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PubMed1997

Electron transfer between myoglobin and electrodes in thin films of phosphatidylcholines and dihexadecylphosphate.

Myoglobin (Mb) in thin films of phosphatidyl cholines (PC) or dihexadecyl phosphate (DHP) gave direct, reversible electron transfer between pyrolytic graphite electrodes and the heme Fe(III)/Fe(II) redox couple of the protein. PC films incorporated much more Mb than DHP films. A model assuming several classes of electroactive sites in the films on the electrode with a dispersion of standard potentials successfully fit square-wave voltammetric data at pulse heights > 50 mV. Electron transfer rate constants in PC and DHP films were significantly larger than for Mb in thin films of an insoluble cationic surfactant. The pH dependence of the formal potential of Mb in the PC films suggested that protonation, possibly inducing conformational change, accompanies electron transfer to MbFe(III) between pH 5 and 11. Mb in PC films was used for catalysis of the reduction of trichloroacetic acid.

Animals↗
PubMed1999

Electrochemical generation of ferrylmyoglobin during oxidation of styrene with films of DNA and a poly (ester sulfonic acid) ionomer.

The chemistry of electrochemically-driven myoglobin-catalyzed oxidation of styrene was investigated in films of DNA or Eastman AQ ionomer on optically transparent electrodes. Conversion of styrene to styrene oxide proceeded via a ferrylmyoglobin radical intermediate. Ferrylmyoglobins were clearly detected by spectroelectrochemistry in films of 1-4 mm thick. The ferrylmyoglobin radical is produced by reaction of metmyoglobin (Mb) in the films with hydrogen peroxide formed by electrochemical catalytic reduