foods. The antimicrobial effect was tested on B. substilis and E. coli. Inhibition of bacterial growth was examined using two methods, i.e. zone of inhibition test on solid media and liquid culture test (optical density measurements). The control and AM films (incorporated with chitosan and lauric acid) were produced by casting method. From the observations, AM films exhibited inhibitory zones. Interestingly, a wide clear zone on solid media was observed for B. substilis growth inhibition whereas inhibition for E. coli was not as effective as B. substilis. From the liquid culture test, the AM films clearly demonstrated a better inhibition against B. substilis than E. coli.

  5. Investigation of Carboxylic Acid-Neodymium Conversion Films on Magnesium Alloy

    Cui, Xiufang; Liu, Zhe; Lin, Lili; Jin, Guo; Wang, Haidou; Xu, Binshi

    2015-01-01

    The new carboxylic acid-neodymium anhydrous conversion films were successfully prepared and applied on the AZ91D magnesium alloy surface by taking absolute ethyl alcohol as solvent and four kinds of soluble carboxylic acid as activators. The corrosion resistance of the coating was measured by potentiodynamic polarization test in 3.5 wt.% NaCl solution in pH 7.0. The morphology, structure, and constituents of the coating were observed by scanning electron microscope, energy dispersivespectrum, x-ray photoelectron spectrum, and Fourier infrared spectrometer. Results show that corrosion resistance properties of samples coated with four different anhydrous conversion films were improved obviously. The corrosion potential increased, corrosion current density decreased, and polarization resistance increased. Among these four kinds of conversion films the one added with phytic exhibits the best corrosion resistant property. The mechanism of anhydrous-neodymium conversion film formation is also analyzed in this paper. It reveals that the gadolinium conversion coating is mainly composed of stable Nd2O3, MgO, Mg(OH)2, and carboxylate of Nd. And that the sample surface is rich in organic functional groups.

  6. Preparation of Porous Alumina Film on Aluminum Substrate by Anodization in Oxalic Acid

    2002-01-01

    Self-ordering of the cell arrangement of the anodic porous alumina was prepared in oxalic acid solution at a constant potential of 40V and at a temperature of 20°C. The honeycomb structure made by one step anodization method and two step anodization method is different.Pores in the alumina film prepared by two step anodization method were more ordered than those by one step anodization method.

  7. Preparation of surfactant-free nanoparticles of methacrylic acid copolymers used for film coating

    Nguyen, Cung An; Konan-Kouakou, Yvette Niamien; Allemann, Eric; Doelker, Eric; Quintanar-Guerrero, David; Fessi, Hatem; Gurny, Robert

    2006-01-01

    The aim of the present study was to prepare surfactant-free pseudolatexes of various methacrylic acid copolymers. These aqueous colloidal dispersions of polymeric materials for oral administration are intended for film coating of solid dosage forms or for direct manufacturing of manoparticles. Nanoparticulate dispersions were produced by an emulsification-diffusion method involving the use of partially water-miscible solvents and the mutual saturation of the aqueous and organic phases prior t...

  8. Thin-film sulfuric acid anodizing as a replacement for chromic acid anodizing

    Kallenborn, K. J.; Emmons, J. R.

    1995-01-01

    Chromic acid has long been used to produce a thin, corrosion resistant (Type I) coating on aluminum. Following anodizing, the hardware was sealed using a sodium dichromate solution. Sealing closes up pores inherent in the anodized coating, thus improving corrosion resistance. The thinness of the brittle coating is desirable from a fatigue standpoint, and chromium was absorbed by the coating during the sealing process, further improving corrosion resistance. Unfortunately, both chromic acid and sodium dichromate contain carcinogenic hexavalent chromium. Sulfuric acid is being considered as a replacement for chromic acid. Sulfuric acid of 10-20 percent concentration has traditionally been used to produce relatively thick (Types II and III) or abrasion resistant (Type III) coatings. A more dilute, that is five weight percent, sulfuric acid anodizing process, which produces a thinner coating than Type II or III, with nickel acetate as the sealant has been developed. The process was evaluated in regard to corrosion resistance, throwing power, fatigue life, and processing variable sensitivity, and shows promise as a replacement for the chromic acid process.

  9. Solar-thermochromism of pseudocrystalline nanodroplets of ionic liquid-Ni{sup II} complexes immobilized inside translucent microporous PVDF films

    Wei, Xianjun; Yu, Linpo; Jin, Xianbo; Wang, Dihua [College of Chemistry and Molecular Sciences, Wuhan University Wuhan (China); Chen, George Z. [College of Chemistry and Molecular Sciences, Wuhan University Wuhan (China); Department of Chemical and Environmental Engineering, University of Nottingham (United Kingdom)

    2009-02-16

    Translucent composite films of poly(vinylidene fluoride), ionic liquid, and nickel complexes are successfully fabricated using thermal modulation of dissolution, casting, and drying. These films exhibit high stability in ambient storage and reversible thermochromic responses in air at temperatures achievable under sunlight, promising intelligent windows for controlling solar heat entering the built environment. (Abstract Copyright [2009], Wiley Periodicals, Inc.)

  10. Effect of different complexing agents on the properties of chemical-bath-deposited ZnS thin films

    Liu, Jun; Wei, Aixiang, E-mail: weiax@gdut.edu.cn; Zhao, Yu

    2014-03-05

    Highlights: • To fabricate high quality ZnS films need to promote the ion-by-ion process and restrain cluster-by-cluster process. • The complexation ability of tri-sodium citrate is stronger than that of hydrazine hydrate. • The nucleation density of nuclei determine the performance of ZnS thin films. -- Abstract: Zinc sulfide (ZnS) thin films were deposited on glass substrates using the chemical bath deposition (CBD) technique. The effects of different complexing agents (tri-sodium citrate, hydrazine hydrate) and their concentrations on the structure, composition, morphology, optical properties and growth mechanism of ZnS thin films were investigated. The results indicated that the chemical-bath-deposited ZnS thin films exhibit poor crystallinity and a high Zn/S atomic ratio with an average transmittance of 75% in the range of visible light. The ZnS thin films prepared using hydrazine hydrate as the complexing agent present a more compact surface, a smaller average particle size, and a sharper absorption edge at 300–340 nm compared with those prepared using tri-sodium citrate. Based on our experimental observations and analysis, we conclude that the predominant growth mechanism of ZnS thin films is an ion-by-ion process. The nucleation density of Zn(OH){sub 2} nuclei on the substrate in the initial stage produces the different morphologies and properties of the ZnS thin films prepared using the two complexing agents.

  11. Oxidation states of molybdenum in oxide films formed in sulphuric acid and sodium hydroxide

    X-ray photoelectron spectroscopy is used to investigate the oxidation states of molybdenum in thin films formed potentiostatically, over a range of potentials, in either 1 mol dm−3 H2SO4 or 10 mol dm−3 NaOH at 20 °C. Mo 3d spectra suggested that MoO2 and Mo(OH)2 were the main components of the films, with smaller amounts of MoO3 and possibly Mo2O5. O 1s spectra indicated the presence of oxygen as oxide and hydroxide species and as bound water. Ion beam analysis revealed the formation of thin films at all potentials, with significant losses of oxidized molybdenum to the electrolyte. - Highlights: ► Oxides are formed on molybdenum in sulphuric acid and sodium hydroxide solutions. ► Molybdenum IV and VI are identified by XPS, with MoO2 species dominating. ► Thicknesses of films are determined by ion beam analysis for a range of potentials. ► Films form at low efficiency due to loss of molybdenum species to electrolyte.

  12. Adsorption orientation of sodium of polyaspartic acid effect on anodic films formed on magnesium alloy

    Liu, YuPing; Zhang, Dingfei; Chen, Changguo; Zhang, Jiangang; Cui, libo

    2011-06-01

    We previously reported organic addition agent in improving the performance of anodic film formed on magnesium alloy. Here we report that the environment-friendly electrolyte with sodium of polyaspartic acid (PASP) affects the anodizing process including the microstructure, phase constituents and corrosion performance. We have used SEM, XRD, XPS and polarization curve to study in detail the electrolyte impact. Our results show that the anodic film in electrolyte with 19.2-28.8 g/L PASP is compact, smooth and high corrosion resistant. And also, increasing the PASP concentration ranging from 9.6 to 28.8 g/L results in enhancing the cell voltage, thickness and the content of compound including MgO and Mg 2SiO 4 in anodic film. Interestingly, the anodic film is non-stoichiometric oxide. Comparing with Tafel curves of the anodic film to the addition of PASP or not to, the corrosion current density is 1-2 magnitudes less than the later. Furthermore, a plausible model we propose that the anodizing process is regulated by two main plausible adsorption orientations of PASP at the surface anode. With the increasing of PASP content, the adsorption orientation may transit from "end-on" to "flat-on". This research using organic addition agent PASP may further broaden applications of organic additive in the anti-corrosion engineering and electrochemical surface treatment of magnesium alloy.

  13. Dynamical properties in uniform and periodic growth modes of ascorbic acid crystal domain from thin solution film

    Yamazaki, Yoshihiro; Kikuchi, Mitsunobu; Toda, Akihiko; Wakita, Jun-ichi; Matsushita, Mitsugu

    2013-01-01

    There exists the threshold-sensitive dynamical transition between the uniform and the periodic growth modes in the domain growth of ascorbic acid crystals from its aqueous supersaturated solution film. The crystal growth induces the solution flow. Humidity controls the fluidity of the solution. The solution flow varies the film thickness. The threshold exists in the thickness of the solution film, and the crystal growth almost stops if the thickness becomes lower than the threshold.

  14. Characterization of bioactive RGD peptide immobilized onto poly(acrylic acid) thin films by plasma polymerization

    Seo, Hyun Suk; Ko, Yeong Mu; Shim, Jae Won [Department of Dental Materials, School of Dentistry, MRC Center, Chosun University, Gwangju (Korea, Republic of); Lim, Yun Kyong; Kook, Joong-Ki [Department of Oral Biochemistry, School of Dentistry, Chosun University, Gwangju (Korea, Republic of); Cho, Dong-Lyun [School of Applied Chemical Engineering and Center for Functional Nano Fine Chemicals, Chonnam National University, Gwangju (Korea, Republic of); Kim, Byung Hoon, E-mail: kim5055@chosun.ac.kr [Department of Dental Materials, School of Dentistry, MRC Center, Chosun University, Gwangju (Korea, Republic of)

    2010-11-01

    Plasma surface modification can be used to improve the surface properties of commercial pure Ti by creating functional groups to produce bioactive materials with different surface topography. In this study, a titanium surface was modified with acrylic acid (AA) using a plasma treatment and immobilized with bioactive arginine-glycine-aspartic acid (RGD) peptide, which may accelerate the tissue integration of bone implants. Both terminals containing the -NH{sub 2} of RGD peptide sequence and -COOH of poly(acrylic acid) (PAA) thin film were combined with a covalent bond in the presence of 1-ethyl-3-3-dimethylaminopropyl carbodiimide (EDC). The chemical structure and morphology of AA film and RGD immobilized surface were investigated by X-ray photoelectron spectroscopy (XPS), Fourier transform infrared (FT-IR), atomic force microscopy (AFM), and scanning electron microscopy (SEM). All chemical analysis showed full coverage of the Ti substrate with the PAA thin film containing COOH groups and the RGD peptide. The MC3T3-E1 cells were cultured on each specimen, and the cell alkaline phosphatase (ALP) activity were examined. The surface-immobilized RGD peptide has a significantly increased the ALP activity of MC3T3-E1 cells. These results suggest that the RGD peptide immobilization on the titanium surface has an effect on osteoblastic differentiation of MC3T3-E1 cells and potential use in osteo-conductive bone implants.

  15. Characterization of bioactive RGD peptide immobilized onto poly(acrylic acid) thin films by plasma polymerization

    Plasma surface modification can be used to improve the surface properties of commercial pure Ti by creating functional groups to produce bioactive materials with different surface topography. In this study, a titanium surface was modified with acrylic acid (AA) using a plasma treatment and immobilized with bioactive arginine-glycine-aspartic acid (RGD) peptide, which may accelerate the tissue integration of bone implants. Both terminals containing the -NH2 of RGD peptide sequence and -COOH of poly(acrylic acid) (PAA) thin film were combined with a covalent bond in the presence of 1-ethyl-3-3-dimethylaminopropyl carbodiimide (EDC). The chemical structure and morphology of AA film and RGD immobilized surface were investigated by X-ray photoelectron spectroscopy (XPS), Fourier transform infrared (FT-IR), atomic force microscopy (AFM), and scanning electron microscopy (SEM). All chemical analysis showed full coverage of the Ti substrate with the PAA thin film containing COOH groups and the RGD peptide. The MC3T3-E1 cells were cultured on each specimen, and the cell alkaline phosphatase (ALP) activity were examined. The surface-immobilized RGD peptide has a significantly increased the ALP activity of MC3T3-E1 cells. These results suggest that the RGD peptide immobilization on the titanium surface has an effect on osteoblastic differentiation of MC3T3-E1 cells and potential use in osteo-conductive bone implants.

  16. Characterization of bioactive RGD peptide immobilized onto poly(acrylic acid) thin films by plasma polymerization

    Seo, Hyun Suk; Ko, Yeong Mu; Shim, Jae Won; Lim, Yun Kyong; Kook, Joong-Ki; Cho, Dong-Lyun; Kim, Byung Hoon

    2010-11-01

    Plasma surface modification can be used to improve the surface properties of commercial pure Ti by creating functional groups to produce bioactive materials with different surface topography. In this study, a titanium surface was modified with acrylic acid (AA) using a plasma treatment and immobilized with bioactive arginine-glycine-aspartic acid (RGD) peptide, which may accelerate the tissue integration of bone implants. Both terminals containing the -NH2 of RGD peptide sequence and -COOH of poly(acrylic acid) (PAA) thin film were combined with a covalent bond in the presence of 1-ethyl-3-3-dimethylaminopropyl carbodiimide (EDC). The chemical structure and morphology of AA film and RGD immobilized surface were investigated by X-ray photoelectron spectroscopy (XPS), Fourier transform infrared (FT-IR), atomic force microscopy (AFM), and scanning electron microscopy (SEM). All chemical analysis showed full coverage of the Ti substrate with the PAA thin film containing COOH groups and the RGD peptide. The MC3T3-E1 cells were cultured on each specimen, and the cell alkaline phosphatase (ALP) activity were examined. The surface-immobilized RGD peptide has a significantly increased the ALP activity of MC3T3-E1 cells. These results suggest that the RGD peptide immobilization on the titanium surface has an effect on osteoblastic differentiation of MC3T3-E1 cells and potential use in osteo-conductive bone implants.

  17. Trifluoroacetic acid as excipient destabilizes melittin causing the selective aggregation of melittin within the centrin-melittin-trifluoroacetic acid complex.

    Pastrana-Rios, Belinda; Del Valle Sosa, Liliana; Santiago, Jorge

    2015-07-01

    Trifluoroacetic acid (TFA) may be the cause of the bottleneck in high resolution structure determination for protein-peptide complexes. Fragment based drug design often involves the use of synthetic peptides which contain TFA (excipient). Our goal was to explore the effects of this excipient on a model complex: centrin-melittin-TFA. We performed Fourier transform infrared, two-dimensional infrared correlation spectroscopies and spectral simulations to analyze the amide I'/I'* band for the components and the ternary complex. Melittin (MLT) was observed to have increased helicity upon its interaction with centrin, followed by the thermally induced aggregation of MLT within the ternary complex in the TFA presence. PMID:26798810

  18. Improvement on stability of square planar rhodium (Ⅰ) complexes for carbonylation of methanol to acetic acid

    蒋华; 潘平来; 袁国卿; 陈新滋

    1999-01-01

    A series of square planar cis-dicarbonyl polymer coordinated rhodium complexes with uncoordinated donors near the central rhodium atoms for carbonylation of methanol to acetic acid are reported. Data of IR, XPS and thermal analysis show that these complexes are very stable. The intramolecular substitution reaction is proposed for their high stability. These complexes show excellent catalytic activity, selectivity and less erosion to the equipment for the methanol carbonylation to acetic acid. The distillation process may be used instead of flash vaporization in the manufacture of acetic acid, which reduces the investment on the equipment.

  19. Structure of Langmuir-Blodgett films of fatty acid salts from electron, x-ray, and neutron diffraction data

    The data on the structure of Langmuir-Blodgett films of fatty acid salts obtained by the methods of electron diffraction structure analysis are compared with the corresponding results of X-ray and neutron reflectivity measurements

  20. Structural investigations of complex perovskite oxide films with X-ray diffraction

    Boldyreva, Ksenia; Rata, Diana; Herklotz, Andreas; Bilani-Zeneli, Orkidia; Huehne, Ruben; Schultz, Ludwig; Doerr, Kathrin [IFW Dresden (Germany)

    2009-07-01

    The electronic and magnetic properties of many complex oxides are highly sensitive to external parameters which include mechanical deformation or strain. Thus, X-ray diffraction methods such as reciprocal space mapping are powerful and indispensable for the characterization of thin films, particularly for evaluating the in-plane strain state. The direct influence of strain on the magnetization of epitaxial La{sub 1-x}Sr{sub x}MnO{sub 3} (LSMO) films has been studied utilizing piezoelectric PMN-PT substrates. On the other hand, La{sub 1-x}Sr{sub x}CoO{sub 3} (LSCO) films also reveal large strain-induced changes of the magnetization and the electrical conductivity. Since the in-plane lattice parameter of the piezoelectric substrate, PMN-PT, of {proportional_to}4.02A is larger than that of most correlated oxides, LaSc{sub 1-x}Al{sub x}O{sub 3} (LSAO) has been explored as a buffer layer showing a lattice parameter that is tunable by the composition x. The lattice structure of (i) LSAO buffers depending on the composition and (ii) of magnetic films (LSMO, LSCO) grown in various strain states is discussed.

  1. Synthesis and complex forming property of phosphor acid derivatives

    Full text:With the aim to get new effective and selective extra gents of noble and non-ferrous metals from acid solution and industrial sewage, research of the dependence of 'structure effectiveness' the various phosphor acid derivatives with logical changeable structure (thio phosphor acids, derivatives of dialkoxythiophosphor, O-alkyl-methylphosphon, alkylphenylphosphon, diphenylphosphine acids also 4 methyl-1,3,2 dioxaphosphorinane) which contain different functional groups, the remains of heterocyclic amines and alkaloids, new derivatives of some analytical reagents were synthesized. The structure of synthesized compounds is approved by the results of IR-, PMR-, mass-spectrum analyze. Researching mass-spectrum decay of synthesized phosphor acid derivatives we defined that differing from O-dihexyl-S-propargyl-benzylthio phosphat, mass spectrum decay of O-dialkyl-S-(piperdynobutin-2-il)thio phosphat is characterized by the appearing [M-H]+ ions and during the decay ions with high intensiveness are formed. Fragmentation of M+ O-alkyl-O-(aminoalkyl)phenylphosphonate proceeds in various directions and characterized with the great number of phosphor containing ions, the possession of the second phenyl radical in the molecule of diphenylphosphon acid derivatives changes the fragmentation of molecular ion of diphenylphosphon acid derivatives. The process of extraction of noble (Au, Ag, Pt, Pd, Os) metals from hydrochloric-sulphur-nitrogen acid medium was analyzed by radioactive indicator's method. It was noticed that structure, strength, conformation of compounds, the temperature, of acid medium (0,1-10 M) and the nature of acids (HCL, H2SO4, HNO3) could have strong influence to the effectiveness of metal extraction. During the research of metals extraction from pure solutions we can see the followings: 1) There are such substances, which can be used as effective group reagent towards the Au, Ag and Pd. 2) Derivatives with acetylene extract ions of gold from medium of

  2. Electrical conduction of polyimide films prepared from polyamic acid (PAA and pre-imidized polyimide (PI solution

    2007-07-01

    Full Text Available Electrical conduction characteristics in two different polyimide films prepared by the imidization of polyamic acid (PAA and pre-imidized polyimide (PI solution were investigated. It is found that the current density of the polyimide film from PAA was higher than that of the polyimide film from PI at the same electric field, even though the conduction mechanism in both polyimide films follows the ionic hopping model. The hopping distance was calculated to be 2.8 nm for PAA type and 3.2 nm for PI type polyimide film. It is also found that the decay rate of the residual electrostatic charges on the polyimide films becomes faster in the PAA type than in the PI type polyimide film.

  3. Highly luminescent polycaprolactone films doped with diaquatris(thenoyltrifluoroacetonate)europium(III) complex

    Forster, Pedro L., E-mail: plforster@ipen.br [Nuclear and Energy Research Institute, National Nuclear Energy Commission, Avenida Professor Lineu Prestes 2242, Cidade Universitária, CEP 05508-000 São Paulo, SP (Brazil); Parra, Duclerc F., E-mail: dfparra@ipen.br [Nuclear and Energy Research Institute, National Nuclear Energy Commission, Avenida Professor Lineu Prestes 2242, Cidade Universitária, CEP 05508-000 São Paulo, SP (Brazil); Lugao, Ademar B. [Nuclear and Energy Research Institute, National Nuclear Energy Commission, Avenida Professor Lineu Prestes 2242, Cidade Universitária, CEP 05508-000 São Paulo, SP (Brazil); Kai, Jiang, E-mail: jkai@puc-rio.br [Department of Chemistry, Pontifical Catholic University of Rio de Janeiro, Rua Marquês de São Vicente 225, Gávea, CEP 22451-900 Rio de Janeiro, RJ (Brazil); Brito, Hermi F., E-mail: hefbrito@iq.usp.br [Institute of Chemistry, University of São Paulo, Avenida Professor Lineu Prestes 748, Cidade Universitária, CEP 05508-000 São Paulo, SP (Brazil)

    2015-11-15

    In this work we report the preparation, characterization, thermal and luminescence properties of highly luminescent polycaprolactone (PCL) polymer films incorporated with diaquatris(thenoyltrifluoroacetonate)europium(III) complex [Eu(tta){sub 3}(H{sub 2}O){sub 2}] (doping concentration at 1, 2, 5, 10 and 15 wt%). Thermogravimetry analysis (TGA) showed no weight loss in the range of 323–473 K for the polymeric systems, suggesting that the interaction between the polymer matrix and the Eu{sup 3+}-complex occurs when the carbonyl groups along the polymer backbone substitute the water molecules in the complex precursor. Differential scanning calorimetry (DSC) showed no significant changes in T{sub m} for the film samples, however crystallinity is affected by non combined complex in the polymer chains. The changes in the curve-fitted FTIR spectral areas for each component peak are gradually changed with the increase of doping concentration. The displacement of the C–O for the β-diketonate complex to new positions in PCLE systems provide good evidence that the metal ion is coordinated through the oxygen atoms deriving from PCL. The observation of characteristic emission bands arising from the {sup 5}D{sub 0}→{sup 7}F{sub J} transitions (J=0–4) dominated by the hypersensitive {sup 5}D{sub 0}→{sup 7}F{sub 2} transition at around 614 nm of Eu{sup 3+} ion indicates the incorporation of the Eu{sup 3+} ions in the system corroborating with the CHN and IR data. Luminescence quenching is observed, with the film of 5% doping concentration of the Eu{sup 3+} complexes showing the highest luminescence intensity among all samples. - Highlights: • Distribution of metal ion along polymer chains influences the fluorescence properties. • PCL acts as co-sensitizer to improve energy transfer from the tta{sup −} ligand to the Eu{sup 3+}. • PCL polymer films doped with Eu{sup 3+} enhance quantum yield and lifetimes. • PCL doping process restrains the polymeric

  4. Concentration of eicosapentaenoic acid (EPA) and docosahexaenoic acid (DHA) of Asian catfish oil by urea complexation: optimization of reaction conditions

    Pornpisanu Thammapat; Sirithon Siriamornpun; Patcharin Raviyan

    2016-01-01

    Optimization of the concentrating conditions of eicosapentaenoic acid (EPA) and docosahexaenoic acid (DHA) extracted from Asian catfish oil was studied to obtain a maximum concentration. The crude fish oil was extracted from the belly flap and adipose tissue of Asian catfish, and the extracted oil was used as fresh crude oil. The EPA and DHA were concentrated by the urea complexation method. A hexagonal rotatable design was applied to examine the effects of crystallization temperatur...

  5. Radiation grafting of 4-vinylpyridine onto PP-g-AAc hydrogel films, and its copper (II) complexes

    Complete text of publication follows. A new polymeric system consisting of a comb type copolymer of 4VP onto PAAc hydrogel, grafted onto PP film net-(PP-g-AAc)-g-4VP, was synthesized by gamma radiation in three consecutive steps. This polymeric system has better mechanical properties that the studied hydrogels, pH sensitivity and the ability to form complex with transition metal ions. The synthesized system has chelating ability with transition metal ions due to its structure containing nitrogen and oxygen atoms. In this work we present the swelling behavior of the supported comb-type hydrogel and its complexes with copper (II) ions in acidic aqueous medium. These systems were studied by IR, UVVis and EPR spectroscopy. Two critical pH values were found for net-(PP-g-AAc)-g-4VP at 4.5 and 7.2. Adsorption capacity of Cu(II) ions by the system is 40 mg/g dry polymer, the capacity increases with the increase of pH. The FTIR spectrum of the supported comb-type hydrogel-copper (II) complex shows the appearance of carboxilate groups due to the ion exchange reaction between the supported comb-type hydrogel and Cu(II) ions. The results suggest pH dependence and a coordination mechanism through carboxylate groups of acrylic acid and the nitrogen atom of the pyridine groups of the supported comb-type hydrogel is propose. The chelating ability and pH-responsive behavior of synthesized system make it an attractive material for possible applications in adsorption, enrichment and separation processes from low level wastewater. The authors are grateful to PAPIIT-UNAM, IN200108; CONACyT and Posgrado de Ingenieria, Facultad de Quimica, for support and to S. Castillo, F. Garcia and B. Leal from the ICN-UNAM, for technical assistance.

  6. Photoluminescent study of Polycarbonate (PC) and Poly(9-vinylcarbazole) (PVK) doped films with europium complex

    Polymers doped with rare earth complexes are advantaged in film production for many applications in the luminescent field. In this study luminescent polymer obtained from polycarbonate (PC) and poly(9-vinylcarbazole) films doped with diaquatris(thenoyltrifluoroacetonate)europium(III) complex [Eu(tta)3(H20)2] were prepared and their calorimetric and luminescent properties in the solid state are reported. The thermal behavior was investigated by differential scanning calorimetry (OSC) and thermogravimetry analysis (TGA). Due of the addition of rare earth Eu(tta)3(H20)2] into PC and PVK matrices, changes were observed in the thermal behavior concerning the glass transition and thermal stability. Characteristic broadened narrow bands arising from the 5D0 -→ 7FJ transitions (J = 0-4) of Eu3+ ion indicate the incorporation of the Eu3+ ions into those polymers. The luminescent films show enhancement emission intensity with an increase in the rare earth concentration in polymeric matrix accompanied by decrease in thermal stability. (author)

  7. CdS thin films obtained by thermal treatment of cadmium(II) complex precursor deposited by MAPLE technique

    Thin films of [Cd{SSi(O-But)3}(S2CNEt2)]2, precursor for semiconducting CdS layers, were deposited on silicon substrates by Matrix-Assisted Pulsed Laser Evaporation (MAPLE) technique. Structural analysis of the obtained films by Fourier transform infrared spectroscopy (FTIR) confirmed the viability of the procedure. After the deposition of the coordination complex, the layers are manufactured by appropriate thermal treatment of the system (thin film and substrate), according to the thermal analysis of the compound. Surface morphology of the thin films was investigated by atomic force microscopy (AFM) and spectroscopic-ellipsometry (SE) measurements.

  8. Transition Metal Complexes of Phosphinous Acids Featuring a Quasichelating Unit: Synthesis, Characterization, and Hetero-bimetallic Complexes.

    Allefeld, Nadine; Bader, Julia; Neumann, Beate; Stammler, Hans-Georg; Ignat'ev, Nikolai; Hoge, Berthold

    2015-08-17

    Diorganophosphane oxides were employed as preligands for the synthesis of catalytically active transition metal complexes of the phosphinous acids (CF3)2POH and (C2F5)2POH. Their reactions with solid PtCl2 and PdCl2 led to the formation of mononuclear phosphinous acid complexes [Cl2M{P(R(f))2OH}2] (M = Pd, Pt; R(f) = C2F5, CF3), which can be crystallized, for example, as its pyridinium salts, 2[HPy](+)[Cl2Pd{P(CF3)2O}2](2-). In vacuo HCl is liberated from the neutral palladium complexes affording mixtures of di- and polynuclear complexes. Moreover, (C2F5)2POH was reacted with several β-diketonato complexes of palladium, platinum, and nickel yielding air- and moisture-stable complexes [(acac)M{[P(R(f))2O]2H}], featuring a quasichelating phosphinous acid phosphinito unit {P(R(f))2O···H···O(R(f))2P}(-). Treatment of [Ni(Cp)2] (Cp = cyclopentadienyl) and [(cod)RhCl]2 (cod = 1,5-cyclooctadiene) with (C2F5)2POH leads to the substitution of one Cp or chloro ligand by a quasichelating unit. The novel coordination compounds were characterized by NMR and IR spectroscopies, mass spectrometry, and X-ray diffraction analysis. The platinum complex [(acac)Pt{[P(C2F5)2O]2H}] (acac = acetylacetonato) was used for the construction of hetero-bimetallic complexes by the treatment with [(cod)RhCl]2 and [Ni(Cp)2]. The trinuclear bimetallic complex [{(acac)Pt[P(C2F5)2O]2}2Ni] is the first structurally characterized hetero-bimetallic species containing a bis(perfluoroalkyl)phosphinito bridge. PMID:26242286

  9. Constitution of novel polyamic acid/polypyrrole composite films by in-situ electropolymerization

    The preparation and characterization of polyamic acid-polypyrrole (PAA/PPy) composite films are reported in this paper. The thin films were synthesized by electrochemical method from a solution containing controlled molar ratio of chemically synthesized polyamic acid (PAA) and pyrrole monomer. Homogenous films were obtained by incorporating PAA into electropolymerized polypyrrole (PPy) thin film. The concentration of PAA (1.37 × 10−6 M) was kept fixed throughout the composite ratio analysis, whilst the concentration of PPy was varied from 1.90 × 10−3 M to 9.90 × 10−3 M. The PAA/PPy thin films were electrodeposited at a glassy carbon electrode (GCE) and characterized using Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, Atomic force microscopy (AFM), Scanning electron microscopy (SEM) and voltammetry. The composition that best represented the homogenous incorporation of PAA into PPy matrix was observed at a PAA/PPy ratio of 1: 4.13 × 10−3. This composite was observed to have two sets of coupled peaks with formal potential 99 mV and 567 mV respectively. The De determined from cyclic voltammetry using the anodic peak currents were found to be twice as high (5.82 × 10−4 cm2/s) compared to the De calculated using the cathodic peak currents (2.60 × 10−4 cm2/s), indicating that the composite favours anodic electron mobility. Surface morphology and spectroscopy data support the formation of a homogenous polymer blend at the synthesis ratio of 1: 4.13 × 10−3

  10. Solution structures of lipoyl domains of the 2-oxo acid dehydrogenase complexes from Azotobacter vinelandii. Implications for molecular recognition.

    Berg, A.

    1997-01-01

    The 2-oxo acid dehydrogenase complexes are large multienzyme complexes that catalyse the irreversible oxidative decarboxylation of a specific 2-oxo acid to the corresponding acyl-CoA derivative. The pyruvate dehydrogenase complex (PDHC) converts the product of the glycolysis, pyruvate, to acetyl-CoA, which enters the tricarboxylic acid cycle. The 2-oxoglutarate dehydrogenase complex (OGDHC functions in the tricarboxylic acid cycle itself by converting 2-oxoglutarate to succinyl-CoA. The branc...

  11. Complexation of lanthanides and actinides with humic acids. Appendix II

    Natural waters are the main transport medium for radionuclides in the geosphere in case of an accidental release of radioactivity from a nuclear waste disposal. Complexation studies of radionuclides with natural organic substances present in aquifers are important to perform in order to predict their behaviour in natural systems. Interactions of two trivalent elements, curium and dysprosium, representative respectively for actinides and lanthanides, have been investigated by Time-Resolved Laser-Induced Spectrofluorometry (TRLIS) allowing to work at low concentrations of cations (10-6 M-10-8 M). By using a 'Fluorescence titration' method, complexing capacities and interaction constants are obtained over a broad pH range (4 to 7) at a constant ionic strength (0.1 M). The complexing behaviour of Cm and Dy is analysed. Data are discussed and compared with existing literature data. (orig.)

  12. Complexation and biodistribution study of 111In complexes of bifunctional phosphinic acid analogues of H4DOTA

    Forsterová, Michaela; Zimová, Jana; Petrík, M.; Lázníček, M.; Lázníčková, A.; Hermann, P.; Melichar, František

    2007-01-01

    Roč. 2, č. 337 (2007), s. 34-34. ISSN 1619-7070 R&D Projects: GA AV ČR 1QS100480501 Institutional research plan: CEZ:AV0Z10480505 Keywords : bifunctional H4DOTA ligands * phosphinic acid analogues, * complexation of 111In Subject RIV: FR - Pharmacology ; Medidal Chemistry

  13. Complexation and extraction of series 4f, 5f and 4d ions by dialkyldithiophosphoric acids

    A study was carried out on the complexing and extracting properties of various dialkyldithiophosphoric acids towards ions of the 4f, 5f and 4d series. Sulphurated donors complex and extract ions of the 4f and 5f series less strongly than their oxygenated homologues. However the affinity of trivalent actinide ions for dialkythiophosphate ions is shown to be greater than that of lanthanides. The conditions of ruthenium extraction from nitric acid are defined

  14. Determination of aminoglycoside antibiotics using complex compounds of chromotropic acid bisazoderivatives with rare earth ions

    Studies of complex formation of bisazo derivatives of chromotropic acid with rare earth ions and aminoglycoside antibiotics have made it possible to choose carboxyarsenazo, orthanyl R and carboxynitrazo as highly sensitive reagents for determining aminoglycoside antibiotics. Conditions have been found for the formation of precipitates of different-ligand complexes containing rare earth ions, bisazo derivatives of chromotropic acid and aminogylcoside antibiotics. A procedure has been worked out of determining the antibiotics in biological samples with carboxyarsenazo

  15. FT-IR spectroscopic studies of fulvic acid from weathered coal and its complexes

    FT-IR spectrum of fulvic acid from wheathered coal of Gongxian is determined using second derivative spectroscopy and the spectroscopic resolution is enhanced. Moreover, FT-IR spectra of the complexes of fulvic acid with Ca2+, Ba2+, Cu2+, Pb2+ and UO22+ under different pH are determined and the nature of the coordination of these complexes is discussed

  16. Water-free Alkaline Polymer-inorganic Acid Complexes with High Conductivity at Ambient Temperature

    O.V.Chervakov; M.V.Andriianova; V.V.Riabenko; A.V.Markevich; E.M.Shembel; D.Meshri

    2007-01-01

    1 Results Recently increased interest is shown to proton conducting materials based on the alkaline polymer-inorganic acid complexes that is caused by a possibility of their application as the high-temperature electrolyte systems for various electrochemical devices (fuel cells,sensors,lithium power sources etc.).Complexes of inorganic acids with the alkaline polymers (polybenzimidazoles[1],polyvinylpyridines[2]) are characterized by high ionic conductivity at ambient temperatures (up to 10-2 Ω-1·cm-1) a...

  17. Complex behaviour of vacancy point-defects in SrRuO3 thin films.

    Schraknepper, Henning; Bäumer, Christoph; Dittmann, Regina; De Souza, Roger A

    2015-01-14

    The behaviour of point defects in thin, epitaxial films of the oxide electrode SrRuO3 was probed by means of diffusion measurements. Thin-film SrRuO3 was deposited by means of pulsed laser deposition (PLD) on (100) oriented, undoped single crystal SrTiO3 substrates. (16)O/(18)O exchange anneals were employed to probe the behavior of oxygen vacancies. Anneals were performed in the temperature range 850 ≤T/K≤ 1100 at an oxygen partial pressure of pO2 = 500 mbar. Samples were subsequently analyzed by means of Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS). The measured oxygen isotope penetration profiles comprised, surprisingly, two features. Oxygen tracer diffusion coefficients determined for thin-film SrRuO3 are amongst the lowest measured for nominally undoped perovskite-type oxides. The activation enthalpy of oxygen tracer diffusion was found to be ≈ 2 eV. Diffusion of Ti from the SrTiO3 substrates into the SrRuO3 thin films, probing the cation defects, was also observed in ToF-SIMS profiles; here, too, the diffusion profiles showed two features. The activation enthalpy of titanium diffusion was found to be ΔHDTi≈ 4 eV. We propose a model-cation sublattice equilibration-that accounts for the appearance of two features in both anion and cation diffusion profiles. We suggest that the observed complex behavior arises from the metastable defect structure of PLD thin films and the unusual defect structure of SrRuO3. PMID:25413988

  18. Metal ion complexation properties of fulvic acids extracted from composted sewage sludge as compared to a soil fulvic acid.

    Esteves da Silva, Joaquim C G; Oliveira, César J S

    2002-07-01

    Complexation properties of an anthropogenic fulvic acid (FA) extracted from a composted sewage sludge (csFA) for Cu(II), Pb(II) and Cd(II) were studied at pH=6 and at a concentration of 25 mg L(-1). For the case of Cu(II), a particular analysis of the complexation phenomena was done at pH values of 3, 4, 5 and 6 and at aqueous FA concentrations of 25, 50 and 100 mg L(-1) by synchronous excitation molecular fluorescence spectroscopy (SyF). Potentiometric titrimetry with Cu(II), Pb(II), Cd(II) and H+ ion-selective electrodes and acid-base conductimetric titrations were used to obtain experimental information about the acid properties and complexation phenomena. A comparison of the results obtained for csFA with a natural soil FA (sFA) was made. Differences have been detected in the structural composition of the two samples and in the structure of the binding sites. In the csFA, binding site structures containing nitrogen probably play an important role in the complexation, besides oxygen containing structures. Complexation by sFA is mainly due to carboxylic and phenolic structures. Nevertheless, this work shows that csFA have macroscopic complexation properties (magnitude of the conditional stability constant and binding sites concentration) somewhat similar to the natural sFA samples. PMID:12188141

  19. Transparent nanocellulosic multilayer thin films on polylactic acid with tunable gas barrier properties.

    Aulin, Christian; Karabulut, Erdem; Tran, Amy; Wågberg, Lars; Lindström, Tom

    2013-08-14

    The layer-by-layer (LbL) deposition method was used for the build-up of alternating layers of nanofibrillated cellulose (NFC) or carboxymethyl cellulose (CMC) with a branched, cationic polyelectrolyte, polyethyleneimine (PEI) on flexible poly (lactic acid) (PLA) substrates. With this procedure, optically transparent nanocellulosic films with tunable gas barrier properties were formed. 50 layer pairs of PEI/NFC and PEI/CMC deposited on PLA have oxygen permeabilities of 0.34 and 0.71 cm(3)·μm/m(2)·day·kPa at 23 °C and 50% relative humidity, respectively, which is in the same range as polyvinyl alcohol and ethylene vinyl alcohol. The oxygen permeability of these multilayer nanocomposites outperforms those of pure NFC films prepared by solvent-casting. The nanocellulosic LbL assemblies on PLA substrates was in detailed characterized using a quartz crystal microbalance with dissipation (QCM-D). Atomic force microscopy (AFM) reveals large structural differences between the PEI/NFC and the PEI/CMC assemblies, with the PEI/NFC assembly showing a highly entangled network of nanofibrils, whereas the PEI/CMC surfaces lacked structural features. Scanning electron microscopy images showed a nearly perfect uniformity of the nanocellulosic coatings on PLA, and light transmittance results revealed remarkable transparency of the LbL-coated PLA films. The present work demonstrates the first ever LbL films based on high aspect ratio, water-dispersible nanofibrillated cellulose, and water-soluble carboxymethyl cellulose polymers that can be used as multifunctional films and coatings with tailorable properties, such as gas barriers and transparency. Owing to its flexibility, transparency and high-performance gas barrier properties, these thin film assemblies are promising candidates for several large-scale applications, including flexible electronics and renewable packaging. PMID:23834391

  20. Sandwich-Architectured Poly(lactic acid)-Graphene Composite Food Packaging Films.

    Goh, Kunli; Heising, Jenneke K; Yuan, Yang; Karahan, Huseyin E; Wei, Li; Zhai, Shengli; Koh, Jia-Xuan; Htin, Nanda M; Zhang, Feimo; Wang, Rong; Fane, Anthony G; Dekker, Matthijs; Dehghani, Fariba; Chen, Yuan

    2016-04-20

    Biodegradable food packaging promises a more sustainable future. Among the many different biopolymers used, poly(lactic acid) (PLA) possesses the good mechanical property and cost-effectiveness necessary of a biodegradable food packaging. However, PLA food packaging suffers from poor water vapor and oxygen barrier properties compared to many petroleum-derived ones. A key challenge is, therefore, to simultaneously enhance both the water vapor and oxygen barrier properties of the PLA food packaging. To address this issue, we design a sandwich-architectured PLA-graphene composite film, which utilizes an impermeable reduced graphene oxide (rGO) as the core barrier and commercial PLA films as the outer protective encapsulation. The synergy between the barrier and the protective encapsulation results in a significant 87.6% reduction in the water vapor permeability. At the same time, the oxygen permeability is reduced by two orders of magnitude when evaluated under both dry and humid conditions. The excellent barrier properties can be attributed to the compact lamellar microstructure and the hydrophobicity of the rGO core barrier. Mechanistic analysis shows that the large rGO lateral dimension and the small interlayer spacing between the rGO sheets have created an extensive and tortuous diffusion pathway, which is up to 1450-times the thickness of the rGO barrier. In addition, the sandwiched architecture has imbued the PLA-rGO composite film with good processability, which increases the manageability of the film and its competency to be tailored. Simulations using the PLA-rGO composite food packaging film for edible oil and potato chips also exhibit at least eight-fold extension in the shelf life of these oxygen and moisture sensitive food products. Overall, these qualities have demonstrated the high potential of a sandwich-architectured PLA-graphene composite film for food packaging applications. PMID:27028268

  1. Pulsed electrodeposition of oxygen-free tin monosulfide thin films using lactic acid/sodium lactate buffered electrolytes

    In this study, tin monosulfide (SnS) thin films have been prepared on indium-tin-oxide-covered glass substrates from an acidic electrolyte containing a pH buffer of lactic acid/sodium lactate using pulsed electrodeposition method. Results from Auger electron spectroscopy confirmed that nearly oxygen-free and stoichiometric SnS thin films were attained. X-ray diffraction and scanning electron micrograph studies indicated the formation of a smooth α-SnS thin film with the orthorhombic structure. Moreover, optical transmission spectroscopy showed a direct optical band gap of 1.39 eV and the photoelectrochemical measurements revealed the p-type conductivity.

  2. Contribution to the study of pertechnetate (sup(99m)Tc) stannous citrate - citric acid complexation

    Pertechnetate/citric acid/stannous citrate complexation carried out from a lyophilisate of stannous citrate in citric medium at pH5 leads to the formation of separable compounds. These compounds are tin-free technetium citrates. Similar results have been described in the case of complexation reactions with glycolic, thioglycolic and thiomalic acids and with other carboxylates such as dimercaptosuccinic acid. These processes include the reduction of Tcsup(VIII) by Snsup(II) in the presence of thiomalic acid under conditions similar to our own: stannous thiomalate in thiomalic medium to which is added the pertechnetate solution producing Tc-thiomalate complexes variable with the reaction pH. Also worth considering is the possible complexation between pertechnetate and the same acid in the absence of reducing ion, following a special procedure (heating). The complexes described here contain the oxotechnetium bond (terminal oxygen-technetium) and a strong probability exists in favour of dimerisation. Their stability, for a reaction in acid solution: pH 5.0/5.5, becomes satisfactory if: the solution is concentrated enough; bubbling by an inert gas is carried out; room temperature is not exceeded. The development takes place through a partial reoxidation characterised by colour change. An original interaction between reduced states of Tc and citric acid may be claimed with certainty under our experimental conditions. The difficulty then lies in the passage to the tracer stage when the isotope sup(99m)Tc is used

  3. Biodegradable starch-based films containing saturated fatty acids: thermal, infrared and raman spectroscopic characterization

    Marcelo M. Nobrega

    2012-01-01

    Full Text Available Biodegradable films of thermoplastic starch and poly (butylene adipate co-terephthalate (PBAT containing fatty acids were characterized thermally and with infrared and Raman spectroscopies. The symmetrical character of the benzene ring in PBAT provided a means to illustrate the difference between these spectroscopic techniques, because a band appeared in the Raman spectrum but not in the infrared. The thermal analysis showed three degradation stages related to fatty acids, starch and PBAT. The incorporation of saturated fatty acids with different molecular mass (caproic, lauric and stearic did not change the nature of the chemical bonds among the components in the blends of starch, PBAT and glycerol, according to the thermal analysis, infrared and Raman spectroscopies.

  4. Obtaining a Flexible Film Elaborated from Cassava Thermoplastic Starch and Polylactic Acid

    Germán A. Arboleda

    2015-01-01

    Full Text Available A flexible film was obtained from a blend of cassava thermoplastic starch and polylactic acid, using maleic anhydride as coupling agent. For this, an experimental design with three factors was used: polylactic acid content, coupling agent content, and temperature profile of the blown extrusion. It was found that the three factors generated significant differences on the response variables of tensile mechanical properties individually as in their triple interaction. Differential scanning calorimetry (DSC was used by understanding the behavior of thermal properties of TPS/PLA blends with and without coupling agent, finding similar results between both. From this, the combination with 28% polylactic acid, 0.87% coupling agent, and 155.75°C temperature profile permitted the obtaining of a material with outstanding mechanical properties and offered advantages from the economic point of view.

  5. Second-harmonic generation in mixed stilbazium salt/arachidic acid Langmuir-Blodgett films

    Liu, Liying; Zheng, Jiabiao; Wang, Wencheng; Zhang, Zhiming; Tao, Fenggang; Xu, Linxiao; Hu, Jiacong

    1992-10-01

    A stilbazium salt was synthesized and its second-order molecular polarizability was deduced to be 1.2×10 -27 esu. Measurements of second-harmonic generation and small-angle X-ray diffraction on Langmuir-Blodgett films of the stilbazium salt/arachide acid mixtures showed that the mixed compounds with molar ratios of 1:2 and 1:5 could form multilayers with large second- order optical nonlinearity. Second harmonic generation study on the alternate multilayers of stilbazium salt/arachide acid and arachidic acid showed that the second-harmonic signals were increasing monotonously up to 80 bilayers, but the increment was lower than the value predicted theoretically by the quadratic law. Possible reasons are discussed.

  6. Silver release and antimicrobial properties of PMMA films doped with silver ions, nano-particles and complexes

    Materials prepared on the base of bioactive silver compounds have become more and more popular due to low microbial resistance to silver. In the present work, the efficiency of polymethylmethacrylate (PMMA) thin films doped with silver ions, nanoparticles and silver–imidazole polymer complex was studied by a combination of AAS, XPS and AFM techniques. The biological activities of the proposed materials were discussed in view of the rate of silver releasing from the polymer matrix. Concentrations of Ag active form were estimated by its ability to interact with L-cysteine using electronic circular dichroism spectroscopy. Rates of the released silver were compared with the biological activity in dependence on the form of embedded silver. Antimicrobial properties of doped polymer films were studied using two bacterial strains: Staphylococcus epidermidis and Escherichia coli. It was found that PMMA films doped with Ag+ had greater activity than those doped with nanoparticles and silver–imidazole polymeric complexes. However, the antimicrobial efficiency of Ag+ doped films was only short-term. Contrary, the antimicrobial activity of silver–imidazole/PMMA films increased in time of sample soaking. - Highlights: • PMMA thin films doped with silver ions, nanoparticles (AgNPs) and silver–imidazole helical complexes (AgIm) were studied. • Silver release from doped polymer films and its biological activity were estimated. • Antimicrobial properties of doped polymer films were also studied. • Ag ions doped films showed the strongest antimicrobial activity, which quickly disappeared. • AgIm and AgNPs doped films showed more stable antimicrobial properties. • AgIm complexes conserve their structure after addition into polymer and after leaching

  7. Silver release and antimicrobial properties of PMMA films doped with silver ions, nano-particles and complexes

    Lyutakov, O., E-mail: lyutakoo@vscht.cz [Department of Solid State Engineering, Institute of Chemical Technology, Prague (Czech Republic); Goncharova, I. [Department of Analytical Chemistry, Institute of Chemical Technology, Prague (Czech Republic); Rimpelova, S. [Department of Biochemistry and Microbiology, Institute of Chemical Technology, Prague (Czech Republic); Kolarova, K.; Svanda, J.; Svorcik, V. [Department of Solid State Engineering, Institute of Chemical Technology, Prague (Czech Republic)

    2015-04-01

    Materials prepared on the base of bioactive silver compounds have become more and more popular due to low microbial resistance to silver. In the present work, the efficiency of polymethylmethacrylate (PMMA) thin films doped with silver ions, nanoparticles and silver–imidazole polymer complex was studied by a combination of AAS, XPS and AFM techniques. The biological activities of the proposed materials were discussed in view of the rate of silver releasing from the polymer matrix. Concentrations of Ag active form were estimated by its ability to interact with L-cysteine using electronic circular dichroism spectroscopy. Rates of the released silver were compared with the biological activity in dependence on the form of embedded silver. Antimicrobial properties of doped polymer films were studied using two bacterial strains: Staphylococcus epidermidis and Escherichia coli. It was found that PMMA films doped with Ag{sup +} had greater activity than those doped with nanoparticles and silver–imidazole polymeric complexes. However, the antimicrobial efficiency of Ag{sup +} doped films was only short-term. Contrary, the antimicrobial activity of silver–imidazole/PMMA films increased in time of sample soaking. - Highlights: • PMMA thin films doped with silver ions, nanoparticles (AgNPs) and silver–imidazole helical complexes (AgIm) were studied. • Silver release from doped polymer films and its biological activity were estimated. • Antimicrobial properties of doped polymer films were also studied. • Ag ions doped films showed the strongest antimicrobial activity, which quickly disappeared. • AgIm and AgNPs doped films showed more stable antimicrobial properties. • AgIm complexes conserve their structure after addition into polymer and after leaching.

  8. The properties of solid Zn(II)-amino acid complexes in the form of suspensions.

    Dolińska, B

    2001-10-01

    An investigation was made into the experimental conditions for the formation of poorly soluble complexes of the divalent Zinc(II) combined with the following selected amino acids: tyrosine, tryptophan, cysteine, histidine, and alanine, in the form of suspensions for parenteral administration. The number of Zn(II)-binding sites in the amino acid (n) as well as the amino acid affinity to Zn(II) (Ka), were determined. Cysteine was found to have the highest number of Zn(II)-binding sites--3, whereas alanine the lowest--1. In the conditions described herein, Zn(II) amino acid complexes of diverse stability (durability) were obtained. The analysis of the kinetics of the binding revealed that the most stable complexes were those formed by Zn(II) in combination with tryptophan (Ka = 405.78 microM(-1) +/- 12.17), and with tyrosine (Ka = 343.88 microM +/- 22.35); whereas the least stable complexes were those formed by Zn(II) in combination with histidine (Ka = 29.90 microM +/- 4.78), and with alanine (Ka = 13.0 microM(-1) +/- 1.04). Cysteine formed complexes of intermediate stability (Ka = 168.53 microM(-1) +/- 12.36). The stability ofthe Zn(II) amino acid complexes obtained was conditioned by both the molecular weight (P = 0.033) of the amino acid and its isoelectric point (P < 0.001). PMID:11718265

  9. Properties study of poly(l-lactic acid) film modified by blending with flexible poly(tetramethylene glycol)

    A series of poly(L-lactic acid)/poly(tetramethylene glycol) (PLLA/PTMG) blend films were prepared by casting the polymer blend solution in chloroform. Surface morphologies of the PLLA/PTMG blend films were investigated by scanning electron microscopy (SEM). Thermal, mechanical, and chemical properties of PLLA/PTMG blend films were studied by differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), tensile tests, and surface contact angle tests. It was revealed that the introduction of flexible PTMG could markedly modify the properties of the PLLA films. (author)

  10. A study on dissociation and complexation of fuivic acid from weathered coal using potentiometric titration

    The dissociation and complexation of fulvic acid from weathered coal (from Gong Xian, Henan Province) are studied by means of potentiometric titrations. The effects of salt concentration and functional group heterogeneity on the apparent dissociation constants are characterized. Some characteristics of the binding of the ions Cu(II), Th(IV) and La(III) on this fulvic acid are determined

  11. Photoactive layer-by-layer films of cellulose phosphate and titanium dioxide containing phosphotungstic acid

    Ullah, Sajjad [Instituto de Química de São Carlos, Universidade de São Paulo, PO Box 780, São Carlos, São Paulo 13564-970 (Brazil); Acuña, José Javier Sáez [Centro de Ciências Naturais e Humanas, Universidade Federal do ABC, Santo Andre, Sao Paulo, 09210-170 (Brazil); Pasa, André Avelino [Surface and Thin Film Laboratory, Physics Department, Federal University of Santa Catarina, PO Box 476, Florianópolis, SC 88040-900 (Brazil); Bilmes, Sara A. [Universidad de Buenos Aires, Facultad Ciencias Exactas y Naturales, Instituto de Química Física de los Materiales, Medio Ambiente y Energía – INQUIMAE, Ciudad Universitaria, Pab. 2, Buenos Aires C1428EHA (Argentina); Vela, Maria Elena; Benitez, Guillermo [Laboratorio de Nanoscopías y Fisicoquímica de Superficies, Instituto de Investigaciones Fisicoquímicas Teóricas y Aplicadas (INIFTA), Universidad Nacional de La Plata – CONICET, diagonal 113 esquina 64. C.C.16.Suc.4, 1900 La Plata (Argentina); Rodrigues-Filho, Ubirajara Pereira, E-mail: uprf@iqsc.usp.br [Instituto de Química de São Carlos, Universidade de São Paulo, PO Box 780, São Carlos, São Paulo 13564-970 (Brazil)

    2013-07-15

    A versatile layer-by-layer (LbL) procedure for the preparation of highly dispersed, adherent and porous multilayer films of TiO{sub 2} nanoparticles (NPs) and phosphotungstic acid (HPW) on a variety of substrates at room temperature was developed based on the use of cellulose phosphate (CP) as an efficient and non-conventional polyelectrolyte. UV/vis absorption spectroscopy confirmed the linear and regular growth of the films with the number of immersion cycles and a strong adsorption ability of CP towards TiO{sub 2} NPs. FTIR spectroscopy showed that HPW binds to the surface of TiO{sub 2} through the oxygen atom at the corner of the Keggin structure. XPS results showed that the interaction between TiO{sub 2} and CP is through Ti–O–P linkage. A model is proposed for the TiO{sub 2}–HPW interaction based on XPS and FTIR results. FEG/SEM study of the surface morphology revealed a porous film structure with a homogenous distribution of the TiO{sub 2} NPs induced by CP. HRTEM studies showed that the resulting composite films consist of crystalline anatase and rutile phases and poly-nano-crystalline HPW with a semi-crystalline TiO{sub 2}–HPW interface. These CP/TiO{sub 2} and CP/TiO{sub 2}/HPW LbL films showed good photoactivity against both saturated and unsaturated species, for instance, stearic acid (SA), crystal violet (CV) and methylene blue (MB) under UV irradiation. The CP/HPW films formed on bacterial cellulose (BC) showed good photochromic response which is enhanced in presence of TiO{sub 2} due to an interfacial electron transfer from TiO{sub 2} to HPW. This simple and environmentally safe method can be used to form coatings on a variety of surfaces with photoactive TiO{sub 2} and TiO{sub 2}/HPW films.

  12. Metals complexation with humic acids in surface water of different natural–climatic zones

    Dinu M. I.

    2013-04-01

    Full Text Available Humic acids extracted from different soils. The stability constants of metal humates and acid dissociation constant humic acids were calculated. Forms of metals in natural waters was determined with use account their chemical composition and content and properties of organic matter. We assessed metals speciation in water objects with account for competitive reactions resulting in formation of hydroxide, hydrocarbonate, sulfate, and chloride metal complexes and obtained a competitive series of metal activity in natural waters of the zones considered.

  13. Retention of ruthenium-nitrosyl complexes in 30% TBP-kerosene-laurohydroxamic acid

    The degradation products of diluent cause RuNO complexes to be retained in the irradiated organic solvent. The Ru retention in 30% TBP-kerosene-laurohydroxamic acid increases with hydroxamic acid concentration, aging temperature and aging time of loaded organic phase. For U concentrations in the aqueous phase above 30 g/l, Ru retention is not influenced by NaNO2, although NaNO2, can destroy the hydroxamic acid. (orig.)

  14. Photoelectrocatalytic degradation of oxalic acid by spray deposited nanocrystalline zinc oxide thin films

    Shinde, S.S. [Electrochemical Materials Laboratory, Department of Physics, Shivaji University, Kolhapur 416004 (India); Shinde, P.S. [Department of Nano-Engineering, Kyungnam University, Masan 631-701 (Korea, Republic of); Sapkal, R.T. [Electrochemical Materials Laboratory, Department of Physics, Shivaji University, Kolhapur 416004 (India); Oh, Y.W. [Department of Nano-Engineering, Kyungnam University, Masan 631-701 (Korea, Republic of); Haranath, D. [National Physical Laboratory, Dr. K.S. Krishnan Road, New Delhi 110 012 (India); Bhosale, C.H. [Electrochemical Materials Laboratory, Department of Physics, Shivaji University, Kolhapur 416004 (India); Rajpure, K.Y., E-mail: rajpure@yahoo.com [Electrochemical Materials Laboratory, Department of Physics, Shivaji University, Kolhapur 416004 (India)

    2012-10-15

    Highlights: Black-Right-Pointing-Pointer Influence of substrate temperature onto the physico-chemical properties. Black-Right-Pointing-Pointer Photochemical, structural, luminescent, optoelectrical and thermal properties. Black-Right-Pointing-Pointer The kinetics of oxalic acid degradation with reaction mechanism. Black-Right-Pointing-Pointer Extent of mineralization by COD and TOC. - Abstract: The high quality nano-crystalline zinc oxide thin films are deposited onto corning glasses by spray pyrolysis technique. The influence of reaction temperature onto their photoelectrochemical, structural, morphological, optoelectronic, luminescence and thermal properties has been investigated. The structural characteristics studied by X-ray diffractometry has complemented by resistivity measurements and UV-Vis spectroscopy. The photoelectrochemical activity shows enhancement in short circuit current (I{sub sc} = 0.357 mA) and open circuit voltage (V{sub oc} = 0.48 V). Direct band gap calculated by considering R and T values of ZnO thin films increases from 3.14-3.21 eV exhibiting a slight blue shift in band edge. Three characteristic luminescence peaks having near band-edge, blue and green emission are observed in the photoluminescence spectra. The specific heat and thermal conductivity study shows the phonon conduction behavior is dominant in films. Photocatalytic degradation of oxalic acid followed with reaction mechanism by using zinc oxide photoelectrode under solar illumination has been investigated.

  15. Photoelectrocatalytic degradation of oxalic acid by spray deposited nanocrystalline zinc oxide thin films

    Highlights: ► Influence of substrate temperature onto the physico-chemical properties. ► Photochemical, structural, luminescent, optoelectrical and thermal properties. ► The kinetics of oxalic acid degradation with reaction mechanism. ► Extent of mineralization by COD and TOC. - Abstract: The high quality nano-crystalline zinc oxide thin films are deposited onto corning glasses by spray pyrolysis technique. The influence of reaction temperature onto their photoelectrochemical, structural, morphological, optoelectronic, luminescence and thermal properties has been investigated. The structural characteristics studied by X-ray diffractometry has complemented by resistivity measurements and UV–Vis spectroscopy. The photoelectrochemical activity shows enhancement in short circuit current (Isc = 0.357 mA) and open circuit voltage (Voc = 0.48 V). Direct band gap calculated by considering R and T values of ZnO thin films increases from 3.14–3.21 eV exhibiting a slight blue shift in band edge. Three characteristic luminescence peaks having near band-edge, blue and green emission are observed in the photoluminescence spectra. The specific heat and thermal conductivity study shows the phonon conduction behavior is dominant in films. Photocatalytic degradation of oxalic acid followed with reaction mechanism by using zinc oxide photoelectrode under solar illumination has been investigated.

  16. Mixture design applied for the study of the tartaric acid effect on starch/polyester films.

    Olivato, J B; Nobrega, M M; Müller, C M O; Shirai, M A; Yamashita, F; Grossmann, M V E

    2013-02-15

    Tartaric acid (TA), a dicarboxylic acid, can act as a compatibiliser in starch/polyester blends. A mixture design was proposed to evaluate the effect of TA on the properties of starch/poly (butylene adipate co-terephthalate) (PBAT) blown films plasticised with glycerol. The interaction between the starch/PBAT and the TA has a positive effect on the tensile strength and puncture force. Additionally, greater proportions of TA increased Young's modulus. The starch+PBAT/TA and Gly/TA interactions contributed to a reduction in the water vapour permeability of the films. The inclusion of TA did not change the crystallinity of the samples. Formulations with intermediate proportions of TA (0.8 g/100 g) were shown to produce the best compatibilising effect. This was observed by DMA analysis as a consequence of the perfect equilibrium between the contributions of TA as a compatibiliser and in the acidolysis of starch, resulting in films with a tensile strength of 5.93 MPa, a possible alternative to non-biodegradable packaging. PMID:23399209

  17. Studies on surface graft polymerization of acrylic acid onto PTFE film by remote argon plasma initiation

    The graft polymerization of acrylic acid (AAc) was carried out onto poly(tetrafluoroethylene) (PTFE) films that had been pretreated with remote argon plasma and subsequently exposed to oxygen to create peroxides. Peroxides are known to be the species responsible for initiating the graft polymerization when PTFE reacts with AAc. We chose different parameters of remote plasma treatment to get the optimum condition for introducing maximum peroxides (2.87 x 10-11 mol/cm2) on the surface. The influence of grafted reaction conditions on the grafting degree was investigated. The maximum grafting degree was 25.2 μg/cm2. The surface microstructures and compositions of the AAc grafted PTFE film were characterized with the water contact angle meter, Fourier-transform infrared spectroscopy (ATR-FTIR) and X-ray photoelectron spectroscopy (XPS). Contact angle measurements revealed that the water contact angle decreased from 108o to 41o and the surface free energy increased from 22.1 x 10-5 to 62.1 x 10-5 N cm-1 by the grafting of the AAc chains. The hydrophilicity of the PTFE film surface was greatly enhanced. The time-dependent activity of the grafted surface was better than that of the plasma treated film

  18. Synthesis and luminescence properties of dye-doped deoxyribonucleic acid films

    Dye-doped deoxyribonucleic acids (DNA)–tetradecyltrimethylammonium (TTA) films have been prepared. Rhodamine 6G, known as laser dyes, can be spontaneously doped by immersing the DNA–TTA film in rhodamine 6G-acetonitrile solutions. It is surmised that rhodamine 6G monomers and dimers diffuse within the hydrophobic TTA sites, and then monomers presumably intercalate between adjacent base pairs of DNA. Optical absorption spectra reveal that rhodamine 6G molecules in the sample undergo an unusual transformation from the dimer state to the monomer state with the elapse of time. Rhidamine 6G molecules doped in DNA–TTA show enhanced photostability and concentration quenching than those in PMMA. The environment, conformation and chemical stability of rhodamine 6G are different between DNA–TTA and PMMA, and are presumably modified by the intercalation. - Highlights: ► Rhodamine 6G can be spontaneously doped into DNA films by the immersion method. ► Rhodamine 6G molecules undergo an unusual transformation from the dimer to monomer state. ► Rhodamine 6G molecules in DNA films show enhanced photostability and concentration quenching than those in PMMA.

  19. Synthesis and luminescence properties of dye-doped deoxyribonucleic acid films

    Kitazawa, N., E-mail: nkita@nda.ac.jp [Department of Materials Science and Engineering, National Defense Academy, 1-10-20 Hashirimizu, Yokosuka, Kanagawa 239-8686 (Japan); Aroonjaeng, W.; Aono, M.; Watanabe, Y. [Department of Materials Science and Engineering, National Defense Academy, 1-10-20 Hashirimizu, Yokosuka, Kanagawa 239-8686 (Japan)

    2012-06-15

    Dye-doped deoxyribonucleic acids (DNA)-tetradecyltrimethylammonium (TTA) films have been prepared. Rhodamine 6G, known as laser dyes, can be spontaneously doped by immersing the DNA-TTA film in rhodamine 6G-acetonitrile solutions. It is surmised that rhodamine 6G monomers and dimers diffuse within the hydrophobic TTA sites, and then monomers presumably intercalate between adjacent base pairs of DNA. Optical absorption spectra reveal that rhodamine 6G molecules in the sample undergo an unusual transformation from the dimer state to the monomer state with the elapse of time. Rhidamine 6G molecules doped in DNA-TTA show enhanced photostability and concentration quenching than those in PMMA. The environment, conformation and chemical stability of rhodamine 6G are different between DNA-TTA and PMMA, and are presumably modified by the intercalation. - Highlights: Black-Right-Pointing-Pointer Rhodamine 6G can be spontaneously doped into DNA films by the immersion method. Black-Right-Pointing-Pointer Rhodamine 6G molecules undergo an unusual transformation from the dimer to monomer state. Black-Right-Pointing-Pointer Rhodamine 6G molecules in DNA films show enhanced photostability and concentration quenching than those in PMMA.

  20. Ascorbic Acid and BSA Protein in Solution and Films: Interaction and Surface Morphological Structure

    Rafael R. G. Maciel

    2013-01-01

    Full Text Available This paper reports on the study of the interactions between ascorbic acid (AA and bovine serum albumin (BSA in aqueous solution as well as in films (BSA/AA films prepared by the layer-by-layer technique. Regarding to solution studies, a hyperchromism (in the range of ultraviolet was found as a function of AA concentration, which suggested the formation of aggregates from AA and BSA. Binding constant, , determined for aggregates from BSA and AA was found to be about 102 M−1, which indicated low affinity of AA with BSA. For the BSA/AA films, it was also noted that the AA adsorption process and surface morphological structures depended on AA concentration. By changing the contact time between the AA and BSA, a hypochromism was revealed, which was associated to decrease of accessibility of solvent to tryptophan due to formation of aggregates. Furthermore, different morphological structures of aggregates were observed, which were attributed to the diffusion-limited aggregation. Since most of studies of interactions of drugs and proteins are performed in solution, the analysis of these processes by using films can be very valuable because this kind of system is able to employ several techniques of investigation in solid state.

  1. Metal complexes of salicylhydroxamic acid (H2Sha), anthranilic hydroxamic acid and benzohydroxamic acid. Crystal and molecular structure of [Cu(phen)2(Cl)]Cl x H2Sha, a model for a peroxidase-inhibitor complex.

    O'Brien, E C; Farkas, E; Gil, M J; Fitzgerald, D; Castineras, A; Nolan, K B

    2000-04-01

    Stability constants of iron(III), copper(II), nickel(II) and zinc(II) complexes of salicylhydroxamic acid (H2Sha), anthranilic hydroxamic acid (HAha) and benzohydroxamic acid (HBha) have been determined at 25.0 degrees C, I=0.2 mol dm(-3) KCl in aqueous solution. The complex stability order, iron(III) > copper(II) > nickel(II) approximately = zinc(II) was observed whilst complexes of H2Sha were found to be more stable than those of the other two ligands. In the preparation of ternary metal ion complexes of these ligands and 1,10-phenanthroline (phen) the crystalline complex [Cu(phen)2(Cl)]Cl x H2Sha was obtained and its crystal structure determined. This complex is a model for hydroxamate-peroxidase inhibitor interactions. PMID:10830846

  2. Structural, chemical and optical properties of the polyethylene-copper sulfide composite thin films synthesized using polythionic acid as sulfur source

    Ancutiene, Ingrida; Navea, Juan G.; Baltrusaitis, Jonas

    2015-08-01

    Synthesis and properties of thin copper sulfide films deposited on polyethylene were explored for the development of low cost hybrid organic-inorganic photovoltaic materials. Polyethylene was used as a model organic host material for thin copper sulfide film formation. Adsorption-diffusion method was used which utilized consecutive exposure of polyethylene to polythionic acid followed by aqueous Cu(II/I) solution. Several crystalline copper sulfide phases were obtained in synthesized samples and elucidated using X-ray diffraction. Surface chemical composition determined using X-ray photoelectron spectroscopy showed the presence of copper sulfides in combination with copper hydroxide. Thickness of the composite material films ranged from several microns to ∼18 μm and depended on the Cu(II/I) exposure time. Bandgap of the materials obtained was measured and ranged from 1.88 to 1.17 eV. Importantly, heating these complex copper sulfide crystalline phase containing films at 100 °C in inert atmosphere invariably resulted in a single copper sulfide, anilite (Cu1.75S), phase. Anilite possesses a bandgap of 1.36 eV and has demonstrated excellent photovoltaic properties. Thus, the method described in this work can be used for a low cost large scale composite thin film photovoltaic material deposition based on anilite as photoactive material.

  3. A new approach to study cadmium complexes with oxalic acid in soil solution

    This study presents a new analytical approach for the determination of heavy metals complexed to low-molecular-weight-organic acids in soil solutions, which combines the sensitivity of differential pulse anodic stripping voltammetry (DPASV) with the molecular insight gained by electrospray ionization mass spectrometry (ESI-MS). The combination of these analytical methods allows the investigation of such complexes in complex matrixes. On the voltammograms of the soil solutions, in addition to the expected complexes of oxalic acid with cadmium and lead, respectively, also peaks belonging to mixed complexes of cadmium, lead, and oxalic acid (OAH2) were observed. In order to verify the possible formation of complexes with OAH2, aqueous solutions of OAH2 with traces of Cd(II) were investigated as model systems. Signals corresponding to several distinct molecular complexes between cadmium and oxalic acid were detected in the model solutions using negative-ion ESI-MS, which follow the general formula [Cdn(X,Y)(2n+1)]-, where n is the number of cadmium atoms, X = Cl-, and Y = OAH-. Some of these complexes were also identified in the ESI mass spectra taken from the soil solutions.

  4. Studies on photolysis of nitrosyl ruthenium complexes in nitric acid media

    The photolysis of nitrosyl ruthenium complexes in nitric acid media has been investigated in detail using low pressure mercury lamp (254 nm). The UV spectra of nitrosyl ruthenium complexes is also studied. The experimental results show that the photolysis of nitrosyl ruthenium in nitric acid media obeys pseudo-first order kinetics. The rate constant is affected by the concentration of nitric acid and has a maximum at 2 mol/L HNO3. In temperature range from 10 degree C to 40 degree C, the rate constant decreases with the increasing of the temperature

  5. Oxidation of aromatic alcohols on zeolite-encapsulated copper amino acid complexes

    Ernst, S.; Teixeira Florencio, J.M. [Kaiserslautern Univ. (Germany). Dept. of Chemistry, Chemical Technology

    1998-12-31

    Copper complexes of the amino acids histidine, arginine and lysine have been introduced into the supercages of zeolite Y and, for the first time, into the large intracrystalline cavities of zeolites EMT and MCM-22. The resulting host/guest compounds are characterized by X-ray powder diffraction, UV/VIS-spectroscopy in the diffuse reflectance mode and by catalytic tests in the liquid-phase oxidation of aromatic alcohols (viz. benzyl alcohol, 2- and 3-methylbenzyl alcohol and 2,5-dimethylbenzyl alcohol) with tertiary-butylhydroperoxide as oxidant. It was observed that intracrystalline copper-amino acid complexes possess remarkable catalytic activity, yielding the corresponding aromatic aldehydes and acids. (orig.)

  6. Luminescence properties of oxide films formed by anodization of aluminum in 12-tungstophosphoric acid

    In this paper, we have investigated luminescence properties of oxide films formed by anodization of aluminum in 12-tungstophosphoric acid. For the first time we have measured weak luminescence during anodization of aluminum in this electrolyte (so-called galvanoluminescence GL) and showed that there are wide GL bands in the visible region of the spectrum and observed two dominant spectral peaks. The first one is at about 425 nm, and the second one shifts with anodization voltage. As the anodization voltage approaches the breakdown voltage, a large number of sparks appear superimposed on the anodic GL. Several intensive band peaks were observed under breakdown caused by electron transitions in W, P, Al, O, H atoms. Furthermore, photoluminescence (PL) of anodic oxide films and anodic-spark formed oxide coatings were performed. In both cases wide PL bands in the range from 320 nm to 600 nm were observed.

  7. Comparative study of polypyrrole films electrosynthesized in alkaline and acid solutions

    The influence of the pH of electropolymerization solutions on the properties of polypyrrole films has been studied using potentiodynamic techniques and faradaic impedance spectroscopy. Scanning electron microscopy (SEM), IR and Raman spectroscopies, thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC) were also used for products characterization. Results indicate that, contrary to what happen with the polymer electrogenerated in acid solutions, the films prepared in alkaline media are stable and present good electrochemical activity in basic solutions. Possible explanations for the observed differences are discussed and it is proposed that the pH of electropolymerization medium directly affects chains organization. Electrosynthesis in solutions of increased basicity results in a more compact and closed polymer structure.

  8. Aldol Condensation Products and Polyacetals in Organic Films Formed from Reactions of Propanal in Sulfuric Acid at Upper Troposphere/Lower Stratosphere (UT/LS) Aerosol Acidities

    Bui, J. V. H.; Perez-Montano, S.; Li, E. S. W.; Nelson, T. E.; Ha, K. T.; Leong, L.; Iraci, L. T.; Van Wyngarden, A. L.

    2015-12-01

    Aerosols in the upper troposphere and lower stratosphere (UT/LS) consist mostly of concentrated sulfuric acid (40-80 wt. %) which is highly reflective towards UV and visible radiation. However, airborne measurements have shown that these particles may also contain a significant amount of organic material. Experiments combining organics (propanal, glyoxal and/or methylglyoxal) with sulfuric acid at concentrations typical of UT/LS aerosols produced highly colored surface films (and solutions) that have the potential to impact chemical, optical and/or cloud-forming properties of aerosols. In order to assess the potential for such films to impact aerosol chemistry or climate properties, experiments were performed to identify the chemical processes responsible for film formation. Surface films were analyzed via Attenuated Total Reflectance-FTIR and Nuclear Magnetic Resonance spectroscopies and are shown to consist primarily of aldol condensation products and cyclic and linear polyacetals, the latter of which are likely responsible for separation from the aqueous phase.

  9. Structural, spectroscopic and computational studies of the 2:1 complex of nipecotic acid with squaric acid

    Highlights: • Centrosymmetric complex of nipecotic acid with squaric acid. • N–H⋯O hydrogen bonds are dominant in a supromolecular structure. • Isolated 2:1 complexes are optimized by the B3LYP/6-311G(d, p) approach. • NMR spectra suggest the same conformation of piperidinium ring in crystal and solution. • FTIR spectrum confirms a medium strong H-bonds in the solid state. - Abstract: The 2:1 centrosymmetric complex of protonated (R) and (S)-nipecotic acids (piperidinium-3-carboxylic acid) with the squarate dianion (3,4-dihydroxy-3-cyclobuten-1,2-dione) (1), has been synthesized and characterized by single-crystal X-ray analysis, FTIR and NMR spectroscopy. Crystals are monoclinic, space group C2/c, Z′ = 0.5. The squarate dianion lays at the center of symmetry. It is surrounded by six stereoisomers of (R) and (S)-nipecotinium acid cations. The molecules are linked by N–H⋯O and COOH⋯O hydrogen bonds of 2.759(2) and 2.619(2) Å, respectively. The piperidine ring adopts a chair conformation with the carboxylic group in equatorial position. The FTIR spectrum shows a broad and intense absorption in the 3400–2000 cm−1 region, typical of medium–strong N–H⋯O and O–H⋯O hydrogen bonds. The 1H and 13C NMR spectra of the investigated complex confirm the structure of 1 in aqueous solution. Two models of the isolated 2:1 complexes (2 and 3) have been optimized at B3LYP/6-311G(d, p) level of theory to predict the more energetically stable structure. In 2 the molecules are linked by the O–H⋯N and O–H⋯O hydrogen bonds, while in 3 by the N–H⋯O and O–H⋯N hydrogen bonds

  10. Spectroscopic study of the Eu3+, Tb3+ and Gd3+ complexes with ligands derived from dicarboxylic acids

    Complexes of Eu3+, Tb3+ and Gd3+ with dipicolinic acid, chelidamic acid and chelidonic acid have been synthesized in order to study the effect of the substituent groups on the luminescence of the lanthanide complexes. The luminescence of the Eu3+ and Tb3+ complexes was quantified by quantum yield measurements. The complexes of Gd3+ have been used to determine the energies of the triplet states of the ligands. The Tb3+ complex synthesized with dipicolinic acid presented the highest quantum yield due to the energy difference between the triplet state of the dipicolinic acid and the emitting level of the Tb3+ ion. (author)

  11. Studies on some simple and mixed ligated oxovanadium(V) complexes of hydroxamic acids

    Some simple and mixed ligands complexes of oxovanadium(V) with benzo-, and salicyl-hydroxamic acids as primary ligands and 2,2-bipyridine and 1,10-phenanthroline as secondary ligands have been prepared and characterised. The structures of the complexes have been assigned on the basis of electronic and infra red spectral data. The IR spectra of the simple complexes reveal the bidentate nature of the primary ligands, whereas in the mixed complexes these ligands exhibit monodentate nature. Magnetic moment studies show that the complexes are diamagnetic. (author). 13 refs., 1 tab., 1 fig

  12. Laser-induced periodic surface structures of thin, complex multi-component films

    Reif, Juergen; Varlamova, Olga; Ratzke, Markus; Uhlig, Sebastian

    2016-04-01

    Femtosecond laser-induced regular nanostructures are generated on a complex multilayer target, namely a piece of a commercial, used hard disk memory. It is shown that after single-shot 800-nm irradiation at 0.26 J/cm2 only the polymer cover layer and—in the center—a portion of the magnetic multilayer are ablated. A regular array of linearly aligned spherical 450-nm features at the uncovered interface between cover and magnetic layers appears not to be produced by the irradiation. Only after about 10 pulses on one spot, classical ripples perpendicular to the laser polarization with a period of ≈700 nm are observed, with a modulation between 40 nm above and 40 nm below the pristine surface and an ablation depth only slightly larger than the thickness of the multilayer magnetic film. Further increase of the pulse number does not result in deeper ablation. However, 770-nm ripples become parallel to the polarization and are swelling to more than 120 nm above zero, much more than the full multilayer film thickness. In the spot periphery, much shallower 300-nm ripples are perpendicular to the strong modulation and the laser polarization. Irradiation with 0.49-J/cm2 pulses from an ultrafast white-light continuum results—in the spot periphery—in the formation of 200-nm ripples, only swelling above zero after removal of the polymer cover, without digging into the magnetic film.

  13. High Throughput Screening of Valganciclovir in Acidic Microenvironments of Polyester Thin Films

    Teilo Schaller

    2015-04-01

    Full Text Available Ganciclovir and valganciclor are antiviral agents used for the treatment of cytomegalovirus retinitis. The conventional method for administering ganciclovir in cytomegalovirus retinitis patients is repeated intravitreal injections. In order to obviate the possible detrimental effects of repeated intraocular injections, to improve compliance and to eliminate systemic side-effects, we investigated the tuning of the ganciclovir pro-drug valganciclovir and the release from thin films of poly(lactic-co-glycolic acid (PLGA, polycaprolactone (PCL, or mixtures of both, as a step towards prototyping periocular valganciclovir implants. To investigate the drug release, we established and evaluated a high throughput fluorescence-based quantification screening assay for the detection of valganciclovir. Our protocol allows quantifying as little as 20 ng of valganciclovir in 96-well polypropylene plates and a 50× faster analysis compared to traditional HPLC measurements. This improvement can hence be extrapolated to other polyester matrix thin film formulations using a high-throughput approach. The acidic microenvironment within the polyester matrix was found to protect valganciclovir from degradation with resultant increases in the half-life of the drug in the periocular implant to 100 days. Linear release profiles were obtained using the pure polyester polymers for 10 days and 60 days formulations; however, gross phase separations of PCL and acid-terminated PLGA prevented tuning within these timeframes due to the phase separation of the polymer, valganciclovir, or both.

  14. Immobilization of Tyrosinase from Avocado Crude Extract in Polypyrrole Films for Inhibitive Detection of Benzoic Acid

    André Brisolari

    2014-07-01

    Full Text Available Inhibition-based biosensors were developed by immobilizing tyrosinase (Tyr, polyphenol oxidase from the crude extract of avocado fruit on electrochemically prepared polypyrrole (PPy films. The biosensors were prepared during the electropolymerization of pyrrole in a solution containing a fixed volume of the crude extract of avocado. The dependence of the biosensor responses on the volume used from the crude extract, values of pH and temperature was studied, and a substrate, catechol, at different concentrations, was amperometrically detected by these biosensors. Benzoic acid, a competitive inhibitor of Try, was added to the catechol solutions at specific concentrations aimed at obtaining the inhibition constant, K’m, which ranged from 1.7 to 4.6 mmol∙L−1 for 0.0 and 60 µmol∙L−1 of benzoic acid, respectively. Studies on the inhibition caused by benzoic acid by using PPy/Try films, and catechol as a substrate, allowed us propose how to develop, under optimized conditions, simple and low-cost biosensors based on the use of avocado fruit.

  15. Database of amino acid-nucleotide contacts in the DNA complexes with homeodomain family proteins

    The analysis of amino acid-nucleotide contacts in interfaces of the protein-DNA complexes, intended to find consistencies in the protein-DNA recognition, is a complex problem that requires analysis of the physicochemical characteristics of these contacts, of the positions of the participating amino acids and nucleotides in the chains of the protein and the DNA, respectively, as well as conservatism of these contacts. Thus, those heterogeneous data should be systematized. For this purpose we have developed a database of amino acid-nucleotide contacts ANTPC (Amino acid Nucleotide Type Position Conservation) following the archetypal example of the proteins in the homeodomain family. We show that it can be used for comparison and classification of interfaces of the protein-DNA complexes

  16. Novel rhenium(V) complexes with thiosemicarbazones of pyruvic or phenylglyoxylic acids

    New rhenium(V) complexes with thiosemicarbazones of pyruvic (L') or phenylglyoxylic (L'') acids were synthesized and isolated in solid state in aqueous solutions of concentrated hydrohalic acids. By the method of elementary analysis formation of complexes, featuring the following composition [ReOL'Cl3]·2H2O, [ReOL''2Br]Br2·2H2O, [ReOL'Br2(OH)]·2H2O, [ReOL''2(OH)]Cl·2H2O, [Re2O3L'2Cl4]·2H2O, was ascertained. Solubility of the complexes in organic solvents was determined

  17. State and dissociation mechanisms of mixed-ligand acidoporphyrin complexes of metals in sulfuric acid solutions

    Dissociation of indium complexes with tetraphenylporphyrin (H2 TPP) and complexes (Cl)In TPP(X)4, where TPP(X)42--dianion of TPP substituted in para-positions of phenyls with OCH3, Br, NO2 groups, in sulfuric acid solutions has been studied by spectrophotometric method. It is shown that complex (Cl)In TPP associated with proton of the solvent dissociates by multistage mechanism, protolytic dissociation of metalloporphyrin under the effect of sulfuric acid molecules being the limiting stage of the process. Proton associated with metalloporphyrin produces inhibiting effect on dissociation

  18. Characterization of folic acid/native cyclodextrins host-guest complexes in solution

    Ceborska, Magdalena; Zimnicka, Magdalena; Wszelaka-Rylik, Małgorzata; Troć, Anna

    2016-04-01

    The complexation of folic acid (FA) with native cyclodextrins was studied and this process was used for the comparison of 1H NMR, ITC and ESIMS for the evaluation of association constants. The stability increases in the series: α-cyclodextrin/FA complexes. The dimerization of FA in water was also studied, as well as its impact on the process of complexation with native cyclodextrins.

  19. Hydrolytic activity of -alkoxide/acetato-bridged binuclear Cu(II) complexes towards carboxylic acid ester

    Weidong Jiang; Bin Xu; Zhen Xiang; Shengtian Huang; Fuan Liu; Ying Wang

    2013-09-01

    Two -alkoxide/acetate-bridged small molecule binuclear copper(II) complexes were synthesized, and used to promote the hydrolysis of a classic carboxylic acid ester, -nitrophenyl picolinate (PNPP). Both binuclear complexes exhibited good hydrolytic reactivity, giving rise to . 15547- and 17462-fold acceleration over background value for PNPP hydrolysis at neutral conditions, respectively. For comparing, activities of the other two mononuclear analogues were evaluated, revealing that binuclear complexes show approximately 150- and 171-fold kinetic advantage over their mononuclear analogues.

  20. Reactions of certain acids with ammoniac 1,2,4-triazole complexes of rhenium (5)

    The process of interaction of formic, acetic, hydrofluoric and sulfuric acids with ammoniac-1,2,4-triazole complexes of rhenium (5) was studied. The complexes [Re2O3(OH)2L2X2(H2O)2], where X=CH3COO, HCOO, F; L=1,2,4-triazole, and [Re2O2(SO4)3L2(H2O)2] were synthesized. The properties of the complexes prepared were characterized by physicochemical methods

  1. Leaching of complex sulphide concentrate in acidic cupric chloride solutions

    M. TCHOUMOU; M. ROYNETTE

    2007-01-01

    The chemical analysis of a complex sulphide concentrate by emission spectrometry and X-ray diffraction shows that it contains essentially copper, lead, zinc and iron in the form of chalcopyrite, sphalerite and galena. A small amount of pyrite is also present in the ore but does not be detected with X-ray diffraction. The cupric chloride leaching of the sulphide concentrate at various durations and solid/liquid ratios at 100 ℃ shows that the rate of dissolution of the ore is the fastest in the first several hours, and after 12 h it does not evolve significantly. If oxygen is excluded from the aqueous cupric chloride solution during the leaching experiment at 100 ℃, the pyrite in the ore will not be leached. The determination of principal dissolved metals in the leaching liquor by flame atomic absorption spectrometry, and the chemical analysis of solid residues by emission spectrometry and X-ray diffraction allow to conclude that the rate of dissolution of the minerals contained in the complex sulphide concentrate are in the order of galena>sphalerite>chalcopyrite.

  2. Characterization of humic acids and humate complexation of Am(III)

    The characterization of selected humic acids and the humate complexation behaviour of Am(III) are described. The commercial humic acid (Na salt) from Aldrich Co. is purified to a protonated form and used as a reference material. Humic and fulvic acids extracted and purified from Gorleben groundwaters (FRG) are taken as site specific materials. The characterization of the reference and site specific materials shows that they have very similar chemical properties and represent typical humic acids as known in the literature. By considering the humic acids as ion-exchangers and taking their loading capacity into account, the complexation constant of Am(III) is determined. The thus determined constant is found to be independent of pH and ionic strength. (orig.)

  3. Metal complexation inhibits the effect of oxalic acid in aerosols as cloud condensation nuclei (CCN

    T. Furukawa

    2010-11-01

    Full Text Available Atmospheric aerosols have both a direct and an indirect cooling effect that influences the radiative balance at the Earth's surface. It has been estimated that the degree of cooling is large enough to cancel the warming effect of carbon dioxide. Among the cooling factors, secondary organic aerosols (SOA play a key role in the solar radiation balance in the troposphere as SOA can act as cloud condensation nuclei (CCN and extend the lifespan of clouds because of their high hygroscopic and water soluble nature. Oxalic acid is one of the major components of SOA, and is produced via several formation pathways in the atmosphere. However, it is not certain whether oxalic acid exists as free oxalic acid or as metal oxalate complexes in aerosols, although there is a marked difference in their solubility in water and their hygroscopicity. We employed X-ray absorption fine structure spectroscopy to characterize the calcium (Ca and zinc (Zn in aerosols collected at Tsukuba in Japan with fractionation based on particle size using an impactor aerosol sampler. It was shown that 10–60% and 20–100% of the total Ca and Zn in the finer particles (<2.1 μm were present as Ca and Zn oxalate complexes, respectively. Oxalic acid can act as CCN because of its hygroscopic properties, while metal complexes are not hygroscopic, and so cannot be CCN. Based on the concentration of noncomplexed and metal-complexed oxalate species, we found that most of the oxalic acid is present as metal oxalate complexes in the aerosols, suggesting that oxalic acid does not act as CCN in the atmosphere. Similar results are expected for other dicarboxylic acids, such as malonic and succinic acids. Thus, it is possible that the cooling effect of organic aerosols assumed in various climate modeling studies is overestimated because of the lack of information on metal oxalate complexes in aerosols.

  4. Determination of stability constants of the Co(II) complexes with weathered coal fulvic acid

    The stability constants of Co(II) complexes with weathered coal fulvic acid are determined by both Schubert method and Stevenson method at pH = 5.3 +- 0.2, I = 0.001-1.0 mol/kg and (30 +- 1) degree C. The modified Schubert method is also used to estimate the stability constants of Co(II) complexes with the fulvic acid. It is shown that the trend of forming poly nuclei complexes of Co(II)-fulvic acid increases with increasing ionic strength in the solution and that 1:1 and 2:1 type complexes, respectively, are formed at different ionic strength. A comparison between the values of lg β obtained by different methods is made

  5. A method for the determination of ascorbic acid using the iron(II)-pyridine-dimethylglyoxime complex

    A simple and rapid spectrophotometric method for the determination of ascorbic acid is proposed. Ascorbic acid reduces iron (III) to iron (II) which forms a red colored complex with dimethylglyoxime in the presence of pyridine. The absorbance of the resulting solution is measured at 514 nm and a linear relationship between absorbance and concentration of ascorbic acid is observed up to 14 μg ml-1. Studies on the interference of substances usually associated with ascorbic acid have been carried out and the applicability of the method has been tested by analysing pharmaceutical preparations of vitamin C

  6. Synthesis, spectral studies and biological evaluation of 2-aminonicotinic acid metal complexes

    Nawaz, Muhammad; Abbasi, Muhammad Waseem; Hisaindee, Soleiman; Zaki, Muhammad Javed; Abbas, Hira Fatima; Mengting, Hu; Ahmed, M. Arif

    2016-05-01

    We synthesized 2-aminonicotinic acid (2-ANA) complexes with metals such as Co(II), Fe(III), Ni(II), Mn(II), Zn(II), Ag(I),Cr(III), Cd(II) and Cu(II) in aqueous media. The complexes were characterized and elucidated using FT-IR, UV-Vis, a fluorescence spectrophotometer and thermo gravimetric analysis (TGA). TGA data showed that the stoichiometry of complexes was 1:2 metal/ligand except for Ag(I) and Mn(II) where the ratio was 1:1. The metal complexes showed varied antibacterial, fungicidal and nematicidal activities. The silver and zinc complexes showed highest activity against Bacillus subtilis and Bacillus licheniformis respectively. Fusarium oxysporum was highly susceptible to nickel and copper complexes whereas Macrophomina phaseolina was completely inert to the complexes. The silver and cadmium complexes were effective against the root-knot nematode Meloidogyne javanica.

  7. Effect of acetic acid on electrochemical deposition of carbon-nitride thin film

    2009-01-01

    Electrochemical deposition method was employed to prepare CNx thin film from methanol-urea solution,and it was shown that adding a little acetic acid in the solution significantly affected the deposition process.After optimizing the experiment conditions,we obtained polycrystalline grains with sizes of about 3―7μm on the faces of single crystal silicon.X-ray diffraction spectrua indicate that the grains are mainly composed of cubic phase mixed with a small amount of β and α phases.

  8. Rapid thermal annealing of spin-coated phosphoric acid films for shallow junction formation

    Sivoththaman, S.; Laureys, W.; Nijs, J.; Mertens, R.

    1997-07-01

    Rapid thermal annealing (RTA) of spin-coated phosphoric acid (H3PO4) films on silicon substrates has been studied for the formation of shallow junctions. The junctions are characterized by spreading resistance profiling. Device quality, shallow (750 °C), below which absorption bands originating from water species are noted. More than 15% efficient, shallow emitter, large-area (10 cm×10 cm) n+pp+ silicon solar cells are fabricated with a short-time processing using this rapid thermal processing technique.

  9. New composite systems on the base of polyethylene porous films covered by polypyrrole and polyacrylic acid

    Elyashevich, G. K.; Rosova, E. Yu.; Andreeva, D. V.; Polotskaya, G. A.; Trchová, Miroslava; Pientka, Zbyněk

    2005-01-01

    Roč. 97, č. 4 (2005), s. 1410-1417. ISSN 0021-8995 R&D Projects: GA ČR GA202/02/0698 Grant ostatní: Russian Foundation of Basic Research(RU) 01-03-32290; Russian Foundation of Basic Research(RU) 04-03-32229 Institutional research plan: CEZ:AV0Z40500505 Keywords : porous polyethylene films * polypyrrole * polyacrylic acid Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 1.072, year: 2005

  10. Structure and properties of moisture-resistant konjac glucomannan films coated with shellac/stearic acid coating.

    Wei, Xueqin; Pang, Jie; Zhang, Changfeng; Yu, Chengcheng; Chen, Han; Xie, Bingqing

    2015-03-15

    A series of moisture-resistant konjac glucomannan films were prepared by coating shellac/stearic acid emulsion on deacetylated konjac glucomannan films (dKGM). The effect of stearic acid content on structure and properties of the coated films were investigated by field emission scanning electron microscopy (FE SEM), Fourier transform infrared spectroscopy (FT-IR), ultraviolet spectroscopy (UV), water vapor permeability (WVP), water uptake, water contact angle, and tensile testing. The results revealed that shellac in the coating adhered intimately to the surface of dKGM film, and provided a substrate for the dispersion of stearic acid which played an important role in enhancement of the moisture barrier properties and mechanical properties of the coated films. The WVP of the coated films decreased from 2.63×10(-11) to 0.37×10(-11)g/(msPa) and the water contact angle increased from 68° to 101.2° when stearic acid content increased from 0wt% to 40wt%, showing the potential applications in food preservation. PMID:25542116

  11. Dye sensitized solar cell applications of CdTiO3–TiO2 composite thin films deposited from single molecular complex

    A heterobimetallic complex [Cd2Ti4(μ-O)6(TFA)8(THF)6]·1.5THF (1) (TFA=trifluoroacetato, THF=tetrahydrofuran) comprising of Cd:Ti (1:2) ratio was synthesized by a chemical reaction of cadmium (II) acetate with titanium (IV) isopropoxide and triflouroacetic acid in THF. The stoichiometry of (1) was recognized by single crystal X-ray diffraction, spectroscopic and elemental analyses. Thermal studies revealed that (1) neatly decomposes at 450 °C to furnish 1:1 ratio of cadmium titanate:titania composite oxides material. The thin films of CdTiO3–TiO2 composite oxides were deposited at 550 °C on fluorine doped tin oxide coated conducting glass substrate in air ambient. The micro-structure, crystallinity, phase identification and chemical composition of microspherical architectured CdTiO3–TiO2 composite thin film have been determined by scanning electron microscopy, X-ray diffraction, Raman spectroscopy and energy dispersive X-ray analysis. The scope of composite thin film having band gap of 3.1 eV was explored as photoanode for dye-sensitized solar cell application. - Graphical abstarct: Microspherical designed CdTiO3–TiO2 composite oxides photoanode film has been fabricated from single source precursor [Cd2Ti4(μ-O)6(TFA)8(THF)6]·1.5THF via aerosol assisted chemical vapor deposition technique for dye sensitized solar cell application. - Highlights: • Synthesis and characterization of a heterobimetallic Cd–Ti complex. • Fabrication of CdTiO3–TiO2 thin film photoelectrode. • Application as dye sensitized photoanode for solar application

  12. Dye sensitized solar cell applications of CdTiO{sub 3}–TiO{sub 2} composite thin films deposited from single molecular complex

    Ehsan, Muhammad Ali [Nanotechnology and Catalysis Centre (NANOCAT), University of Malaya, Lembah Pantai, 50603 Kuala Lumpur (Malaysia); Khaledi, Hamid [Department of Chemistry, Faculty of Science, University of Malaya, Lembah Pantai, 50603 Kuala Lumpur (Malaysia); Pandikumar, Alagarsamy; Huang, Nay Ming [Department of Physics, Faculty of Science, University of Malaya, Lembah Pantai, 50603 Kuala Lumpur (Malaysia); Arifin, Zainudin [Department of Chemistry, Faculty of Science, University of Malaya, Lembah Pantai, 50603 Kuala Lumpur (Malaysia); Mazhar, Muhammad, E-mail: mazhar42pk@yahoo.com [Department of Chemistry, Faculty of Science, University of Malaya, Lembah Pantai, 50603 Kuala Lumpur (Malaysia)

    2015-10-15

    A heterobimetallic complex [Cd{sub 2}Ti{sub 4}(μ-O){sub 6}(TFA){sub 8}(THF){sub 6}]·1.5THF (1) (TFA=trifluoroacetato, THF=tetrahydrofuran) comprising of Cd:Ti (1:2) ratio was synthesized by a chemical reaction of cadmium (II) acetate with titanium (IV) isopropoxide and triflouroacetic acid in THF. The stoichiometry of (1) was recognized by single crystal X-ray diffraction, spectroscopic and elemental analyses. Thermal studies revealed that (1) neatly decomposes at 450 °C to furnish 1:1 ratio of cadmium titanate:titania composite oxides material. The thin films of CdTiO{sub 3}–TiO{sub 2} composite oxides were deposited at 550 °C on fluorine doped tin oxide coated conducting glass substrate in air ambient. The micro-structure, crystallinity, phase identification and chemical composition of microspherical architectured CdTiO{sub 3}–TiO{sub 2} composite thin film have been determined by scanning electron microscopy, X-ray diffraction, Raman spectroscopy and energy dispersive X-ray analysis. The scope of composite thin film having band gap of 3.1 eV was explored as photoanode for dye-sensitized solar cell application. - Graphical abstarct: Microspherical designed CdTiO{sub 3}–TiO{sub 2} composite oxides photoanode film has been fabricated from single source precursor [Cd{sub 2}Ti{sub 4}(μ-O){sub 6}(TFA){sub 8}(THF){sub 6}]·1.5THF via aerosol assisted chemical vapor deposition technique for dye sensitized solar cell application. - Highlights: • Synthesis and characterization of a heterobimetallic Cd–Ti complex. • Fabrication of CdTiO{sub 3}–TiO{sub 2} thin film photoelectrode. • Application as dye sensitized photoanode for solar application.

  13. Synthesis and characterization of electrochromic plate-like tungsten oxide films by acidic treatment of electrochemical anodized tungsten

    Highlights: • Plate-like WO3·2H2O films were prepared by electrochemical anodization followed by acidic treatment. • The enhanced electrochromic properties of the films were caused by their high surface area. • The WO3 films demonstrated electrochemical stability after the first 100 cycles. - Abstract: Tungsten films on ITO glass were anodized into a porous amorphous WO3 film morphology at 60 V. The follow-up acidic treatment of the anodized WO3 films in H2SO4 solution transformed the morphology into plate-like WO3·2H2O. Glancing incident X-ray diffraction and Raman scattering spectra indicated that the growth of plate-like WO3·2H2O films was caused by a dissolution–precipitation reaction in H2SO4 solution. The plate-like WO3·2H2O transformed into monoclinic WO3 by dehydration at 400 °C, and it collapsed into a dense particle-like one at 500 °C due to the strain of dehydration. Due to its highly porous plate-like morphology, the 400 °C-annealed WO3 film has the highest optical modulation of 52% and coloration efficiency of 71 cm2/C at 633 nm

  14. Amino acid detection using fluoroquinolone–Cu2+ complex as a switch-on fluorescent probe by competitive complexation without derivatization

    In this work, we describe the use of fluoroquinolone–Cu2+ complex as a competitive switch-on fluorescence probe for amino acid determination without derivatization. The fluorescence intensity of this probe, which has been reduced due to effective quenching by Cu2+ ion, increases drastically by an addition of amino acid (glycine, phenylalanine, sarcosine, aspargine, alanine, proline, arginine, aspartic acid, glutamic acid, lysine, leucine and isoleucine). The overall stability constants of Cu2+ ion complexes with amino acids were determined by fluorometric titration of fluoroquinolone-Cu2+ complex with the amino acid solution. Furthermore, the probe shows high calibration sensitivity toward aspartic acid. The fluorescence signal depends linearly on the amino acid concentration within the range of concentration from 1.2×10−7 to 1.1×10−5 mol L−1 for aspartic acid. The detection limit was found 2.7×10−8 mol L−1 with the relative standard deviation (RSD%) about 2.1% (five replicate). -- Highlights: • Amino acids are detected by using fluoroquinolone–Cu2+ complex as fluorescent probe. • Amino acids were detected based on a competitive complexation reaction. • Probe has been able to recognize amino acids through switch-on fluorescence behavior. • Ultra-trace level of aspartic and glutamic acid is determined without derivatization

  15. Amino acid detection using fluoroquinolone–Cu{sup 2+} complex as a switch-on fluorescent probe by competitive complexation without derivatization

    Farokhcheh, Alireza; Alizadeh, Naader, E-mail: alizaden@modares.ac.ir

    2014-01-15

    In this work, we describe the use of fluoroquinolone–Cu{sup 2+} complex as a competitive switch-on fluorescence probe for amino acid determination without derivatization. The fluorescence intensity of this probe, which has been reduced due to effective quenching by Cu{sup 2+} ion, increases drastically by an addition of amino acid (glycine, phenylalanine, sarcosine, aspargine, alanine, proline, arginine, aspartic acid, glutamic acid, lysine, leucine and isoleucine). The overall stability constants of Cu{sup 2+} ion complexes with amino acids were determined by fluorometric titration of fluoroquinolone-Cu{sup 2+} complex with the amino acid solution. Furthermore, the probe shows high calibration sensitivity toward aspartic acid. The fluorescence signal depends linearly on the amino acid concentration within the range of concentration from 1.2×10{sup −7} to 1.1×10{sup −5} mol L{sup −1} for aspartic acid. The detection limit was found 2.7×10{sup −8} mol L{sup −1} with the relative standard deviation (RSD%) about 2.1% (five replicate). -- Highlights: • Amino acids are detected by using fluoroquinolone–Cu{sup 2+} complex as fluorescent probe. • Amino acids were detected based on a competitive complexation reaction. • Probe has been able to recognize amino acids through switch-on fluorescence behavior. • Ultra-trace level of aspartic and glutamic acid is determined without derivatization.

  16. Formation and characterization of thin films from phthalocyanine complexes: An electrosynthesis study using the atomic-force microscope

    (μ-Cyano)(phthalocyaninato)metal(III) [PcMCN]n species with a central transition metal ion, such as Fe(III) and Co(III), were used to prepare molecular films on a highly oriented pyrolytic graphite electrode substrate by using the cyclic voltammetry technique. In order to investigate the influence of the ligand on the film properties, 1,8-dihydroxyanthraquinone and 2,6-dihydroxyanthraquinone as bivalent ligands were employed. The structure of the molecular materials was analyzed by infrared spectroscopy. The in situ film formation, texture, composition and conductivity of each film were further investigated using atomic force microscopy, scanning electron microscopy, energy-dispersive X-ray spectroscopy and the four-probe technique, respectively. The [PcMCN]n complexes provided conductive films with an electrical conductivity of 1 x 10-6 Ω-1 cm-1 at 298 K

  17. Formation and characterization of thin films from phthalocyanine complexes: An electrosynthesis study using the atomic-force microscope

    Sanchez Vergara, M.E. [Departamento de Ingenieria Mecatronica, Escuela de Ingenieria, Universidad Anahuac del Norte, Avenida Lomas de la Anahuac s/n, Col. Lomas Anahuac, 52786, Huixquilucan (Mexico)]. E-mail: elena.sanchez@anahuac.mx; Islas Bernal, I.F. [Instituto de Fisica, Universidad Nacional Autonoma de Mexico, Circuito Exterior, Ciudad Universitaria, 04510, Mexico D.F. (Mexico); Rivera, M. [Instituto de Fisica, Universidad Nacional Autonoma de Mexico, Circuito Exterior, Ciudad Universitaria, 04510, Mexico D.F. (Mexico); Ortiz Rebollo, A. [Instituto de Investigaciones en Materiales, Universidad Nacional Autonoma de Mexico, A.P. 70-360, Coyoacan, 04510, Mexico, D.F. (Mexico); Alvarez Bada, J.R. [Instituto Tecnologico y de Estudios Superiores de Monterrey, Campus Ciudad de Mexico, Calle del Puente 222, Col. Ejidos de Huipulco, 14380, Mexico D.F. (Mexico)

    2007-05-07

    ({mu}-Cyano)(phthalocyaninato)metal(III) [PcMCN]{sub n} species with a central transition metal ion, such as Fe(III) and Co(III), were used to prepare molecular films on a highly oriented pyrolytic graphite electrode substrate by using the cyclic voltammetry technique. In order to investigate the influence of the ligand on the film properties, 1,8-dihydroxyanthraquinone and 2,6-dihydroxyanthraquinone as bivalent ligands were employed. The structure of the molecular materials was analyzed by infrared spectroscopy. The in situ film formation, texture, composition and conductivity of each film were further investigated using atomic force microscopy, scanning electron microscopy, energy-dispersive X-ray spectroscopy and the four-probe technique, respectively. The [PcMCN]{sub n} complexes provided conductive films with an electrical conductivity of 1 x 10{sup -6} {omega}{sup -1} cm{sup -1} at 298 K.

  18. An Amperometric Biosensor for Uric Acid Determination Prepared From Uricase Immobilized in Polyaniline-Polypyrrole Film

    Fatma Arslan

    2008-09-01

    Full Text Available A new amperometric uric acid biosensor was developed by immobilizing uricase by a glutaraldehyde crosslinking procedure on polyaniline-polypyrrole (pani-ppy composite film on the surface of a platinum electrode. Determination of uric acid was performed by the oxidation of enzymatically generated H2O2 at 0.4 V vs. Ag/AgCl. The linear working range of the biosensor was 2.5×10-6 – 8.5×10-5 M and the response time was about 70 s. The effects of pH, temperature were investigated and optimum parameters were found to be 9.0, 55 oC, respectively. The stability and reproducibility of the enzyme electrode have been also studied.

  19. Phosphorescent emissions of phosphine copper(I) complexes bearing 8-hydroxyquinoline carboxylic acid analogue ligands

    The pseudotetrahedral complexes of [Cu(PPh3)2(L)], where L=8-hydroxy-2-methylquinoline-7-carboxylic acid (1), 8-hydroxy-2,5-dimethylquinoline-7-carboxylic acid (2) or 5-chloro-8-hydroxy-2-methylquinoline-7-carboxylic acid (3) have been synthesized and structurally characterized by X-ray crystallography. Their properties have been examined through combinations of IR, NMR, electronic absorption spectroscopy and cyclic voltammetry. The complexes exhibit extraordinary photophysical properties. Complex (1) in solid state exhibits an emission quantum yield of 4.67% and an excited life time of 1.88 ms (frozen DCM solution up to 6.7 ms). When dissolved in a coordinating solvent (acetonitrile) the charge transfer emission was quenched on a microsecond scale. - Highlights: • Synthesis of copper(I) complexes with 8-hydroxyquinoline carboxylic acid ligands. • Very long lived phosphorescent copper(I) complexes. • [Cu(PPh3)2(L)] where L=8-hydroxy-2-methylquinoline-7-carboxylic acid luminesce in the solid state exhibits extremely long lifetime on millisecond scale (1.9 ms). • In frozen MeOH:EtOH solution lifetime increases to 7 ms. • Quantum efficiency equal to 4.7%

  20. Phosphorescent emissions of phosphine copper(I) complexes bearing 8-hydroxyquinoline carboxylic acid analogue ligands

    Małecki, Jan G., E-mail: gmalecki@us.edu.pl [Department of Crystallography, Institute of Chemistry, University of Silesia, Szkolna 9 street, 40-006 Katowice (Poland); Łakomska, Iwona, E-mail: iwolak@chem.umk.pl [Department of Chemistry, Nicolaus Copernicus University, Toruń (Poland); Maroń, Anna [Department of Crystallography, Institute of Chemistry, University of Silesia, Szkolna 9 street, 40-006 Katowice (Poland); Szala, Marcin [Institute of Chemistry, University of Silesia, ul. Szkolna 9, 40-006 Katowice (Poland); Fandzloch, Marzena [Department of Chemistry, Nicolaus Copernicus University, Toruń (Poland); Nycz, Jacek E., E-mail: jacek.nycz@us.edu.pl [Institute of Chemistry, University of Silesia, ul. Szkolna 9, 40-006 Katowice (Poland)

    2015-05-15

    The pseudotetrahedral complexes of [Cu(PPh{sub 3}){sub 2}(L)], where L=8-hydroxy-2-methylquinoline-7-carboxylic acid (1), 8-hydroxy-2,5-dimethylquinoline-7-carboxylic acid (2) or 5-chloro-8-hydroxy-2-methylquinoline-7-carboxylic acid (3) have been synthesized and structurally characterized by X-ray crystallography. Their properties have been examined through combinations of IR, NMR, electronic absorption spectroscopy and cyclic voltammetry. The complexes exhibit extraordinary photophysical properties. Complex (1) in solid state exhibits an emission quantum yield of 4.67% and an excited life time of 1.88 ms (frozen DCM solution up to 6.7 ms). When dissolved in a coordinating solvent (acetonitrile) the charge transfer emission was quenched on a microsecond scale. - Highlights: • Synthesis of copper(I) complexes with 8-hydroxyquinoline carboxylic acid ligands. • Very long lived phosphorescent copper(I) complexes. • [Cu(PPh{sub 3}){sub 2}(L)] where L=8-hydroxy-2-methylquinoline-7-carboxylic acid luminesce in the solid state exhibits extremely long lifetime on millisecond scale (1.9 ms). • In frozen MeOH:EtOH solution lifetime increases to 7 ms. • Quantum efficiency equal to 4.7%.

  1. A complex of equine lysozyme and oleic acid with bactericidal activity against Streptococcus pneumoniae.

    Emily A Clementi

    Full Text Available HAMLET and ELOA are complexes consisting of oleic acid and two homologous, yet functionally different, proteins with cytotoxic activities against mammalian cells, with HAMLET showing higher tumor cells specificity, possibly due to the difference in propensity for oleic acid binding, as HAMLET binds 5-8 oleic acid molecules per protein molecule and ELOA binds 11-48 oleic acids. HAMLET has been shown to possess bactericidal activity against a number of bacterial species, particularly those with a respiratory tropism, with Streptococcus pneumoniae displaying the greatest degree of sensitivity. We show here that ELOA also displays bactericidal activity against pneumococci, which at lower concentrations shows mechanistic similarities to HAMLET's bactericidal activity. ELOA binds to S. pneumoniae and causes perturbations of the plasma membrane, including depolarization and subsequent rupture, and activates an influx of calcium into the cells. Selective inhibition of calcium channels and sodium/calcium exchange activity significantly diminished ELOA's bactericidal activity, similar to what we have observed with HAMLET. Finally, ELOA-induced death was also accompanied by DNA fragmentation into high molecular weight fragments - an apoptosis-like morphological phenotype that is seen during HAMLET-induced death. Thus, in contrast to different mechanisms of eukaryote cell death induced by ELOA and HAMLET, these complexes are characterized by rather similar activities towards bacteria. Although the majority of these events could be mimicked using oleic acid alone, the concentrations of oleic acid required were significantly higher than those present in the ELOA complex, and for some assays, the results were not identical between oleic acid alone and the ELOA complex. This indicates that the lipid, as a common denominator in both complexes, is an important component for the complexes' bactericidal activities, while the proteins are required both to solubilize

  2. Trifluoroacetic acid as excipient destabilizes melittin causing the selective aggregation of melittin within the centrin-melittin-trifluoroacetic acid complex

    Belinda Pastrana-Rios

    2015-07-01

    Full Text Available Trifluoroacetic acid (TFA may be the cause of the bottleneck in high resolution structure determination for protein-peptide complexes. Fragment based drug design often involves the use of synthetic peptides which contain TFA (excipient. Our goal was to explore the effects of this excipient on a model complex: centrin-melittin-TFA. We performed Fourier transform infrared, two-dimensional infrared correlation spectroscopies and spectral simulations to analyze the amide I'/I'* band for the components and the ternary complex. Melittin (MLT was observed to have increased helicity upon its interaction with centrin, followed by the thermally induced aggregation of MLT within the ternary complex in the TFA presence.

  3. Chitosan-bound pyridinedicarboxylate Ni(II) and Fe(III) complex biopolymer films as waste water decyanidation agents.

    Adewuyi, Sheriff; Jacob, Julianah Modupe; Olaleye, Oluwatoyin Omolola; Abdulraheem, Taofiq Olanrewaju; Tayo, Jubril Ayopo; Oladoyinbo, Fatai Oladipupo

    2016-10-20

    Chitosan is a biopolymer with immense structural advantage for chemical and mechanical modifications to generate novel properties, functions and applications. This work depicts new pyridinedicarboxylicacid (PDC) crosslinked chitosan-metal ion films as veritable material for cyanide ion removal from aqueous solution. The PDC-crosslinked chitosan-metal films (PDC-Chit-Ni(II) and PDC-Chit-Fe(III)) were formed by complexing PDC-crosslinked chitosan film with anhydrous nickel(II) and iron(III) chloride salts respectively. The PDC-Chit and its metal films were characterized employing various analytical and spectroscopic techniques. The FT-IR, UV-vis and the XRD results confirm the presence of the metal ions in the metal coordinated PDC-crosslinked chitosan film. The surface morphological difference of PDC-Chit-Ni(II) film before and after decyanidation was explored with scanning electron microscopy. Furthermore, the quantitative amount of nickel(II) and iron(III) present in the complex were determined using Atomic Absorption Spectrophotometer as 32.3 and 37.2μg/g respectively which portends the biopolymer film as a good complexing agent. Removal of cyanide from aqueous solution with PDC-Chit, PDC-Chit-Ni(II) and PDC-Chit-Fe(III) films was studied with batch equilibrium experiments. At equilibrium, decyanidation capacity (DC) followed the order PDC-Chit-Ni (II)≈PDC-Chit-Fe(III)>PDC-Chit. PDC-Chit-Ni(II) film gave 100% CN(-) removal within 40min decyanidation owing to favorable coordination geometry. PMID:27474675

  4. Electrodeposited polypyrrole (PPy)/para (toluene sulfonic acid) (pTS) free-standing film for lithium secondary battery application

    Highlights: ► Free-standing polypyrrole-para (toluene sulfonic acid) (PPy-pTS) film. ► The films are soft, lightweight, mechanically robust, and highly electrically conductive. ► Application as cathode material for lithium secondary battery ► PPy-pTS film with 30 min deposition time exhibited higher discharge capacity (85 mAh g−1) beyond 80 cycles than the PPy-pTS films with 1 h deposition time (76 mAh g−1) and 2 h deposition time (55 mAh g−1). - Abstract: Highly flexible and bendable free-standing polypyrrole-para (toluene sulfonic acid) (PPy-pTS) films were prepared using the electropolymerization method. The films are soft, lightweight, mechanically robust, and highly electrically conductive. The films display a cauliflower-like structure consisting of micron-scale spherical grains, which are related to dopant intercalation in the polymeric chains. The electrochemical behaviour of the free-standing films was examined as cathode against lithium counter electrode. Electrochemical tests demonstrated that the PPy-pTS film with 30 min deposition time exhibited higher discharge capacity (85 mAh g−1) beyond 80 cycles than the PPy-pTS films with 1 h deposition time (76 mAh g−1) and 2 h deposition time (55 mAh g−1) at 0.1 mA cm−2 over a potential range of 2.5–4.3 V. The free-standing films can be used as electrode materials to satisfy the new market demand for flexible and bendable polymer batteries.

  5. Delivering drug-polymer complex via quick dissolving film: A step towards the development of an appropriate pediatric formulation

    Viralkumar Patel

    2013-01-01

    Full Text Available Lack of suitable prednisolone formulations for treatment of asthma could limit treatment compliance in pediatric population and hence the aim of this study was to develop prednisolone-polymer complexes with enhanced solubility and to incorporate this complex into orally disintegrating films to enable rapid drug delivery. The prednisolone-polymeric complexes were prepared using solvent evaporation and freeze drying techniques with a drug-polymer ratio of 1:1 using hydroxypropyl β-cyclodextrin (HP β-CD, hydroxypropyl methylcellulose 4 cps, and polyvinylpyrrolidone K-30 as polymeric carriers and the parameters such as an aqueous solubility, dissolution profile, and solid-state characterization using differential scanning calorimetry (DSC of the complexes determined. The optimized complex was then incorporated into films prepared using solvent casting technique and the weight variation, thickness, solid-state characterization, in vitro disintegration and dissolution profiles of the films were then determined. The highest prednisolone solubility was seen with the prednisolone-HP β-CD complex prepared by freeze drying (1.82 mg/mL followed by the same complex prepared by solvent evaporation (1.70 mg/mL. The solubility′s were significantly higher compared to prednisolone powder (0.2 mg/mL ( P < 0.05. DSC analysis of complexes revealed a reduction in area of the endothermic peak indicating the presence of amorphous drug while in comparison, the DSC analysis of films did not show endothermic peak showing complete absence of crystalline drug. The film was thin, uniform in weight and thickness, showing rapid disintegration of 55 s with almost complete drug release within 3 min. The study revealed the incorporated drug-polymer complex have maintained the amorphous state and enabled rapid drug release.

  6. Comparison of chondroitin sulfate and hyaluronic Acid doped conductive polypyrrole films for adipose stem cells.

    Björninen, Miina; Siljander, Aliisa; Pelto, Jani; Hyttinen, Jari; Kellomäki, Minna; Miettinen, Susanna; Seppänen, Riitta; Haimi, Suvi

    2014-09-01

    Polypyrrole (PPy) is a conductive polymer that has aroused interest due to its biocompatibility with several cell types and high tailorability as an electroconductive scaffold coating. This study compares the effect of hyaluronic acid (HA) and chondroitin sulfate (CS) doped PPy films on human adipose stem cells (hASCs) under electrical stimulation. The PPy films were synthetized electrochemically. The surface morphology of PPy-HA and PPy-CS was characterized by an atomic force microscope. A pulsed biphasic electric current (BEC) was applied via PPy films non-stimulated samples acting as controls. Viability, attachment, proliferation and osteogenic differentiation of hASCs were evaluated by live/dead staining, DNA content, Alkaline phosphatase activity and mineralization assays. Human ASCs grew as a homogenous cell sheet on PPy-CS surfaces, whereas on PPy-HA cells clustered into small spherical structures. PPy-CS supported hASC proliferation significantly better than PPy-HA at the 7 day time point. Both substrates equally triggered early osteogenic differentiation of hASCs, although mineralization was significantly induced on PPy-CS compared to PPy-HA under BEC. These differences may be due to different surface morphologies originating from the CS and HA dopants. Our results suggest that PPy-CS in particular is a potential osteogenic scaffold coating for bone tissue engineering. PMID:24823653

  7. Optical constants of anodic aluminum oxide films formed in oxalic acid solution

    The anodic aluminum oxide (AAO) films with highly ordered nanopore arrays were prepared in oxalic acid solution under different anodizing voltage and time, its surface and cross section appearances were characterized by using field emission scanning electron microscopy, the transmission spectra with the interference fringes were measured at normal incidence over the wavelength range 200 to 2500 nm. Then the modified Swanepoel method was used for the determination of the optical constants and thickness of the free standing AAO films. The results indicate that the refractive index increases with the increase of anodizing voltage and the decrease of anodizing time, which is mainly due to the content of Al2O3 with octahedron increases in the AAO films. The dispersion of the refractive index is discussed in terms of the single-oscillator Wemple-DiDomenico model, and the energy dependence of the absorption coefficient can be described using the direct transition model proposed by Tauc. Likewise, the optical energy gap Eg is derived from Tauc's extrapolation, and Eg increases from 4.178 to 4.256 eV with the anodizing voltage, but is weakly dependent on anodizing time. All the results are self-consistent in the paper

  8. Optical constants of anodic aluminum oxide films formed in oxalic acid solution

    Wang Jian [College of Physics and Electronic Engineering, Northwest Normal University, Lanzhou 730070 (China); Wang Chengwei [College of Physics and Electronic Engineering, Northwest Normal University, Lanzhou 730070 (China); State Key Laboratory of Solid Lubrication, Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Lanzhou 730000 (China)], E-mail: cwwang@nwnu.edu.cn; Li Yan [College of Physics and Electronic Engineering, Northwest Normal University, Lanzhou 730070 (China); Liu Weimin [State Key Laboratory of Solid Lubrication, Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Lanzhou 730000 (China)

    2008-09-01

    The anodic aluminum oxide (AAO) films with highly ordered nanopore arrays were prepared in oxalic acid solution under different anodizing voltage and time, its surface and cross section appearances were characterized by using field emission scanning electron microscopy, the transmission spectra with the interference fringes were measured at normal incidence over the wavelength range 200 to 2500 nm. Then the modified Swanepoel method was used for the determination of the optical constants and thickness of the free standing AAO films. The results indicate that the refractive index increases with the increase of anodizing voltage and the decrease of anodizing time, which is mainly due to the content of Al{sub 2}O{sub 3} with octahedron increases in the AAO films. The dispersion of the refractive index is discussed in terms of the single-oscillator Wemple-DiDomenico model, and the energy dependence of the absorption coefficient can be described using the direct transition model proposed by Tauc. Likewise, the optical energy gap E{sub g} is derived from Tauc's extrapolation, and E{sub g} increases from 4.178 to 4.256 eV with the anodizing voltage, but is weakly dependent on anodizing time. All the results are self-consistent in the paper.

  9. Water Soluble Usnic Acid-Polyacrylamide Complexes with Enhanced Antimicrobial Activity against Staphylococcus epidermidis

    Iolanda Francolini

    2013-04-01

    Full Text Available Usnic acid, a potent antimicrobial and anticancer agent, poorly soluble in water, was complexed to novel antimicrobial polyacrylamides by establishment of strong acidic-base interactions. Thermal and spectroscopic analysis evidenced a molecular dispersion of the drug in the polymers and a complete drug/polymer miscibility for all the tested compositions. The polymer/drug complexes promptly dissolved in water and possessed a greater antimicrobial activity against Staphylococcus epidermidis than both the free drug and the polymer alone. The best results were obtained with the complex based on the lowest molecular weight polymer and containing a low drug content. Such a complex showed a larger inhibition zone of bacterial growth and a lower minimum inhibitory concentration (MIC with respect to usnic acid alone. This improved killing effect is presumably due to the reduced size of the complexes that allows an efficient cellular uptake of the antimicrobial complexes. The killing effect extent seems to be not significantly dependent on usnic acid content in the samples.

  10. Copper Complexes of Nicotinic-Aromatic Carboxylic Acids as Superoxide Dismutase Mimetics

    Virapong Prachayasittikul

    2008-12-01

    Full Text Available Nicotinic acid (also known as vitamin B3 is a dietary element essential for physiological and antihyperlipidemic functions. This study reports the synthesis of novel mixed ligand complexes of copper with nicotinic and other select carboxylic acids (phthalic, salicylic and anthranilic acids. The tested copper complexes exhibited superoxide dismutase (SOD mimetic activity and antimicrobial activity against Bacillus subtilis ATCC 6633, with a minimum inhibition concentration of 256 μg/mL. Copper complex of nicotinic-phthalic acids (CuNA/Ph was the most potent with a SOD mimetic activity of IC50 34.42 μM. The SOD activities were observed to correlate well with the theoretical parameters as calculated using density functional theory (DFT at the B3LYP/LANL2DZ level of theory. Interestingly, the SOD activity of the copper complex CuNA/Ph was positively correlated with the electron affinity (EA value. The two quantum chemical parameters, highest occupied molecular orbital (HOMO and lowest unoccupied molecular orbital (LUMO, were shown to be appropriate for understanding the mechanism of the metal complexes as their calculated energies show good correlation with the SOD activity. Moreover, copper complex with the highest SOD activity were shown to possess the lowest HOMO energy. These findings demonstrate a great potential for the development of value-added metallovitamin-based therapeutics.

  11. Polymetallic citric complexes as precursors for spray-pyrolysis deposition of thin LaFeO3 films

    A method for the deposition of thin films of the perovskite LaFeO3 on glass is proposed. The films are prepared by spray pyrolysis using an ethylene glycol solution of mixed metal citrate complexes and O2 or N2 as carrier gas at substrate temperatures between 350 °C and 400 °C and post-deposition annealing at 350–480 °C in air. The phase composition, crystal structure, morphology and adhesion of the prepared films (40–600 nm thick) are studied by X-ray diffraction, energy dispersive X-ray microanalysis, scanning electron microscopy, and atomic force microscopy. The influence of the conditions of deposition and post-deposition annealing is studied and optimal parameters of the procedure are described. Single phase dense uniform films with crystallites of approx. 30 nm are obtained. - Highlights: • A method for spray-pyrolysis deposition of thin films of LaFeO3 is proposed. • Mixed metal citrate complexes in ethylene glycol are used as a starting material. • Films with thickness varying from 40 to 600 nm are prepared. • Stoichiometric, uniform and dense films with good adhesion are obtained

  12. Data of thermal degradation and dynamic mechanical properties of starch–glycerol based films with citric acid as crosslinking agent

    González Seligra, Paula; Medina Jaramillo, Carolina; Famá, Lucía; Goyanes, Silvia

    2016-01-01

    Interest in biodegradable edible films as packaging or coating has increased because their beneficial effects on foods. In particular, food products are highly dependents on thermal stability, integrity and transition process temperatures of the packaging. The present work describes a complete data of the thermal degradation and dynamic mechanical properties of starch–glycerol based films with citric acid (CA) as crosslinking agent described in the article titled: “Biodegradable and non-retrogradable eco-films based on starch–glycerol with citric acid as crosslinking agent” González Seligra et al. (2016) [1]. Data describes thermogravimetric and dynamical mechanical experiences and provides the figures of weight loss and loss tangent of the films as a function of the temperature. PMID:27158645

  13. Data of thermal degradation and dynamic mechanical properties of starch-glycerol based films with citric acid as crosslinking agent.

    González Seligra, Paula; Medina Jaramillo, Carolina; Famá, Lucía; Goyanes, Silvia

    2016-06-01

    Interest in biodegradable edible films as packaging or coating has increased because their beneficial effects on foods. In particular, food products are highly dependents on thermal stability, integrity and transition process temperatures of the packaging. The present work describes a complete data of the thermal degradation and dynamic mechanical properties of starch-glycerol based films with citric acid (CA) as crosslinking agent described in the article titled: "Biodegradable and non-retrogradable eco-films based on starch-glycerol with citric acid as crosslinking agent" González Seligra et al. (2016) [1]. Data describes thermogravimetric and dynamical mechanical experiences and provides the figures of weight loss and loss tangent of the films as a function of the temperature. PMID:27158645

  14. Rare earth(III) complexes with an amino acid derived from isonicotinic acid hydrazide: synthesis, characterization and antifungal activities

    Shen, X.; Shi, X.F.; Liu, Y.S.; Yao, T.M. [Department of Chemistry, Tongji University, Shanghai (China); Xie, Y.Y. [Shanghai Institute of Materia Medica, Chinese Academy of Sciences, Shanghai (China)

    1998-12-31

    Rare earth(III) complexes, RE{sub 2}(CPI){sub 3}{center_dot}nH{sub 2}O (RE = La, Ce, Pr, Sm, Gd, Tb, Dy, Er, Yb, Sc, n =3; RE = Nd, Eu, n = 4; H{sub 2}CPI 1-[(N-carboxymethyl-N-phenyl) amino] [acetylisonicotinic acid hydrazide]), have been synthesized and characterized by IR, UV and {sup 1}H NMR spectroscopy, magnetic susceptibility, elemental analysis, molar conductivity and TGA measurement. Preliminary pharmaceutical tests showed that these complex exhibit definite inhibition activities against S. Sake Yake and C. Albicans (Robin) Berkh 50. (author) 16 refs, 4 figs, 3 tabs

  15. Rare earth(III) complexes with an amino acid derived from isonicotinic acid hydrazide: synthesis, characterization and antifungal activities

    Rare earth(III) complexes, RE2(CPI)3·nH2O (RE = La, Ce, Pr, Sm, Gd, Tb, Dy, Er, Yb, Sc, n =3; RE = Nd, Eu, n = 4; H2CPI 1-[(N-carboxymethyl-N-phenyl)amino]acetylisonicotinic acid hydrazide], have been synthesized and characterized by IR, UV and 1H NMR spectroscopy, magnetic susceptibility, elemental analysis, molar conductivity and TGA measurement. Preliminary pharmaceutical tests showed that these complex exhibit definite inhibition activities against S. Sake Yake and C. Albicans (Robin) Berkh 50. (author)

  16. Anodic luminescence, structural, photoluminescent, and photocatalytic properties of anodic oxide films grown on niobium in phosphoric acid

    Stojadinović, Stevan; Tadić, Nenad; Radić, Nenad; Stefanov, Plamen; Grbić, Boško; Vasilić, Rastko

    2015-11-01

    This article reports on properties of oxide films obtained by anodization of niobium in phosphoric acid before and after the dielectric breakdown. Weak anodic luminescence of barrier oxide films formed during the anodization of niobium is correlated to the existence of morphological defects in the oxide layer. Small sized sparks generated by dielectric breakdown of formed oxide film cause rapid increase of luminescence intensity. The luminescence spectrum of obtained films on niobium under spark discharging is composed of continuum radiation and spectral lines caused by electronic spark discharging transitions in oxygen and hydrogen atoms. Oxide films formed before the breakdown are amorphous, while after the breakdown oxide films are partly crystalline and mainly composed of Nb2O5 hexagonal phase. The photocatalytic activity of obtained oxide films after the breakdown was investigated by monitoring the degradation of methyl orange. Increase of the photocatalytic activity with time is related to an increase of oxygen vacancy defects in oxide films formed during the process. Also, higher concentration of oxygen vacancy defects in oxide films results in higher photoluminescence intensity.

  17. Controlled release of tyrosol and ferulic acid encapsulated in chitosan-gelatin films after electron beam irradiation

    Benbettaïeb, Nasreddine; Assifaoui, Ali; Karbowiak, Thomas; Debeaufort, Frédéric; Chambin, Odile

    2016-01-01

    This work deals with the study of the release kinetics of antioxidants (ferulic acid and tyrosol) incorporated into chitosan-gelatin edible films after irradiation processes. The aim was to determine the influence of electron beam irradiation (at 60 kGy) on the retention of antioxidants in the film, their release in water (pH=7) at 25 °C, in relation with the barrier and mechanical properties of biopolymer films. The film preparation process coupled to the irradiation induced a loss of about 20% of tyrosol but did not affect the ferulic acid content. However, 27% of the ferulic acid remained entrapped in the biopolymer network during the release experiments whereas all tyrosol was released. Irradiation induced a reduction of the release rate for both compounds, revealing that cross-linking occurred during irradiation. This was confirmed by the mechanical properties enhancement which tensile strength value significantly increased and by the reduction of permeabilities. Although molecular weights, molar volume and molecular radius of the two compounds are very similar, the effective diffusivity of tyrosol was 40 times greater than that of ferulic acid. The much lower effective diffusion coefficient of ferulic acid as determined from the release kinetics was explained by the interactions settled between ferulic acid molecules and the gelatin-chitosan matrix. As expected, the electron beam irradiation allowed modulating the retention and then the release of antioxidants encapsulated.

  18. Data of thermal degradation and dynamic mechanical properties of starch–glycerol based films with citric acid as crosslinking agent

    González Seligra, Paula; Medina Jaramillo, Carolina; Famá, Lucía; Goyanes, Silvia

    2016-01-01

    Interest in biodegradable edible films as packaging or coating has increased because their beneficial effects on foods. In particular, food products are highly dependents on thermal stability, integrity and transition process temperatures of the packaging. The present work describes a complete data of the thermal degradation and dynamic mechanical properties of starch–glycerol based films with citric acid (CA) as crosslinking agent described in the article titled: “Biodegradable and non-retro...

  19. Phase behavior, interaction and properties of acetic acid lignin-containing polyurethane films coupled with aminopropyltriethoxy silane

    Wang, H. H.; Mou, J; Y. H. Ni; G. Q. Fei; C. L. Si; J. Zou

    2013-01-01

    A series of novel acetic acid lignin-containing polyurethane (LPU) films coupled with aminopropyltriethoxy silane (APTS) (LPUSi) or the mixture of APTS and trimethylol propane (TMP) (LPUSiT) were prepared. With 2% APTS addition, the crosslinking density increased, and the resultant films were endowed with good mechanical properties and water resistance. It was also found that the hydrogen bonding interaction between –NH and –C=O of urethane was destroyed, and new hydrogen bonds between APTS a...

  20. Control of pathogenic and spoilage microorganisms from cheese surface by whey protein films containing malic acid, nisin and natamycin

    Sousa, Isabel; Pintado, Cristina M.B.S.; Ferreira, Maria A.S.S.

    2010-01-01

    The inhibitory effects of nisin, natamycin and malic acid, incorporated in whey protein films with pH 3, were investigated alone or with addition of sucrose esters, Tween80 or EDTA. Water vapour permeability measurements and mechanical and rheological tests were also assessed. EDTA and Tween80 did not sig- nificantly (P < 0.05) influence the inhibitory activity of films against Pseudomonas aeruginosa and Yarrow- ia lipolytica in contrast with the improved effect against Listeria m...

  1. The Synergistic Biologic Activity of Oleanolic and Ursolic Acids in Complex with Hydroxypropyl-γ-Cyclodextrin

    Codruţa Soica

    2014-04-01

    Full Text Available Oleanolic and ursolic acids are natural triterpenic compounds with pentacyclic cholesterol-like structures which gives them very low water solubility, a significant disadvantage in terms of bioavailability. We previously reported the synthesis of inclusion complexes between these acids and cyclodextrins, as well as their in vivo evaluation on chemically induced skin cancer experimental models. In this study the synergistic activity of the acid mixture included inside hydroxypropyl-gamma-cyclodextrin (HPGCD was monitored using in vitro tests and in vivo skin cancer models. The coefficient of drug interaction (CDI was used to characterize the interactions as synergism, additivity or antagonism. Our results revealed an increased antitumor activity for the mixture of the two triterpenic acids, both single and in complex with cyclodextrin, thus proving their complementary biologic activities.

  2. Communication: Physical origins of ionization potential shifts in mixed carboxylic acids and water complexes

    Gu, Quanli; Tang, Zhen; Su, Peifeng; Wu, Wei; Yang, Zhijun; Trindle, Carl O.; Knee, Joseph L.

    2016-08-01

    The ionization potential (IP) of the aromatic alpha hydroxy carboxylic acid, 9-hydroxy-9-fluorene carboxylic acid (9HFCA), is shifted by complexation with hydrogen bonding ligands such as water and formic acid. Generalized Kohn-Sham energy decomposition analysis decomposes the intermolecular binding energies into a frozen energy term, polarization, correlation, and/or dispersion energy terms, as well as terms of geometric relaxation and zero point energy. We observe that in each dimer the attractive polarization always increases upon ionization, enhancing binding in the cation and shifting the IP toward the red. For 9HFCA—H2O, a substantial decrease of the repulsive frozen energy in cation further shifts the IP toward red. For 9HFCA—HCOOH, the increase of the frozen energy actually occurs in the cation and shifts the IP toward blue. Consistent with the experimental measurements, our analysis provides new, non-intuitive perspectives on multiple hydrogen bonds interactions in carboxylic acids and water complexes.

  3. Sequence and structural features of binding site residues in protein-protein complexes: comparison with protein-nucleic acid complexes

    Selvaraj S

    2011-10-01

    Full Text Available Abstract Background Protein-protein interactions are important for several cellular processes. Understanding the mechanism of protein-protein recognition and predicting the binding sites in protein-protein complexes are long standing goals in molecular and computational biology. Methods We have developed an energy based approach for identifying the binding site residues in protein–protein complexes. The binding site residues have been analyzed with sequence and structure based parameters such as binding propensity, neighboring residues in the vicinity of binding sites, conservation score and conformational switching. Results We observed that the binding propensities of amino acid residues are specific for protein-protein complexes. Further, typical dipeptides and tripeptides showed high preference for binding, which is unique to protein-protein complexes. Most of the binding site residues are highly conserved among homologous sequences. Our analysis showed that 7% of residues changed their conformations upon protein-protein complex formation and it is 9.2% and 6.6% in the binding and non-binding sites, respectively. Specifically, the residues Glu, Lys, Leu and Ser changed their conformation from coil to helix/strand and from helix to coil/strand. Leu, Ser, Thr and Val prefer to change their conformation from strand to coil/helix. Conclusions The results obtained in this study will be helpful for understanding and predicting the binding sites in protein-protein complexes.

  4. Oxidation of formic acid on platinum surfaces decorated with cobalt(III) macrocyclic complexes

    Stevanović, S.; Babić-Samardžija, K.; Sovilj, S. P.; Tripković, A.; Jovanović, V. M.

    2009-09-01

    Platinum electrode decorated with three different mixed-ligand cobalt(III) complexes of the general formula [Co(Rdtc)cyclam](ClO4)2 [cyclam = 1,4,8,11-tetraazacyclotetradecane, Rdtc- = morpholine-(Morphdtc), piperidine-(Pipdtc), and 4-methylpiperidine-(4-Mepipdtc) dithiocarbamates, respectively] was used to study oxidation of formic acid in acidic solution. The complexes were adsorbed on differently prepared Pt surfaces, at open circuit potential. The preliminary results show increased catalytic activity of Pt for formic acid oxidation with complex ion adsorbed on the polycrystalline surfaces. The increase in catalytic activity depends on the structure of the complex applied and follows the order of metal-coordinated bidentate ligand as Morphdtc > Pipdtc > 4-Mepipdtc. Based on IR and NMR data, the main characteristics of the Rdtc ligands do not vary dramatically, but high symmetry of the corresponding complexes decreases in the same order. Accordingly, the complexes are distinctively more mobile, causing chemical interactions to occur on the surface with appreciable speed and enhanced selectivity. The effect of the complexes on catalytic activity presumably depends on structural changes on Pt surfaces caused by their adsorption.

  5. Luminescent polymethacrylate composite nanofibers containing a benzoic acid rare earth complex: Morphology and luminescence properties

    Highlights: • We synthesize PMMA composite nanofibers containing benzoic acid rare earth complex. • We investigate the effects of nanofiber morphology on luminescence properties. • Nanofibers with different morphologies had different luminescence characteristics. • Fluorescence intensity and emission lifetime of porous nanobeads were the highest. • Nanofibers with a porous structure showed the stronger fluorescent recognition ability. - Abstract: In this study, we systematically investigated the morphologies and luminescence properties of luminescent polymethacrylate composite nanofibers containing a benzoic acid rare earth complex. The analysis results indicated that the benzoic acid rare earth complex, Tb(4-methylbenzoic acid)3phen, was distributed uniformly in the polymethacrylate nanofibers, which were fabricated by electrostatic spinning. The Tb(4-methylbenzoic acid)3phen content in the polymethacrylate nanofibers was as high as 20% (mass%). The emission peaks of the as-prepared polymethacrylate composite nanofibers corresponded to the characteristic 5D4–7F6,5,4,3 transitions of Tb3+ ions. The highest emission peak was observed at 548 nm and corresponded to the 5D4–7F5 transition. When the Tb(4-methylbenzoic acid)3phen content was less than 1%, even a 0.2% increase in the content increased the fluorescence intensity markedly. The thermal stability of the rare earth complex was higher in the as-prepared nanofibers; the initial decomposition temperature of the polymethacrylate composite nanofiber reached 291 °C. Composite nanofibers with different morphologies exhibited different luminescence characteristics. The fluorescence intensity and emission lifetime of porous nanobeads were nine and two times higher, respectively, than those of smooth nanofibers. The better morphological and luminescence properties exhibited by the synthesized luminescent polymethacrylate composite nanofibers should result in the use of benzoic acid rare earth complexes in

  6. Luminescent polymethacrylate composite nanofibers containing a benzoic acid rare earth complex: Morphology and luminescence properties

    Zhao, Fulai [Tianjin Municipal Key Lab of Fiber Modification and Functional Fiber, Tianjin Polytechnic University, 300387 Tianjin (China); Xi, Peng, E-mail: xpsyq0007@sina.com [Tianjin Municipal Key Lab of Fiber Modification and Functional Fiber, Tianjin Polytechnic University, 300387 Tianjin (China); State Key laboratory of Polymer Physics and Chemistry, Institute of Chemistry, Chinese Academy of Sciences, 100080 Beijing (China); Xia, Haiying; Wang, Chaohua; Gao, Li [Tianjin Municipal Key Lab of Fiber Modification and Functional Fiber, Tianjin Polytechnic University, 300387 Tianjin (China); Cheng, Bowen, E-mail: Bowen@tjpu.edu.cn [Tianjin Municipal Key Lab of Fiber Modification and Functional Fiber, Tianjin Polytechnic University, 300387 Tianjin (China)

    2015-08-25

    Highlights: • We synthesize PMMA composite nanofibers containing benzoic acid rare earth complex. • We investigate the effects of nanofiber morphology on luminescence properties. • Nanofibers with different morphologies had different luminescence characteristics. • Fluorescence intensity and emission lifetime of porous nanobeads were the highest. • Nanofibers with a porous structure showed the stronger fluorescent recognition ability. - Abstract: In this study, we systematically investigated the morphologies and luminescence properties of luminescent polymethacrylate composite nanofibers containing a benzoic acid rare earth complex. The analysis results indicated that the benzoic acid rare earth complex, Tb(4-methylbenzoic acid){sub 3}phen, was distributed uniformly in the polymethacrylate nanofibers, which were fabricated by electrostatic spinning. The Tb(4-methylbenzoic acid){sub 3}phen content in the polymethacrylate nanofibers was as high as 20% (mass%). The emission peaks of the as-prepared polymethacrylate composite nanofibers corresponded to the characteristic {sup 5}D{sub 4}–{sup 7}F{sub 6,5,4,3} transitions of Tb{sup 3+} ions. The highest emission peak was observed at 548 nm and corresponded to the {sup 5}D{sub 4}–{sup 7}F{sub 5} transition. When the Tb(4-methylbenzoic acid){sub 3}phen content was less than 1%, even a 0.2% increase in the content increased the fluorescence intensity markedly. The thermal stability of the rare earth complex was higher in the as-prepared nanofibers; the initial decomposition temperature of the polymethacrylate composite nanofiber reached 291 °C. Composite nanofibers with different morphologies exhibited different luminescence characteristics. The fluorescence intensity and emission lifetime of porous nanobeads were nine and two times higher, respectively, than those of smooth nanofibers. The better morphological and luminescence properties exhibited by the synthesized luminescent polymethacrylate composite

  7. Studies on beryllium complexes. V. Chelation of Be2+ ions by anthranilic acid

    After having determined the formation constants of anthranilic acid, the anthranilic acid-Be2+ - H2O system (0.5 M NaClO3 and t=25 deg C) has been studied. The complex BeA+ and the hydroxylated species Be2(OH)A2+, Be3(OH)3A2+, Be3(OH)3A2+ have been identified

  8. Effect of ionic strength on complexation of Pu(IV) with humic acid

    Szabo, G; Guczi, J.; Reiller, Pascal; Miyajima, T.; Bulman, R.,

    2010-01-01

    Successful geochemical modelling of the migration of radioactive materials, such as the transuranic elements, from nuclear waste repositories is dependent upon an understanding of their interaction with biogeopolymers such as humic acids, the most likely complexing agents in groundwaters. An established silica/humic acid composite has been evaluated as a model substrate for naturally occurring humate-coated minerals that are likely to be present in the vicinity of the repositories. The bindin...

  9. Fatty acid nitroalkenes induce resistance to ischemic cardiac injury by modulating mitochondrial respiration at complex II

    Koenitzer, Jeffrey R; Gustavo Bonacci; Woodcock, Steven R.; Chen-Shan Chen; Nadiezhda Cantu-Medellin; Kelley, Eric E.; Schopfer, Francisco J.

    2016-01-01

    Nitro-fatty acids (NO2-FA) are metabolic and inflammatory-derived electrophiles that mediate pleiotropic signaling actions. It was hypothesized that NO2-FA would impact mitochondrial redox reactions to induce tissue-protective metabolic shifts in cells. Nitro-oleic acid (OA-NO2) reversibly inhibited complex II-linked respiration in isolated rat heart mitochondria in a pH-dependent manner and suppressed superoxide formation. Nitroalkylation of Fp subunit was determined by BME capture and the s...

  10. Electrocatalytic and simultaneous determination of isoproterenol, uric acid and folic acid at molybdenum (VI) complex-carbon nanotube paste electrode

    Beitollahi, Hadi, E-mail: h.beitollahi@yahoo.com [Environment Department, Research Institute of Environmental Sciences, International Center for Science, High Technology and Environmental Sciences, Kerman (Iran, Islamic Republic of); Sheikhshoaie, Iran [Department of Chemistry, Faculty of Science, Shahid Bahonar University of Kerman, Kerman 76175-133 (Iran, Islamic Republic of)

    2011-11-30

    Highlights: > A molybdenum (VI) complex-carbon nanotube paste electrode have been fabricated. > This electrode reduced the oxidation potential of isoproterenol by about 175 mV. > It resolved the voltammetric waves of isoproterenol, uric acid and folic acid. - Abstract: This paper describes the development, electrochemical characterization and utilization of a novel modified molybdenum (VI) complex-carbon nanotube paste electrode for the electrocatalytic determination of isoproterenol (IP). The electrochemical profile of the proposed modified electrode was analyzed by cyclic voltammetry (CV) that showed a shift of the oxidation peak potential of IP at 175 mV to less positive value, compared with an unmodified carbon paste electrode. Differential pulse voltammetry (DPV) in 0.1 M phosphate buffer solution (PBS) at pH 7.0 was performed to determine IP in the range from 0.7 to 600.0 {mu}M, with a detection limit of 35.0 nM. Then the modified electrode was used to determine IP in an excess of uric acid (UA) and folic acid (FA) by DPV. Finally, this method was used for the determination of IP in some real samples.

  11. Light responsive thin films of micelles of PS-b-PVP complexed with diazophenol chromophore

    We have incorporated push–pull azobenzene units into diblock-copolymer micelles by supramolecular assembly. Specifically, we encapsulated a phenol-functionalized chromophore, DO13, within PS-b-P4VP micelles in toluene by means of H-bond interactions developed between DO13 molecules and pyridine groups of P4VP block. The solutions were spin-coated onto glass substrates resulting in multi- or mono-layered thin films of micelles with P4VP(DO13) core and PS corona. We show that the use of DO13 as a building block of micellar aggregates allowed us to manipulate the developed nanostructures. Spherical to cylindrical micellar transition was found when we increased the degree of chromophore complexation. Also, it was found that the polymer concentration in the solution plays an important role in determining the micellar nanostructures. The chain extension and change in composition of the P4VP core in the presence of the chromophore may be responsible for the structural changes observed in the micelles. The optical properties of the thin films have been investigated focusing on the effect of the micellar morphology over the photoinduced birefringence. The optical anisotropy (Δn) increased with respect to the analogous homogeneous system P4VP(DO13), indicating that the protective micelle environment can enhance the optical properties of the embedded chromophores significantly. Furthermore, we show very interesting new results in which we have related changes in optical properties to the film morphology (spheres to cylinders). This can be exploited for producing optical devices having improved optoelectronic properties and stability. (paper)

  12. Asymmetric epoxidation of allylic alcohols catalyzed by vanadium-binaphthylbishydroxamic Acid complex.

    Noji, Masahiro; Kobayashi, Toshihiro; Uechi, Yuria; Kikuchi, Asami; Kondo, Hisako; Sugiyama, Shigeo; Ishii, Keitaro

    2015-03-20

    A vanadium-binaphthylbishydroxamic acid (BBHA) complex-catalyzed asymmetric epoxidation of allylic alcohols is described. The optically active binaphthyl-based ligands BBHA 2a and 2b were synthesized from (S)-1,1'-binaphthyl-2,2'-dicarboxylic acid and N-substituted-O-trimethylsilyl (TMS)-protected hydroxylamines via a one-pot, three-step procedure. The epoxidations of 2,3,3-trisubstituted allylic alcohols using the vanadium complex of 2a were easily performed in toluene with a TBHP water solution to afford (2R)-epoxy alcohols in good to excellent enantioselectivities. PMID:25714329

  13. Co(II) complexes of amino acids and peptides in aqueous solution studied by 170 NMR

    Structural, dynamic and kinetic 170 NMR investigations of the complexation of metal ions with amino acids and peptides were performed in Glicine, proling cyclo(Ala '1'70-Ala), cyclo-(Gly170-Pro) and cyclo(Pro170-Gly). The 170 carboxyl and carbonylsignals of paramagnetic complexes with amino acids were observed and allowed for the determinatio, in several cases, of the stoichiometry of the ocmplexes formed and the kinetic and thermodynamic parameters characterizing ligand exchange. It was found that the paramagnetic ions bind to the oxygen of the peptide carboxyl group. (H.W.). 25 refs.; 10 figs.; 3 tabs

  14. Preparation of porous monolayer film by immersing the stearic acid Langmuir-Blodgett monolayer on mica in salt solution

    Wang, S. [Institute of Near-Field Optics and Nano Technology, School of Physics and Optoelectronic Technology, Dalian University of Technology, Street No. 2 Linggong Road, Dalian 116024 (China); Li, Y.L.; Zhao, H.L.; Liang, H. [Institute of Photo-Biophysics, School of Physics and Electronic, Henan University, Jinming, Kaifeng 475004, Henan (China); Liu, B., E-mail: boliu@henu.edu.cn [Institute of Photo-Biophysics, School of Physics and Electronic, Henan University, Jinming, Kaifeng 475004, Henan (China); Pan, S., E-mail: span@dlut.edu.cn [Institute of Near-Field Optics and Nano Technology, School of Physics and Optoelectronic Technology, Dalian University of Technology, Street No. 2 Linggong Road, Dalian 116024 (China)

    2012-11-15

    Highlights: Black-Right-Pointing-Pointer Porous film has been prepared by immersing the stearic acid Langmuir-Blodgett monolayer on mica in salt solution. Black-Right-Pointing-Pointer The mechanism relies on the electrostatic screening effect of the cations in salt solution. Black-Right-Pointing-Pointer The factors influencing the size and area of the pores were investigated. - Abstract: Porous materials have drawn attention from scientists in many fields such as life sciences, catalysis and photonics since they can be used to induce some materials growth as expected. Especially, porous Langmuir-Blodgett (LB) film is an ideal material with controlled thickness and flat surface. In this paper, stearic acid (SA), which has been extensively explored in LB film technique, is chosen as the template material with known parameters to prepare the LB film, and then the porous SA monolayer film is obtained by means of etching in salt solution. The main etching mechanism is suggested that the cations in the solution block the electrostatic interaction between the polar carboxyl group of SA and the electronegative mica surface. The influencing factors (such as concentration of salt solution, valence of cation and surface pressure) of the porous SA film are systematically studied in this work. The novel method proposed in this paper makes it convenient to prepare porous monolayer film for designed material growth or cell culture.

  15. Preparation of porous monolayer film by immersing the stearic acid Langmuir–Blodgett monolayer on mica in salt solution

    Highlights: ► Porous film has been prepared by immersing the stearic acid Langmuir–Blodgett monolayer on mica in salt solution. ► The mechanism relies on the electrostatic screening effect of the cations in salt solution. ► The factors influencing the size and area of the pores were investigated. - Abstract: Porous materials have drawn attention from scientists in many fields such as life sciences, catalysis and photonics since they can be used to induce some materials growth as expected. Especially, porous Langmuir–Blodgett (LB) film is an ideal material with controlled thickness and flat surface. In this paper, stearic acid (SA), which has been extensively explored in LB film technique, is chosen as the template material with known parameters to prepare the LB film, and then the porous SA monolayer film is obtained by means of etching in salt solution. The main etching mechanism is suggested that the cations in the solution block the electrostatic interaction between the polar carboxyl group of SA and the electronegative mica surface. The influencing factors (such as concentration of salt solution, valence of cation and surface pressure) of the porous SA film are systematically studied in this work. The novel method proposed in this paper makes it convenient to prepare porous monolayer film for designed material growth or cell culture.

  16. Mononuclear metal complexes of organic carboxylic acid derivatives: Synthesis, spectroscopic characterization, thermal investigation and antimicrobial activity

    Abd El-Wahab, Zeinab H.

    2007-05-01

    Two Schiff base ligands bearing organic acid moiety, vis., N-(2-thienylmethylidene)-2-amino-4-chlorobenzoic acid (HL 1) and N-(2-hydroxybenzylidene)-2-amino-4-chlorobenzoic acid (H 2L 2) have been synthesized by the interaction of 2-thiophenecarboxaldehyde and 2-hydroxybenzaldehyde with 2-amino-4-chlorobenzoic acid. Co(II), Ni(II), Cu(II) and Zn(II) complexes of these ligands have been prepared. They are characterized on the basis of analytical data, molar conductance, IR, 1H NMR, UV-vis, mass spectra, magnetic measurements, thermal analysis and X-ray powder diffraction technique. The molar conductance data reveal that these complexes are non-electrolytes. The ligands are coordinated to the metal ions in a terdentate manner with ONO/ONS donor sites of the carbonyl oxygen, azomethine nitrogen and phenolic oxygen or thiophenic sulphur. An octahedral structure is proposed for the prepared metal complexes and some ligand field parameters ( Dq, B and β) in addition to CFSE were calculated. The thermal stability of the metal complexes is evaluated. The Schiff base ligands and their metal complexes have been tested against four species of bacteria as well as four species of fungi and the results have been compared with some known antibiotics.

  17. Synthesis and characterization of CdS/PVA nanocomposite thin films from a complexing agent free system

    Highlights: ► Polymer–CdS nanocomposite thin films have been synthesized by in situ thermolysis of the precursors confined in polymer matrix. ► Thesynthetic method is free from complexing agent. ► The film was prepared within a short period (10–60 min) compared to conventionalCBD method, which takes longer time. ► Our method can yield pinhole free, homogeneous and transparent films very well adhered to thesubstrate. ► The film is suitable for application as a window layer in solar cell. - Abstract: CdS/PVA nanocomposite thin films have been deposited on glass substrates by in situ thermolysis of precursors dispersed in polyvinyl alcohol (PVA). The synthetic technique reported in this study is free from complexing agent and hence no need to control the pH of the solution as in the case of conventional CBD. The as-prepared films were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), selected area electron diffraction (SAED), UV–vis spectroscopy, and photoluminescence (PL) spectra. The XRD and SAED results indicated the formation of CdS nanoparticles with hexagonal phase in the PVA matrix. The photoluminescence and UV–vis spectroscopy revealed that CdS/PVA films showed quantum confinement effect. From the shift in optical band gap, particle sizes were calculated using effective mass approximation (EMA) method and it was found to be in agreement with the results obtained from TEM observations. The SEM results indicated that as grown films were homogeneous with no visible pinholes and cracks. The film prepared at100 °C was found to be suitable for application as a window layer in solar cell.

  18. Recognition of amino acids and anions by a Zn(Ⅱ)-methylazacalix[4]pyridine complex

    2009-01-01

    As a powerful macrocyclic host molecule with unique conformation and cavity structure that are fine-tuned by the bridging nitrogen atoms, methylazacalix[4]pyridine (MACP-4) has been shown to selectively recognize Zn2+ and form stable Zn(Ⅱ)-MACP-4 complexes both in solid state and solution with an association constant up to 5.97 (logKs). The molecular recognition of Zn(Ⅱ)-MACP-4 complexes towards various amino acids and anions with different geometry was investigated by using the spectral titration methods and X-ray analysis. The Zn(Ⅱ)-MACP-4 complex was found to recognize the 17 amino acids tested with the association constant up to 3.97 (logKs). On the other hand, the Zn(Ⅱ)-MACP-4 complex selectively interacted with anions and the maximum association constant of 3.9 (logKs) was obtained.

  19. Functionalization of conducting polymer with novel Co(II) complex: Electroanalysis of ascorbic acid

    We report for the first time the functionalization of a conducting polymer with a metal complex in order to develop a new type of catalytic material exhibiting better electronic communication through their delocalized π electrons. The Co(II) complex having hydroxyl group as functional moiety is chemically coupled with carboxyl group of polyanthranilic acid which itself is a self doped conducting polymer. The covalent linkage between Co(II) and -OH group is confirmed using UV-vis, FT-IR and NMR spectroscopic techniques. The Co(II) complex functionalized polymer does exhibit excellent redox behavior and stability with mixed properties of Co(II) complex and π-conjugated polymer. The material possesses potential benefits in sensors/biosensor applications and it is demonstrated for the electroanalysis of ascorbic acid at a level of nano molar concentration.

  20. Oxidation of saturated hydrocarbons with peroxyacetic acid catalyzed by vanadium complexes

    Gonzalez Cuervo, Laura; Kozlov, Yuriy N.; Süss-Fink, Georg; Shul’pin, Georgiy B.

    2009-01-01

    Peroxyacetic acid (PAA) oxidizes alkanes in acetonitrile or acetic acid at 60 °C if a soluble vanadium(V) salt, n-Bu4NVO3 (1), is used as a catalyst. Corresponding ketones, alcohols and alkyl hydroperoxides are the main products. Methane, ethane, propane, cyclohexane, and other higher alkanes were substrates in the oxidations. The proposed mechanism involves the formation of a complex between (1) and PAA with equilibrium constants 3.3 and 6.8 dm3 mol−1 for acetonitrile and acetic acid as solv...

  1. Synthesis and evaluation of 3-acyl-tetronic acid-containing metal complexing agents

    Potential metal chelators containing one or several acyl-tetronic acid moieties were prepared from cyclic or acyclic amines and polyamines, and from bis(phenols) by reaction with 1-4 equiv of 3 bromoacetyl-tetronic acid in the presence of potassium carbonate. The affinity constants of the chelating agents for toxic metallic cations Cd2+, Cs+, and Pb2+ and for dimethylarsinic acid were measured, at pH 7.5 and 9.3. Compound 4, an acyclic triamine containing four acyl-tetronic moieties, was found to complex efficiently all the tested species. (authors)

  2. Efeito da adição de ácidos graxos em filmes à base de pectina The effect of addition of fatty acids on pectin films

    Juliana A. Batista

    2005-12-01

    Full Text Available Os objetivos deste trabalho foram desenvolver filmes à base de pectina de baixo teor de esterificação, amidada, com adição dos ácidos graxos láurico (AL, palmítico (AP e esteárico (AE e caracterizá-los quanto às propriedades de permeabilidade ao vapor de água (PVA e ao oxigênio, propriedades mecânicas (tensão de ruptura e elongação, solubilidade em água e opacidade, além de observar a morfologia da superfície dos filmes utilizando microscopia eletrônica de varredura (MEV. A adição de 12 e 18% dos ácidos promoveu aumento da PVA e da elongação e redução da tensão de ruptura, em relação aos filmes com 6% de ácido graxo. Todos os filmes apresentaram-se 100% solúveis em água e mais opacos quando os ácidos graxos foram adicionados. A partir da MEV, foi observado que os ácidos graxos não se incorporaram à matriz filmogênica.The purposes of this research were to develop and characterize composite biofilms produced with low methoxyl amidated pectin plus lauric, palmitic and stearic acids. Water vapor permeability, oxigen permeability, mechanical properties (tensile strength and elongation, water solubility, opacity and, surface morphology were evaluated. The increase of fatty acids addition to 12 and 18% resulted in an increase in water vapor permeability and elongation and a decrease in tensile strength compared to the level of 6% of fatty acids. All formulations produced films showing 100% water solubility. As observed by scanning electronic microscopy the fatty acids were not homogeneously incorporated on the filmogenic matrices.

  3. Complex high-frequency magnetization dynamics and magnetoimpedance in thin films

    Silva, R.B. da [Departamento de Fisica, CCNE, Universidade Federal de Santa Maria, 97105-900 Santa Maria, RS (Brazil)]. E-mail: rbarreto1975@gmail.com; Viegas, A.D.C. [Departamento de Fisica, CCNE, Universidade Federal de Santa Maria, 97105-900 Santa Maria, RS (Brazil); Correa, M.A. [Departamento de Fisica, CCNE, Universidade Federal de Santa Maria, 97105-900 Santa Maria, RS (Brazil); Andrade, A.M.H. de [Departamento de Fisica, CCNE, Universidade Federal de Santa Maria, 97105-900 Santa Maria, RS (Brazil); Sommer, R.L. [Centro Brasileiro de Pesquisas Fisicas-CBPF, Rua Dr. Xavier Sigaud 150, Urca, 22290-180, Rio de Janeiro, RJ (Brazil)

    2006-10-01

    High-frequency differential magnetic permeability and magnetoimpedance measurements were performed in Fe{sub 73.5}Cu{sub 1}Nb{sub 3}Si{sub 13.5}B{sub 9} as-made and annealed thin films at frequencies up to 1.8 GHz. The results show complex dynamical properties characterized by multiple ferromagnetic resonance modes at relatively low frequencies for the amorphous as-made sample. After the thermal treatments, the resonance frequencies increase drastically exceeding the upper limit of 1.8 GHz for our equipment. This increase can possibly associated to higher local magnetic fields that are, in turn, associated to the formation of nanocrystalline grains randomly oriented.

  4. Site-selective electroless nickel plating on patterned thin films of macromolecular metal complexes.

    Kimura, Mutsumi; Yamagiwa, Hiroki; Asakawa, Daisuke; Noguchi, Makoto; Kurashina, Tadashi; Fukawa, Tadashi; Shirai, Hirofusa

    2010-12-01

    We demonstrate a simple route to depositing nickel layer patterns using photocross-linked polymer thin films containing palladium catalysts, which can be used as adhesive interlayers for fabrication of nickel patterns on glass and plastic substrates. Electroless nickel patterns can be obtained in three steps: (i) the pattern formation of partially quaterized poly(vinyl pyridine) by UV irradiation, (ii) the formation of macromolecular metal complex with palladium, and (iii) the nickel metallization using electroless plating bath. Metallization is site-selective and allows for a high resolution. And the resulting nickel layered structure shows good adhesion with glass and plastic substrates. The direct patterning of metallic layers onto insulating substrates indicates a great potential for fabricating micro/nano devices. PMID:21069972

  5. Hydrogen bonding in oxalic acid and its complexes: A database study of neutron structures

    R Chitra; Amit Das; R R Choudhury; M Ramanadham; R Chidambaram

    2004-08-01

    The basic result of carboxylic group that the oxygen atom of the –OH never seems to be a hydrogen bond acceptor is violated in the cases, namely urea oxalic acid and bis urea oxalic acid complexes, where the hydroxyl oxygen atom is an acceptor of a weak N–H... O hydrogen bond. The parameters of this hydrogen bond, respectively in these structures are: hydrogen acceptor distance 2.110 Å and 2.127 Å and the bending angle at hydrogen, 165.6° and 165.8°. The bond strength around the hydroxyl oxygen is close to 1.91 valence units, indicating that it has hardly any strength left to form hydrogen bonds. These two structures being highly planar, force the formation of this hydrogen bond. As oxalic acid is the common moiety, the structures of the two polymorphs, -oxalic acid and -oxalic acid, also were looked into in terms of hydrogen bonding and packing.

  6. Comb-like ionic complexes of hyaluronic acid with alkyltrimethylammonium surfactants

    Tolentino, Ainhoa; Alla Bedahnane, Abdelilah; Martínez de Ilarduya Sáez de Asteasu, Domingo Antxon; Muñoz Guerra, Sebastián

    2013-01-01

    Stoichiometric complexes of hyaluronic acid with alkyltrimethylammonium surfactants bearing octadecyl, eicosyl and docosyl groups were prepared by ionic coupling in aqueous solution. The complexes were non soluble in water but soluble in organic solvents. In the solid state they self-assembled in a biphasic layered structure with the alkyl side chains forming a separate phase that melted in the 50–60 °C range. They were stable to heating up to above 200 °C.

  7. NMR study of reactions between Pd, Ru, and Rh nitrite complexes and sulfamic acid

    Interaction of Pd, Ru and Rh nitrite complexes with sulfamic acid was studied by the method of 14N, 15N and 17O NMR. Reference of chemical shifts was made, prevailing complex forms being ascertained. It was established that cis-nitroaquacomplexes are products of the interaction at room temperature. Coordination of sulfaminate-ion during long-term allowance to stand or during heating of the solutions was revealed

  8. Study of molecular complexation of glycyrrhizic acid with chloramphenicol by electrospray ionization mass spectrometry

    Vetrova, Elena V.; Lekar, Anna V.; Filonova, Olga V.; Borisenko, Sergey N.; Maksimenko, Elena V.; Borisenko, Nikolay I.

    2015-01-01

    Context: Glycyrrhizic acid (GA) is a triterpene glycoside representing the main active component of licorice root extract obtained from plants of the Glycyrrhiza glabra L. and widely used as a complex-forming agent for the synthesis of new transport forms of the well-known drugs. Aims: For the first time, the complexation of GA with chloramphenicol antibiotic (ChlA) was investigated by electrospray ionization mass spectrometry (ESI MS). Subjects and Methods: ESI MS was utilized in order to de...

  9. Synthesis and spectroscopic studies of iron (III) complex with a quinolone family member (pipemidic acid)

    Skrzypek, D.; Szymanska, B.; Kovala-Demertzi, Dimitra; Wiecek, Joanna; Talik, E.; Demertzis, Mavroudis A.

    2006-12-01

    The interaction of iron (III) with pipemidic acid, Hpipem, afforded the complex [Fe (pipem) (HO)2 (H2O)]2. The new complex has been characterised by elemental analyses, infra-red, EPR and XPS spectroscopies. The monoanion, pipem, exhibits O, O ligation through the carbonyl and carboxylato oxygen atoms. Six coordinate dimer distorted octahedral configuration has been proposed for [Fe (pipem) (HO)2 (H2O)]2.

  10. Therapeutic Potentials of Silver Nanoparticle Complex of α-Lipoic Acid

    Lakshmy Ramachandran; Cherupally Krishnan Krishnan Nair

    2011-01-01

    Silver (SN) nanoparticles were re‐dispersed in aqueous solution of Pluronic F127 and complexed with the antioxidant, alpha‐ Lipoic acid (LA). The nanoparticle ‐ LA complex (SN‐LA) was characterized using SEM. SN‐ LA exhibited DPPH radical scavenging activity in vitro and anti‐ inflammatory activity against acute and chronic paw models of edema in mice. SN‐LA protected mice from whole body gamma radiation induced body weight losses and mortality reveal...

  11. Arsenic speciation and identification of monomethylarsonous acid and monomethylthioarsonic acid in a complex matrix.

    Yathavakilla, Santha Ketavarapu V; Fricke, Michael; Creed, Patricia A; Heitkemper, Douglas T; Shockey, Nohora V; Schwegel, Carol; Caruso, Joseph A; Creed, John T

    2008-02-01

    Anion-exchange chromatography was utilized for speciation of arsenite (As(III)), arsenate (As(V)), dimethylarsinic acid (DMA(V)), monomethylarsonic acid (MMA(V)), monomethylarsonous acid (MMA(III)), and the new As species monomethylthioarsonic acid (MMTA), using inductively coupled plasma mass spectrometric (ICPMS) detection. MMA(III) and MMTA were identified for the first time in freeze-dried carrot samples that were collected over 25 years ago as part of a joint U.S. EPA, U.S. FDA, and USDA study on trace elements in agricultural crops. The discovery of MMA(III) and MMTA in terrestrial foods necessitated the analytical characterization of synthetic standards of both species, which were used for standard addition in carrot extracts. The negative ion mode, high-resolution electrospray mass spectrometry (HR-ESI-MS) data produced molecular ions of m/z 122.9418 and 154.9152 for MMA(III) and MMTA, respectively. However, ESI-MS was not sensitive enough to directly identify MMA(III) and MMTA in the carrot extracts. Therefore, to further substantiate the identification of MMA(III) and MMTA, two additional separations using an Ion-120 column were developed using the more sensitive ICPMS detection. The first separation used 20 mM tetramethylammonium hydroxide at pH 12.2 with MMA(III) eluting in less than 7 min. In the second separation, MMTA eluted at 11.2 min by utilizing 40 mM ammonium carbonate at pH 9.0. Oxidation of MMA(III) and MMTA to MMA(V) with hydrogen peroxide was observed for standards and carrot extracts alike. Several samples of carrots collected from local markets in 2006 were also analyzed and found to contain low levels of inorganic arsenic species. PMID:18181583

  12. Determination of complex formation constants by phase sensitive alternating current polarography: Cadmium-polymethacrylic acid and cadmium-polygalacturonic acid.

    Garrigosa, Anna Maria; Gusmão, Rui; Ariño, Cristina; Díaz-Cruz, José Manuel; Esteban, Miquel

    2007-10-15

    The use of phase sensitive alternating current polarography (ACP) for the evaluation of complex formation constants of systems where electrodic adsorption is present has been proposed. The applicability of the technique implies the previous selection of the phase angle where contribution of capacitive current is minimized. This is made using Multivariate Curve Resolution by Alternating Least Squares (MCR-ALS) in the analysis of ACP measurements at different phase angles. The method is checked by the study of the complexation of Cd by polymethacrylic (PMA) and polygalacturonic (PGA) acids, and the optimal phase angles have been ca. -10 degrees for Cd-PMA and ca. -15 degrees for Cd-PGA systems. The goodness of phase sensitive ACP has been demonstrated comparing the determined complex formation constants with those obtained by reverse pulse polarography, a technique that minimizes the electrode adsorption effects on the measured currents. PMID:19073101

  13. A convenient method for the preparation of barbituric and thiobarbituric acid transition metal complexes

    Refat, Moamen S.; El-Korashy, Sabry A.; Ahmed, Ahmed S.

    2008-12-01

    A convenient method for the preparation of barbiturate transition metal complexes: (i) Cr 3+, Mn 2+, Fe 3+, Zn 2+ and Cd 2+ ions with barbituric acid (H 2L) and (ii) Cr 3+ and Mo 5+ with 2-thiobarbituric acid (H 2L') was reported and this has enabled seven complexes to be formulated as: [Cr(HL) 2(OH)(H 2O)]·H 2O, [Mn(HL) 2(H 2O) 2], [Fe 2(L)(OH) 3(H 2O) 4]·2H 2O, [Zn(HL) 2], [Cd(HL) 2], [Cr(HL')(OH) 2(H 2O)]·H 2O and [Mo(HL') 2]Cl. These new barbiturate complexes were synthesized and characterized by elemental analysis, molar conductivity, magnetic measurements, spectral methods (mid infrared, 1H NMR, mass, X-ray powder diffraction and UV/vis spectra) and simultaneous thermal analysis (TG and DTG) techniques. The molar conductance measurements proved that, all complexes of barbituric and 2-thiobarbituric acids are non-electrolytes except for [Mo(HL') 2]Cl. The electronic spectra and magnetic susceptibility measurements were used to infer the structures. The IR spectra of the ligands and their complexes are used to identify the mode of coordination. Kinetic and thermodynamic parameters such as: E*, Δ H*, Δ S* and Δ G* are estimated according to the DTG curves. The two ligands and their complexes have been studied for their possible biological antifungal activity.

  14. Stability constants of mixed ligand complexes of lanthanide(III) and yttrium(III) with complexone and substituted salicylic acids

    Salicylic acid and substituted salicylic acids are potential antimicrobial agents. Binary complexes of salicylic acid and its substituted derivatives with lanthanide(III) and yttrium(III) metal ions have been reported. There are reports on the ternary metal complexing equilibria with some lanthanide(III) and yttrium(III) metal ions involving aminopolycarboxylic acid as one ligand and salicylic acid (SA) and other related compounds as the second ligands. Ethylene glycol bis(2-aminoethylether)- N, N, N', N'-tetraacetic acid (EGTA) is an important member of aminopolycarboxylic acid and finds many applications in medicine and biology. Recently, few ternary complexes have been reported using EGTA as ligand. In view of biological importance of simple and mixed ligand complexes EGTA, SA and DNSA (3,5-dinitrosalicylic acid), a systematic study has been undertaken for the determination of stability constant and the results are reported. (author). 6 refs., 1 fig., 2 tabs

  15. Characterization of Active Packaging Films Made from Poly(Lactic Acid)/Poly(Trimethylene Carbonate) Incorporated with Oregano Essential Oil.

    Liu, Dong; Li, Hongli; Jiang, Lin; Chuan, Yongming; Yuan, Minglong; Chen, Haiyun

    2016-01-01

    Antimicromial and antioxidant bioactive films based on poly(lactic acid)/poly(trimenthylene carbonate) films incorporated with different concentrations of oregano essential oil (OEO) were prepared by solvent casting. The antimicrobial, antioxidant, physical, thermal, microstructural, and mechanical properties of the resulting films were examined. Scanning electron microscopy analysis revealed that the cross-section of films became rougher when OEO was incorporated into PLA/PTMC blends. Differential scanning calorimetry analysis indicated that crystallinity of PLA phase decreased by the addition of OEO, but this did not affect the thermal stability of the films. Water vapor permeability of films slightly increased with increasing concentration of OEO. However, active PLA/PTMC/OEO composite films showed adequate barrier properties for food packaging application. The antimicrobial and antioxidant capacities were significantly improved with the incorporation of OEO (p < 0.05). The results demonstrated that an optimal balance between the mechanical, barrier, thermal, antioxidant, and antimicrobial properties of the films was achieved by the incorporation of 9 wt % OEO into PLA/PTMC blends. PMID:27240336

  16. Fabrication of a novel bone ash-reinforced gelatin/alginate/hyaluronic acid composite film for controlled drug delivery.

    Alemdar, Neslihan

    2016-10-20

    In this study, a novel pH-sensitive composite film with enhanced thermal and mechanical properties was prepared by the incorporation of bone ash at varying concentrations from 0 to 10v.% into gelatin/sodium alginate/hyaluronic acid (Gel/SA/HyA) polymeric structure for colon-specific drug delivery system. Films were characterized by FT-IR, SEM, and XRD analyses. Thermal and mechanical performances of films were determined by DSC, TGA and universal mechanical tester, respectively. Results proved that thermal stability and mechanical properties of bone ash-reinforced composite films improved significantly with respect to that of neat Gel/SA/HyA film. Cytotoxicity assay for composite films was carried out by using L929 cells. Water uptake capacity of films was determined by swelling test. Herein, release experiments of 5-Fluorouracil (5-FU) were performed in two different solutions (pH 2.1 and 7.4). The results assured that Gel/SA/HyA film containing BA could be considered as a potential biomaterial for controlled drug delivery systems. PMID:27474650

  17. Characterization of Active Packaging Films Made from Poly(Lactic Acid/Poly(Trimethylene Carbonate Incorporated with Oregano Essential Oil

    Dong Liu

    2016-05-01

    Full Text Available Antimicromial and antioxidant bioactive films based on poly(lactic acid/poly(trimenthylene carbonate films incorporated with different concentrations of oregano essential oil (OEO were prepared by solvent casting. The antimicrobial, antioxidant, physical, thermal, microstructural, and mechanical properties of the resulting films were examined. Scanning electron microscopy analysis revealed that the cross-section of films became rougher when OEO was incorporated into PLA/PTMC blends. Differential scanning calorimetry analysis indicated that crystallinity of PLA phase decreased by the addition of OEO, but this did not affect the thermal stability of the films. Water vapor permeability of films slightly increased with increasing concentration of OEO. However, active PLA/PTMC/OEO composite films showed adequate barrier properties for food packaging application. The antimicrobial and antioxidant capacities were significantly improved with the incorporation of OEO (p < 0.05. The results demonstrated that an optimal balance between the mechanical, barrier, thermal, antioxidant, and antimicrobial properties of the films was achieved by the incorporation of 9 wt % OEO into PLA/PTMC blends.

  18. Effect of complex amino acid imbalance on growth of tumor in tumor-bearing rats

    Yin-Cheng He; Yuan-Hong Wang; Jun Cao; Ji-Wei Chen; Ding-Yu Pan; Ya-Kui Zhou

    2003-01-01

    AIM: To investigate the effect of complex amino acid imbalance on the growth of tumor in tumor-bearing (TB) rats.METHODS: Sprague-Dawlley (SD) rats underwent jejunostomy for nutritional support. A suspension of Walker256 carcinosarcoma cells was subcutaneously inoculated.TB rats were randomly divided into groups A, B, C and D according to the formula of amino acids in enteral nutritional solutions, respectively. TB rats received jejunal feedings supplemented with balanced amino acids (group A),methionine-depleted amino acids (group B), valine-depleted amino acids (group C) and methionine- and valine-depleted complex amino acid imbalance (group D) for 10 days. Tumor volume, inhibitory rates of tumor, cell cycle and life span of TB rats were investigated.RESULTS: The G0/G1 ratio of tumor cells in group D (80.5±9.0) % was higher than that in groups A, B and C which was 67.0±5.1 %, 78.9±8.5 %, 69.2±6.2 %, respectively (P<0.05). The ratio of S/G2M and PI in group D were lower than those in groups A, B and C. The inhibitory rate of tumor in groups B, C and D was 37.2 %, 33.3 % and 43.9 %,respectively (P<0.05). The life span of TB rats in group D was significantly longer than that in groups B, C, and A.CONCLUSION: Methionine/valine-depleted amino acid imbalance can inhibit tumor growth. Complex amino acids of methionine and valine depleted imbalance have stronger inhibitory effects on tumor growth.

  19. Stability study of polyacrylic acid films plasma-polymerized on polypropylene substrates at medium pressure

    Plasma polymerization of acrylic acid has become an interesting research subject, since these coatings are expected to be beneficial for biomedical applications due to their high surface density of carboxylic acid functional groups. However, the application of these monomers is counteracted by their low stability in humid environments, since a high stability is a required characteristic for almost any biological application. The present work investigates whether it is possible to obtain stable deposits with a high retention of carboxylic acid functions by performing plasma polymerization on polypropylene substrates with a dielectric barrier discharge operating at medium pressure. In order to obtain coatings with the desired properties, the plasma parameters need to be optimized. Therefore, in this paper, the influence of discharge power and location of the substrate in the discharge chamber is examined in detail. The properties of the deposited films are studied using contact angle measurements, X-ray photoelectron spectroscopy, atomic force microscopy and Fourier transform infrared spectroscopy. Moreover, to determine whether the obtained deposits are soluble in water, the coatings are once again analyzed after rinsing in water. This paper will clearly show that stable COOH-rich surfaces can be obtained at high discharge power and close to the monomer inlet, which might open perspectives for future biomedical applications.

  20. Double-decker phthalocyanine complex: Scanning tunneling microscopy study of film formation and spin properties

    Komeda, Tadahiro; Katoh, Keiichi; Yamashita, Masahiro

    2014-05-01

    We review recent studies of double-decker and triple-decker phthalocyanine (Pc) molecules adsorbed on surfaces in terms of the bonding configuration, electronic structure and spin state. The Pc molecule has been studied extensively in surface science. A Pc molecule can contain various metal atoms at the center, and the class of the molecule is called as metal phthalocyanine (MPc). If the center metal has a large radius, like as lanthanoid metals, it becomes difficult to incorporate the metal atom inside of the Pc ring. Pc ligands are placed so as to sandwich the metal atom, where the metal atom is placed out of the Pc plane. The molecule in this configuration is called as a multilayer-decker Pc molecule. After the finding that the double-decker Pc lanthanoid complex shows single-molecule magnet (SMM) behavior, it has attracted a large attention. This is partly due to a rising interest for the ‘molecular spintronics’, in which the freedoms of spin and charge of an electron are applied to the quantum process of information. SMMs represent a class of compounds in which a single molecule behaves as a magnet. The reported blocking temperature, below which a single SMM molecule works as an quantum magnet, has been increasing with the development in the molecular design and synthesis techniques of multiple-decker Pc complex. However, even the bulk properties of these molecules are promising for the use of electronic materials, the films of multi-decker Pc molecules is less studied than those for the MPc molecules. An intriguing structural property is expected for the multi-decker Pc molecules since the Pc planes are linked by metal atoms. This gives an additional degree of freedom to the rotational angle between the two Pc ligands, and they can make a wheel-like symmetric rotation. Due to a simple and well-defined structure of a multi-decker Pc complex, the molecule can be a model molecule for molecular machine studies. The multi-decker Pc molecules can provide

  1. CdS thin films obtained by thermal treatment of cadmium(II) complex precursor deposited by MAPLE technique

    Rotaru, Andrei [INFLPR - National Institute for Laser, Plasma and Radiation Physics, PPAM - Lasers Department, 409 Atomistilor Bvd., Magurele RO-077125, Bucharest (Romania); Mietlarek-Kropidlowska, Anna [Gdansk University of Technology, Chemistry Faculty, 11/12 G. Narutowicza Str., PL-90-233 Gdansk (Poland); Constantinescu, Catalin, E-mail: catalin.constantinescu@inflpr.ro [INFLPR - National Institute for Laser, Plasma and Radiation Physics, PPAM - Lasers Department, 409 Atomistilor Bvd., Magurele RO-077125, Bucharest (Romania); Scarisoreanu, Nicu; Dumitru, Marius [INFLPR - National Institute for Laser, Plasma and Radiation Physics, PPAM - Lasers Department, 409 Atomistilor Bvd., Magurele RO-077125, Bucharest (Romania); Strankowski, Michal [Gdansk University of Technology, Chemistry Faculty, 11/12 G. Narutowicza Str., PL-90-233 Gdansk (Poland); Rotaru, Petre [University of Craiova, Faculty of Physics, 13 A.I. Cuza St., Craiova RO-200585, Dolj (Romania); Ion, Valentin [INFLPR - National Institute for Laser, Plasma and Radiation Physics, PPAM - Lasers Department, 409 Atomistilor Bvd., Magurele RO-077125, Bucharest (Romania); Vasiliu, Cristina [INOE 2000 - National Institute for Optoelectronics, 1 Atomistilor Bvd., Magurele RO-077125, Bucharest (Romania); Becker, Barbara [Gdansk University of Technology, Chemistry Faculty, 11/12 G. Narutowicza Str., PL-90-233 Gdansk (Poland); Dinescu, Maria [INFLPR - National Institute for Laser, Plasma and Radiation Physics, PPAM - Lasers Department, 409 Atomistilor Bvd., Magurele RO-077125, Bucharest (Romania)

    2009-05-15

    Thin films of [Cd{l_brace}SSi(O-Bu{sup t}){sub 3}{r_brace}(S{sub 2}CNEt{sub 2})]{sub 2}, precursor for semiconducting CdS layers, were deposited on silicon substrates by Matrix-Assisted Pulsed Laser Evaporation (MAPLE) technique. Structural analysis of the obtained films by Fourier transform infrared spectroscopy (FTIR) confirmed the viability of the procedure. After the deposition of the coordination complex, the layers are manufactured by appropriate thermal treatment of the system (thin film and substrate), according to the thermal analysis of the compound. Surface morphology of the thin films was investigated by atomic force microscopy (AFM) and spectroscopic-ellipsometry (SE) measurements.

  2. Studies on vanadium salicyl hydroxamic acid complexes - a 1:4 metal-ligand system

    Vanadium reacts with salicyl hydroxamic acid to form a blue-violet coloured complex with lambdasub(max) at 475 nm at pH 3.3. The metal-ligand ratio in the complex is 1:4. The step-wise formation constants of the complexes have been evaluated by Yatsimirskii's and Leden's graphical extrapolation methods from extractive photometric data. The values from log K1, log K3 and log K2, and log K4 are 3.65 +- 0.05, 2.50 +- 0.05, 2.30 +- 0.05 and 2.15 +- 0.05 respectively. (author)

  3. Decomposition Reaction of Zn-MPA(3-Mercaptopropionic Acid) Complex Under Microwave Irradiation

    JIAN Wen-ping; LIU Sheng; LI Jun; YANG Wen-sheng

    2008-01-01

    The thermal decomposition of Zn-MPA complex was investigated under microwave irradiation. ZnO and ZnS nanocrystals could be obtained by decomposing Zn-MPA(3-mercaptopropionic acid) complex under different reaction conditions. It was found that both the pH value of the solution and the molar ratio of Zn2+ and MPA can play an important role in the formation of ZnO and ZnS nanocrystals. MPA mainly acts as an S source or as a complexing agent.This study provides a new route for the controllable preparation of semiconductor nanocrystals.

  4. Synthesis and structural studies of some trivalent lanthanide complexes of isonicotinic acid hydrazide

    Trivalent lanthanides have been found to form complexes with isonicotinic acid hydrazide (INH) of the type M(INH)3X3 [X=Cl, SCN; M=La(III), Pr(III), Nd(III), Sm(III) and Gd(III)]. The complexes have been characterized by elemental analysis, molar conductance, magnetic susceptibility, infrared and electronic spectral studies. The nephelauxetic ratio (β), covalency (δ) and bonding parameter (b1/1) have been calculated from the electronic spectra. Infrared spectral studies reveal that INH acts as a neutral bidentate chelating ligand in all the complexes and that thiocyanate is N-bonded. (author)

  5. [The favorable effect of humic acid based complex micro-element preparations in cadmium exposure].

    Hudák, A; Náray, M; Nagy, I; Molnár, M; Gömöry, I; Ungváry, G

    1997-06-01

    The authors have studied the effect of consumption of a humic acid based complex microelement preparation (potassium, magnesium, iron, zinc, manganese, copper, vanadium, cobalt, molibden, selenium bound to humic acids) for six weeks (10 ml daily) on the biological exposure indices (blood and urine cadmium levels) and clinical laboratory parameters (liver and kidney tests, blood picture) of men (n = 18; 39.7 +/- 10.4 years of age;) working in cadmium exposure for 8.3 +/- 5.0 years. The initial mean blood and urine cadmium levels of the non-smoking subjects was twice higher than that of the non-smoking male controls living in the same urban area (n = 35), and significantly correlated with the length of exposure. Their mean serum alanin-aminotransferase, gamma-glutamyl-transferase, creatinine, uric acid and urinary N-acetyl-beta-D-glucosaminidase levels were significantly higher than that of the controls. After the six-week treatment blood cadmium level, activity of serum alanin-aminotransferase, serum uric acid and urinary protein concentrations decreased significantly, the abnormal serum iron levels normalized. According to this results, the absorption of cadmium decreased on the effect of the complex microelement supplementation and the adverse laboratory changes attributable partly to cadmium exposure improved. Therefore humic acid based complex microelement supplementation is recommended as an effective tool for prevention and health protection in occupational cadmium exposure as well as for smokers known to be considerably burdened by cadmium. PMID:9254361

  6. Electrocatalytic oxidation and voltammetric determination of ciprofloxacin employing poly(alizarin red)/graphene composite film in the presence of ascorbic acid, uric acid and dopamine.

    Zhang, Xin; Wei, Youli; Ding, Yaping

    2014-07-01

    A glassy carbon electrode modified with poly(alizarin red)/electrodeposited graphene (PAR/EGR) composite film was prepared and applied to detect ciprofloxacin (CPFX) in the presence of ascorbic, uric acid and dopamine. The morphology and interface property of PAR/EGR films were examined by scanning electron microscopy (SEM) and electrochemical impedance spectroscopy (EIS). The electrocatalytic oxidation of CPFX on AR/EGR was investigated by cyclic voltammetry (CV) and differential pulse voltammetry (DPV). The linearity ranged from 4 × 10(-8) to 1.2 × 10(-4) M with a detection limit (S/N=3) of 0.01 μM. The modified electrode could be applied to the individual determination of CPFX as well as the simultaneous determination of CPFX, ascorbic acid, uric acid and dopamine. This method proved to be a simple, selective and rapid way to determine CPFX in pharmaceutical preparation and biological media. PMID:24952626

  7. Activity of Picolinic Acid in Combination with the Antiprotozoal Drug Quinacrine against Mycobacterium avium Complex

    Shimizu, Toshiaki; Tomioka, Haruaki

    2006-01-01

    We studied the in vitro and in vivo antimicrobial activities of picolinic acid (PA) in combination with the antiprotozoal drug quinacrine against intramacrophage Mycobacterium avium complex (MAC). Quinacrine significantly potentiated the anti-MAC activity of PA, suggesting the usefulness of this combination in the clinical control of MAC infection.

  8. Oxalic acid complexes: Promising draw solutes for forward osmosis (FO) in protein enrichment

    Ge, Qingchun

    2015-01-01

    Highly soluble oxalic acid complexes (OACs) were synthesized through a one-pot reaction. The OACs exhibit excellent performance as draw solutes in FO processes with high water fluxes and negligible reverse solute fluxes. Efficient protein enrichment was achieved. The diluted OACs can be recycled via nanofiltration and are promising as draw solutes.

  9. Influence of solvent on proton transport in complexes of pyridine alkalines with trifluoroacetic acid

    The influence of solvent on proton transport in complexes of pyridine alkalines with trifluoroacetic acid was studied by nuclear magnetic resonance. The values of proton chemical shift are given. The influence of solution strength on chemical shift is also presented. (A.S.)

  10. Synthesis and Spectroscopic studies on cadmium halide complexes of isonicotinic acid

    In this study infrared spectra (4000-400cm-1) are reported for the cadmium(II) halide isonicotinic acid complexes. Vibrational assignments are given for all observed bands. Some structure spectra correlations and frequency shifts were found. It's found the frequency shifts depends on the halogen for a given metal. Certain chemical formulas were determined using elemental analysis results

  11. Zirconium complexes with lactic acid in the solution and solid states

    Demkowicz, Paul Andrew

    Lactic acid complexes of zirconium are used in a great number of industrial applications. Among these is their use as crosslinking agents for hydraulic fracturing fluids used in secondary oil recovery operations. Because of a poor understanding of zirconium lactate complex chemistry and crosslinking reactions, however, the design of superior fluid systems is often not guided by sound chemical principles and leads to empirical guesswork. Zirconium lactate solutions were characterized using Fourier transform infrared (FT-IR) spectroscopy, 1H, 13C, and 17O nuclear magnetic resonance (NMR) spectroscopy, and potentiometry. The results indicate that lactic acid is coordinated bidentate to zirconium via the alcohol and carboxylate groups. The average number of lactate ligands per zirconium ion is approximately 2 and is demonstrated to be relatively constant from pH 4--9. The lability of the lactate complexes increases as the pH is decreased. The NMR data reveal that there are both large and small complex molecules present in solution, with the size of the complex depending on the extent of zirconium hydrolysis. Large complexes consist of lactic acid coordinated to polynuclear zirconium hydroxy ions. The molecular size of these complexes is sufficient to hinder their tumbling in solution and cause broadening of the measured NMR signals. Small complexes involve lactic acid coordinated to hydroxylated species containing fewer zirconium ions, such that the rotational motion in solution is sufficiently rapid to result in narrow NMR signals. Zirconium lactate complexes were precipitated from solution and analyzed in the solid state using FT-IR spectroscopy, 13C magic angle spinning (MAS) NMR spectroscopy, elemental analysis, thermal gravitational analysis, and x-ray diffraction. Two distinct types of crystalline compounds were synthesized with four lactate ligands per zirconium ion. The coordination of lactic acid to zirconium is different in the two compounds, with one showing

  12. Surface complexation modeling of uranium (Vi) retained onto zirconium diphosphate in presence of organic acids

    In the field of nuclear waste disposal, predictions regarding radionuclide migration through the geosphere, have to take account the effects of natural organic matter. This work presents an investigation of interaction mechanisms between U (Vi) and zirconium diphosphate (ZrP2O7) in presence of organic acids (citric acid and oxalic acid). The retention reactions were previously examined using a batch equilibrium method. Previous results showed that U (Vi) retention was more efficient when citric acid or oxalic acid was present in solid surface at lower ph values. In order to determine the retention equilibria for both systems studied, a phosphorescence spectroscopy study was carried out. The experimental data were then fitted using the Constant Capacitance Model included in the FITEQL4.0 code. Previous results concerning surface characterization of ZrP2O7 (surface sites density and surface acidity constants) were used to constraint the modeling. The best fit for U (Vi)/citric acid/ZrP2O7 and U (Vi)/oxalic acid/ZrP2O7 systems considered the formation of a ternary surface complex. (Author)

  13. Structural and ionic conductivity behavior in hydroxypropylmethylcellulose (HPMC) polymer films complexed with sodium iodide (NaI)

    Rani, N. Sandhya; Sannappa, J.; Demappa, T.; Mahadevaiah

    2013-02-01

    Solid polymer electrolyte films based on Hydroxypropylmethylcellulose (HPMC) complexed with Sodium Iodide (NaI) were prepared using solution cast method. The dissolution of the salt into the polymer host and the micro structural properties of pure and NaI complexed HPMC polymer electrolyte films were confirmed by X - Ray diffraction (XRD) studies. The XRD results revealed that the amorphous domains of HPMC polymer matrix was increased with increase in the NaI salt concentration. The degree of crystallanity and crystallite size is high for pure HPMC samples. Direct current (dc) conductivity was measured in the temperature range of 313-383k. Temperature dependence of dc electrical conductivity and activation energy regions data indicated the dominance of ion type charge transport in these polymer electrolyte films.

  14. Methods of staining target chromosomal DNA employing high complexity nucleic acid probes

    Gray, Joe W.; Pinkel, Daniel; Kallioniemi, Ol'li-Pekka; Kallioniemi, Anne; Sakamoto, Masaru

    2006-10-03

    Methods and compositions for staining based upon nucleic acid sequence that employ nucleic acid probes are provided. Said methods produce staining patterns that can be tailored for specific cytogenetic analyses. Said probes are appropriate for in situ hybridization and stain both interphase and metaphase chromosomal material with reliable signals. The nucleic acid probes are typically of a complexity greater than 50 kb, the complexity depending upon the cytogenetic application. Methods and reagents are provided for the detection of genetic rearrangements. Probes and test kits are provided for use in detecting genetic rearrangements, particularly for use in tumor cytogenetics, in the detection of disease related loci, specifically cancer, such as chronic myelogenous leukemia (CML), retinoblastoma, ovarian and uterine cancers, and for biological dosimetry. Methods and reagents are described for cytogenetic research, for the differentiation of cytogenetically similar but genetically different diseases, and for many prognostic and diagnostic applications.

  15. Investigation of complexing reactions of terbium(3) ions with anions of salicylic and 5-sulfosalicylic acids in aqueous solutions

    Complexing of terbium(3) ions with anions of salicylic and 5-sulfosalicylic acids was investigated by luminescence-kinetic method. Values of stability and dissociation constants of formed complexes were obtained

  16. Electrochemical synthesis of FeS2 thin film: An effective material for peroxide sensing and terephthalic acid degradation

    Electrochemically FeS2 thin films have been synthesized on ITO substrates at room temperature (25 °C). UV–Vis, X-ray diffraction (XRD) and field emission scanning electron microscope (FESEM) were used for the characterization of nanostructure FeS2 thin films. Two probe I–V measurements convey that the material is p type and a p-n junction (diode) was found to be developed between FeS2 and ITO layer. Cyclic voltametry study shows that FeS2/ITO electrode facilitates the reduction of hydrogen peroxide and exhibits excellent electro-catalytic activity towards its sensing. Photocatalytic study reveals that the synthesized thin films are also efficient to degrade terephthalic acid (TA). - Graphical abstract: Electrochemically FeS2 thin films have been synthesized on ITO substrate. The synthesized material is effective for the reduction of H2O2 and the sensitivity of the material is strongly dependent on pH and temperature. Photocatalytic study reveals that the material is quite effective towards decomposition of terephthalic acid. These results indicate that the material can play a dual role as pollutant cleanup for environmental interest. - Highlights: • Electrochemically FeS2 thin films are synthesized. • The material is effective to sense the H2O2 and degrade terephthalic acid. • It plays a dual role as pollutant cleanup for environmental interest

  17. Electrochemical synthesis of FeS{sub 2} thin film: An effective material for peroxide sensing and terephthalic acid degradation

    Jana, Sumanta [Department of Chemistry, Indian Institute of Engineering Science and Technology, Shibpur, Howrah, 711103 WB (India); Mondal, Palash; Tripathi, Subhankar [Department of Chemistry, Vivekananda Mahavidyalaya, Burdwan, 713103 WB (India); Mondal, Anup [Department of Chemistry, Indian Institute of Engineering Science and Technology, Shibpur, Howrah, 711103 WB (India); Chakraborty, Biswajit, E-mail: biswajitmailbag@gmail.com [Department of Chemistry, Vivekananda Mahavidyalaya, Burdwan, 713103 WB (India)

    2015-10-15

    Electrochemically FeS{sub 2} thin films have been synthesized on ITO substrates at room temperature (25 °C). UV–Vis, X-ray diffraction (XRD) and field emission scanning electron microscope (FESEM) were used for the characterization of nanostructure FeS{sub 2} thin films. Two probe I–V measurements convey that the material is p type and a p-n junction (diode) was found to be developed between FeS{sub 2} and ITO layer. Cyclic voltametry study shows that FeS{sub 2}/ITO electrode facilitates the reduction of hydrogen peroxide and exhibits excellent electro-catalytic activity towards its sensing. Photocatalytic study reveals that the synthesized thin films are also efficient to degrade terephthalic acid (TA). - Graphical abstract: Electrochemically FeS{sub 2} thin films have been synthesized on ITO substrate. The synthesized material is effective for the reduction of H{sub 2}O{sub 2} and the sensitivity of the material is strongly dependent on pH and temperature. Photocatalytic study reveals that the material is quite effective towards decomposition of terephthalic acid. These results indicate that the material can play a dual role as pollutant cleanup for environmental interest. - Highlights: • Electrochemically FeS{sub 2} thin films are synthesized. • The material is effective to sense the H{sub 2}O{sub 2} and degrade terephthalic acid. • It plays a dual role as pollutant cleanup for environmental interest.

  18. Grafting of acrylic acid onto polypropylene films irradiated with argon ions

    Polypropylene (PP) foils were irradiated with 100 keV energy Argon ions at different fluences ranging from 1012 up to 2 x 1015 cm-2 and then grafted with acrylic acid (AA). The grafting yield was measured by weight difference and the structural changes on the films were analysed using Fourier transform infrared spectroscopy (FTIR). Different parameters that determined the grafting process such us fluence, grafting time and monomer concentration were analysed. The grafting reached an optimum value at 79% in aqueous solution at 30 min grafting time. The grafting yield as a function of the ion fluence plot, presented a maximum value, as previously found in a study of heavy beam on polymers

  19. Separation and PurificationHomologous Compounds byof Dodecanedioic Acid from Its Falling Film Crystallization

    李裕; 刘有智; 齐雪琴

    2004-01-01

    Separation and purification of dodecanedioic acid (DDDA) from its homologous compounds were studied experimentally by falling film crystallization (FFC). The influences of various operation parameters, including crystallizing time, flow rate of melt and temperature of glycerine bath, on purity of DDDA and crystallizing rate were investigated. Over 99% (by mole) DDDA was obtained for a feed composition of 96% (by mole). The main factors affecting the separation efficiency are flow rate of melt and temperature of glycerine bath. The crystallizing layer of DDDA was further purified by sweating and blasting. A set of optimized operation data are provided for better understanding the mechanism of heat and mass transfer in FFC, and for further industrial application of DDDA purification process.

  20. Flexible, all-organic ammonia sensor based on dodecylbenzene sulfonic acid-doped polyaniline films

    A stable chlorobenzene dispersion of conducting polyaniline (PANI) has been obtained by doping emeraldine base with dodecylbenzene sulfonic acid (DBSA) and studied by spectrophotometric measurements in the UV-vis-IR range. The electrical properties of PANI: DBSA films obtained from the above dispersion have been investigated under different temperature and relative humidity conditions. All-organic chemoresistive devices have been developed by spin-coating the PANI: DBSA dispersion on flexible substrates, and then by depositing electrodes on the top, from a carbon nanotube conducting ink. Sensing tests performed under exposition to calibrated amounts of ammonia reveal that these simple and inexpensive sensors are able to detect ammonia at room temperature in a reliable way, with a sensitivity linearly related to concentration in the range between 5 ppm and 70 ppm.

  1. Holographic gratings recorded in poly(lactic acid)/azo-dye films

    Cambiasso, Javier; Goyanes, Silvia; Ledesma, Silvia

    2015-09-01

    Diffraction gratings were recorded in biodegradable polymer films of poly(lactic acid) doped with the photoisomerisable azo-dye (Disperse Orange 3). It is shown that the diffraction efficiency of the recorded grating can be improved by 220% via an all-optical treatment. This all-optical treatment consists of a pre-irradiation of the sample with the writing laser beam at high power during a short period of time, preventing damage of the material, followed by a much longer inscription at relatively low power. Furthermore, it is shown that the addition of a small amount of 0.05 wt% of multi-walled carbon nanotubes to the photoresponsive polymer increases the maximum diffraction efficiency as well as the remanent efficiency by 20%. Finally, this last photoresponsive nano-composite is also sensitive to the pre-irradiation treatment.

  2. Investigation of neodymium complex with acid chrome blue K by beta-correction spectrophotometry

    The neodymium complex with acid chrome blue K (ACBK) at pH 10 has been studied in detail by beta-correction spectrophotometry. The cationic surfactant, cetyltrimethylammonium bromide (CTAB) is useful for increasing the sensitivity and solubility of ligand and complex. The characteristic factors of complex are calculated, for example, complex ratio and stability constant. Results show that Nd(ACBK)3 is formed and its real not apparent molar absorptivity is the first to be determined as follows : ε520 Nd(ACBK)3 = 5.54 x 104 dm3 mol-1 cm-1 at pH 10. In addition, the cumulative stability constant of complex Nd(ACBK)3 is still computed to be 1.72 x 1016 in ionic strength 0.1 M and at temperature 15 deg. (author)

  3. Electrochemical determination of ascorbic acid at p-phenylenediamine film-holes modified glassy carbon electrode

    Olana Bikila Nagasa

    2015-01-01

    Full Text Available In this work the determination of ascorbic acid (AA at glassy carbon electrode (GCE modified with a perforated film produced by reduction of diazonium generated in situ from p-phenylenediamine (PD is reported. Holes were intentionally created in the modifier film by stripping a pre-deposited gold nanoparticles. The modified electrodes were electrochemically characterized by common redox probes: hydroquinone, ferrocyanide and hexamineruthenium(III. The cyclic voltammetric and amperometric response of AA using the modified electrodes was compared with that of bare GCE. The bare GCE showed a linear response to AA in the concentration range of 5 mM to 45 mM with detection limit of 1.656 mM and the modified GCE showed a linear response to AA in the concentration range of 5 μM to 45 μM with detection limit of 0.123 μM. The effect of potential intereferents on amperometric signal of AA at the modified GCE was examined and found to be minimal. The inter-electrode reproducibility, stability, and accuracy were determined. The modified electrode showed excellent inter-electrode reproducibility, accuracy and stability. The modified electrode reported is a promising candidate for use in electroanalysis of AA.

  4. Antimicrobial Hyaluronic Acid-Cefoxitin Sodium Thin Films Produced by Electrospraying.

    Ahire, Jayesh J; Dicks, Leon M T

    2016-08-01

    The healing properties of hyaluronic acid (HA) in the recovery of wounds are well known. Cefoxitin (Cef), a cephalosporin antibiotic, is generally used to prevent and treat postoperative infections. In this study, we describe the incorporation of Cef in HA thin films (Cef-HAF) by using electrospraying. Scanning electron microscopy images showed that HA-containing thin films (HAF) were composed of numerous nanoparticles (255 ± 177 nm in diameter) with irregular surfaces, connected to each other with nanofibers of 50 ± 11 nm in diameter. Cef-HAF contained fewer, but larger, particles (551 ± 293 nm) with smooth surfaces and were interconnected with nanofibers of 61 ± 13 nm in diameter. Differences in surface morphology between HAF and Cef-HAF were confirmed by atomic force microscopy. Fourier transform infrared and X-ray diffraction analyses revealed that Cef was not modified when incorporated into Cef-HAF and remained active against Klebsiella pneumoniae Xen 39, Staphylococcus aureus Xen 36 and Listeria monocytogenes EDGe. Nanofiber scaffolds of HA-containing Cef may be used in dressings to control postoperative infections. PMID:27146506

  5. Transfer molding processes for nanoscale patterning of poly-L-lactic acid (PLLA) films

    Dhakal, Rabin; Peer, Akshit; Biswas, Rana; Kim, Jaeyoun

    2016-03-01

    Nanoscale patterned structures composed of biomaterials exhibit great potential for the fabrication of functional biostructures. In this paper, we report cost-effective, rapid, and highly reproducible soft lithographic transfer-molding techniques for creating periodic micro- and nano-scale textures on poly (L-lactic acid) (PLLA) surface. These artificial textures can increase the overall surface area and change the release dynamics of the therapeutic agents coated on it. Specifically, we use the double replication technique in which the master pattern is first transferred to the PDMS mold and the pattern on PDMS is then transferred to the PLLA films through drop-casting as well as nano-imprinting. The ensuing comparison studies reveal that the drop-cast PLLA allows pattern transfer at higher levels of fidelity, enabling the realization of nano-hole and nano-cone arrays with pitch down to ~700 nm. The nano-patterned PLLA film was then coated with rapamycin to make it drug-eluting.

  6. Probing inclusion complexes of cyclodextrins with amino acids by physicochemical approach.

    Roy, Mahendra Nath; Roy, Aditi; Saha, Subhadeep

    2016-10-20

    Formations of host-guest inclusion complexes of two natural amino acids, viz., l-Leucine and l-Isoleucine as guests with α and β-cyclodextrins have been investigated which include diverse applications in modern science such as controlled delivery in the field of pharmaceuticals, food processing etc. Surface tension and conductivity studies establish the formation of inclusion complexes with 1:1 stoichiometry. The interactions of cyclodextrins with amino acids have been supported by density, viscosity, refractive index, hydration and solvation number measurements indicating higher degree of inclusion in case of α-cyclodextrin. l-Leucine interacts more with the hydrophobic cavity of cyclodextrin than its isomer. With the help of stability constant by NMR titration, hydrophobic effect, H-bonds and structural effects the formations of inclusion complexes have been explained. PMID:27474589

  7. Synthesis and physicochemical study of rhenium(V) complexes with phenylglyoxylic acid thiosemicarbazone

    With high yield (75-93 %) rhenium(V) complexes were prepared with thiosemicarbazone of phenylglyoxylic acid (L) of the composition [ReOLX3]·2H2O, [ReOL2X]X2·2H2O, [ReOLX2(OH)]·2H2O, [ReOL2(OH)]X2 (X = Cl, Br). The compounds prepared were characterized by the methods of elementary and thermal analyses, IR spectroscopy and conductometry. It was ascertained that depending on synthesis conditions, initial concentration of hydrohalic acid first of all, rhenium(V) complexes are formed with different number of ligands in the inner sphere. In all the complexes studied ligand L is coordinated by rhenium atom in bidentate way via sulfur and nitrogen atoms of hydrazine fragment, forming a five-member chelate node

  8. Competition effect of some metal ions on the complexation of strontium with humic acid. Vol. 4

    Interaction of radioactive strontium with humic acid present in water streams is of main importance to learn about the fate of strontium in case of accidental release. In this work, formation of Sr-humate precipitate was studied radiometrically and colorimetric at different PH's. The investigations indicated that formation of the precipitated complex increases with increasing strontium concentration till saturation. The competition effect of other cations in solution such as Ca, Mg, Ba, and Ni was investigated. The humate complexes of these cations were studied colorimetric, and the competition behaviour was investigated using the radiotracer of strontium. The results indicated that presence of Ba, Mg and Ni decreases the Sr-humate complex, while increasing Ca concentration enhances precipitation of Sr with humic acid. 10 figs

  9. Separation of glycols from dilute aqueous solutions via complexation with boronic acids

    Randel, L.A.; King, C.J.

    1991-07-01

    This work examines methods of separating low molecular weight glycols from dilute aqueous solution. Extraction into conventional solvents is generally not economical, since, in the literature reviewed, distribution ratios for the two- to four-carbon glycols are all less than one. Distribution ratios can be increased, however, by incorporating into the organic phase an extracting agent that will complex with the solute of interest. The extracting agent investigated in this work is 3-nitrophenylboronic acid (NPBA). NPBA, a boric acid derivative, reversibly complexes with many glycols. The literature on complexation of borate and related compounds with glycols, including mechanistic data, measurement techniques, and applications to separation processes, provides information valuable for designing experiments with NPBA and is reviewed herein. 88 refs., 15 figs., 24 tabs.

  10. Dye sensitized solar cell applications of CdTiO3-TiO2 composite thin films deposited from single molecular complex

    Ehsan, Muhammad Ali; Khaledi, Hamid; Pandikumar, Alagarsamy; Huang, Nay Ming; Arifin, Zainudin; Mazhar, Muhammad

    2015-10-01

    A heterobimetallic complex [Cd2Ti4(μ-O)6(TFA)8(THF)6]·1.5THF (1) (TFA=trifluoroacetato, THF=tetrahydrofuran) comprising of Cd:Ti (1:2) ratio was synthesized by a chemical reaction of cadmium (II) acetate with titanium (IV) isopropoxide and triflouroacetic acid in THF. The stoichiometry of (1) was recognized by single crystal X-ray diffraction, spectroscopic and elemental analyses. Thermal studies revealed that (1) neatly decomposes at 450 °C to furnish 1:1 ratio of cadmium titanate:titania composite oxides material. The thin films of CdTiO3-TiO2 composite oxides were deposited at 550 °C on fluorine doped tin oxide coated conducting glass substrate in air ambient. The micro-structure, crystallinity, phase identification and chemical composition of microspherical architectured CdTiO3-TiO2 composite thin film have been determined by scanning electron microscopy, X-ray diffraction, Raman spectroscopy and energy dispersive X-ray analysis. The scope of composite thin film having band gap of 3.1 eV was explored as photoanode for dye-sensitized solar cell application.

  11. Peat humic acids and their complex forming properties as influenced by peat humification

    Dudare, D.; Klavins, M.

    2012-04-01

    To study paleoenvironmental changes of importance is understanding of processes of organic matter diagenesis, especially changes of refractory part of natural organic substances - humic substances. Studies of the living organic matter humification process are also essential for understanding of the carbon biogeochemical cycle. The aim of this study was to analyze peat organic matter diagenesis: changes of properties of humic acids, relations between the humification process, properties of peat, peat humic acids, their ability to interact with metal ions, as well ability to accumulate metals. The analysis were carried out on samples of humic substances preparatively extracted from three ombrotrophic bog peat profiles to identify the links between peat age, decomposition and humification degree, botanical composition and properties of peat humic acids elemental (C, H, N, O), functional (-COOH, -OH) composition, structural characteristics - UV, fluorescence, FTIR. The found variability of peat properties is less significant than differences in the properties of peat-forming living matter, thus revealing the dominant impact of humification process on the properties of peat. Correspondingly, composition of peat humic acids is little affected by differences in the properties of precursor living organic material, and such indicators as decomposition degree, humification degree, humic acid elemental ratio and concentrations of acidic functional groups are the best descriptors of changes in organic matter during the process of organic matter diagenesis and humification. Peat ability to accumulate major and trace elements depends on the character of element supply, potency of metal ions to bind functionalities in the peat, with an emphasis on the structure of peat humic acid, pH reaction, oxygen presence, presence of complexing compounds, inorganic ions and many other factors. Major and trace element presence in peat is of importance as an indicator of peat genesis and

  12. Concentration of eicosapentaenoic acid (EPA and docosahexaenoic acid (DHA of Asian catfish oil by urea complexation: optimization of reaction conditions

    Pornpisanu Thammapat

    2016-04-01

    Full Text Available Optimization of the concentrating conditions of eicosapentaenoic acid (EPA and docosahexaenoic acid (DHA extracted from Asian catfish oil was studied to obtain a maximum concentration. The crude fish oil was extracted from the belly flap and adipose tissue of Asian catfish, and the extracted oil was used as fresh crude oil. The EPA and DHA were concentrated by the urea complexation method. A hexagonal rotatable design was applied to examine the effects of crystallization temperature and urea-to-fatty acid ratio on the total content of EPA and DHA (Y1 and the liquid recovery yield (Y2 . The second order polynomial regression models for Y1 and Y2 were employed to generate the response surfaces. Under the optimum conditions of -20 °C and a urea-to-fatty acid ratio of 4 (w/w, the total concentration of EPA and DHA could be increased by up to 88%, while a liquid recovery yield of 26% was obtained.

  13. Effects of acetic acid on microstructure and electrochemical properties of nano cerium oxide films coated on AA7020-T6 aluminum alloy

    H. Hasannejad; T. Shahrabi; M. Aliofkhazraei

    2009-01-01

    Nano cerium oxide films were applied on AA7020-T6 aluminum alloy and the effects of acetic acid concentration on the microstructure and electrochemical properties of the coated samples were investigated by using scanning electron microscopy (SEM), X-ray diffraction (XRD), crack-flee films with well-developed grains were obtained and grain sizes of the films decreased. Elimination of cracks and decreasing grain size of the nano cerium oxide films caused corrosion resistance to increase.

  14. Theoretical and experimental studies on the electronic, optical, and structural properties of poly-pyrrole-2-carboxylic acid films

    Highlights: • Novel approach for preparing a functionalized polypyrrole film. • Comparative experimental and theoretical results – conjugated polymers. • Accurate electronic, structural, and optical properties obtained for poly-pyrrole-2-carboxylic acid films. • Proposal of mechanism of electropolymerization of pyrrole-2-carboxylic acid films. - Abstract: A theoretical approach is used here to explain experimental results obtained from the electrosynthesis of polypyrrole-2-carboxylic acid (PPY-2-COOH) films in nonaqueous medium. An analysis of the Fukui function (reactivity index) indicates that the monomer (pyrrole-2-carboxylic acid, PY-2-COOH), and dimers and trimers are oxidized in the C4 or C5 positions of the heterocyclic ring of the PY-2-COOH structure. After calculating the heat of formation using semiempirical Austin Model 1 post-Hartree–Fock parameterization for dimer species, both C4 and C5 positions adjacent to the aromatic rings of PPY-2-COOH were considered the most susceptible ones to oxidative coupling reactions. The ZINDO-S/CI semiempirical method was used to simulate the electronic transitions typically seen in the UV–VIS–NIR range in monomer and oligomers with different conjugation lengths. The use of an electrochemical quartz crystal microbalance provides sufficient information to propose a polymerization mechanism of PY-2-COOH based on molecular modeling and experimental results

  15. Solid-phase synthesis of europium and terbium complexes of quinolinic acid

    The regularities of mechanochemical synthesis and spectral-luminescent properties of europium and terbium compounds with dicarboxylic quinoline acid were studied. The compounds Ln2(XH)3D · 2H2O, Ln = Eu3+, Tb3+, XH - quinoline acid anion, D - 1,10-phenanthroline, 2,2'-dipyridyl, diphenyl guanidine, benzotriazole were prepared. The synthesis of the europium and terbium complexes aqueous solutions was also conducted for comparison by the reaction of the rare earth chlorides(nitrates) with alcohol solution of the acid and neutral ligand. The data of element analysis and X-ray diffraction are given. IR-spectra and luminescence spectra of europium and quinoline acid synthesized as mechanochemically, so traditional method, are identical to each other

  16. Complexes of molybdenum (6) and tungsten (6) with amino- and pyridine carboxylic acids

    Spitsyn, V.I.; Mozgin, S.V.; Felin, M.G.; Subbotina, N.A.; Ajzenberg, M.I. (Moskovskij Gosudarstvennyj Univ. (USSR))

    1984-01-01

    By interaction of Na/sub 2/MO/sub 4/ with amino acid excess in muriatic medium the complexes Mo/sub 2/O/sub 4/ (OH)/sub 3/L (LH-anthranilic, nicotinic acids, histidine), Mo/sub 2/O/sub 5/ (OH)L' (L'H-..cap alpha..- and ..beta..-alanine, valine, isonicotinic acid), W/sub 3/O/sub 8/ (OH) (H/sub 2/O)/sub 4/ L'' (L'H-nicotinic, isonicotinic acids, histidine) are isolated. On the basis of the data of elementary analysis, IR spectroscopy and thermogravimetry assumptions on their composition and structure have been suggested.

  17. Effect of environmental factors on the complexation of iron and humic acid

    Kai Fang; Dongxing Yuan; Lei Zhang; Lifeng Feng; Yaojin Chen; Yuzhou Wang

    2015-01-01

    A method of size exclusion chromatography coupled with ultraviolet spectrophotometry and off-line graphite furnace atomic absorption spectrometry was developed to assess the complexation properties of iron (Fe) and humic acid (HA) in a water environment.The factors affecting the complexation of Fe and HA,such as ionic strength,pH,temperature and UV radiation,were investigated.The Fe-HA complex residence time was also studied.Experimental results showed that pH could influence the deprotonation of HA and hydrolysis of Fe,and thus affected the complexation of Fe and HA.The complexation was greatly disrupted by the presence of NaCl.Temperature had some influence on the complexation.The yield of Fe-HA complexes showed a small decrease at high levels of UV radiation,but the effect of UV radiation on Fe-HA complex formation at natural levels could be neglected.It took about 10 hr for the complexation to reach equilibrium,and the Fe-HA complex residence time was about 20 hr.Complexation of Fe and HA reached a maximum level under the conditions of pH 6,very low ionic strength,in the dark and at a water temperature of about 25℃,for 10 hr.It was suggested that the Fe-HA complex could form mainly in freshwater bodies and reach high levels in the warm season with mild sunlight radiation.With changing environmental parameters,such as at lower temperature in winter or higher pH and ionic strength in an estuary,the concentration of the Fe-HA complex would decrease.

  18. An interesting grafting reactivity of EB preirradiated polypropylene film[Radiation grafting; Polypropylene; Free radical; peroxide; Acrylic acid; Acrylamide

    Chen Jie E-mail: chenjjd@online.sh.cn; Yang Liming; Chen Liqin; Wu Minhong; Nho, Y.C.; Kaetsua, Isao

    2004-02-01

    An interesting grafting reactivity of electron beam preirradiated polypropylene (PP) film was found by grafting of acrylic acid (AAc) and acrylamide (AAm) repeatedly or intermittently. The preirradiated PP film could be grafted several times intermittently and the free radicals or peroxides on the samples could be determined after several times grafting reaction. The effects of storage time, reaction time and repeated reaction times on the degree of grafting were investigated. The trapped radicals, peroxy-radicals and peroxides on the preirradiated and reacted PP films were determined by using electron spin resonance (ESR) and 1,1-diphenyl-2-picryl hydrazyl (DPPH), respectively. An interpenetrating polymer networks (IPN) with both temperature and pH sensitive properties was obtained by two times grafting of AAm and AAc onto preirradiated PP film.

  19. MORPHOLOGICAL STUDY ON THE ORIENTED CHITOSAN FILM OBTAINED FROM PRE-SHEARED LIQUID CRYSTALLINE SOLUTION IN DICHLOROACETIC ACID

    Zhong-ming Hu; Li-heng Wu; Da-cheng Wu; Shou-xi Chen

    2001-01-01

    The oriented chitosan films obtained from pre-sheared liquid crystalline chitosan/dichloroacetic acid (DCA)solutions were studied by means of polarized optical microscopy (POM), scanning electron microscopy (SEM), infra-red dichroism technique and wide angle X-ray diffraction (WAXD). The shear induced band texture in the film was found to correspond to the sinusoidal fibrillar microstructure along the shearing direction on the basis of POM and SEM observations.The sinusoidal fibril was found to be lying within the film plane. The model of chitosan molecular orientation in the presheared film with band texture can be established assuming that the main chain orients in the shearing direction and the side group is perpendicular to the shearing direction. The WAXD azimuthal scanning at 2θ = 20° indicates that the (002) plane orients perpendicular to the shearing direction.``

  20. Fluorescence and Judd-Ofelt analysis of rare earth complexes with maleic anhydride and acrylic acid

    WEN Shipeng; ZHANG Xiaoping; HU Shui; ZHANG Liqun; LIU Li

    2008-01-01

    Two kinds of Eu-complexes, Eu(TTA)2(Phen)(AA) and Eu(TTA)2(Phen)(MA) (HTFA=2-Thenoyltrifluoroacetone, Phen=1,10-phenanthroline, AA=acrylic acid, MA=Maleic anhydride), which combined the excellent fluorescence properties of Eu(TTA)2(Phen)(H2O) and the reactivity of acrylic acid and maleic anhydride with radicals, were synthesized. The two complexes were characterized by elemental analysis, infrared (IR) spectra, and X-ray photoelectron spectroscopy (XPS). Based on the data shown from the fluorescent spectra of the Eu-MA and Eu-AA complexes, the Ωλ (λ=2 and 4) experimental intensity parameters were calculated. The results demonstrated that the Ω2 intensity parameters for the two complexes were smaller than those for the Eu(TTA)2(Phen)(H2O) complex, indicating that a less symmetri-cal chemical environment existed in the complexes. It implied that the radiative efficiency of the 5D0 of these two complexes could be en-hanced by ligand of MA and AA, respectively. The luminescent lifetime of the Eu-AA (τ=7.26×10-4 s) or Eu-MA complex (τ=-8.12×10-4 s) was higher than that of the Eu(TTA)2(Phen)(H2O) complex, which was attributed to the substitution of the water molecule (H2O) in Eu(TTA)2(Phen)(H2O) by the MA or AA ligand.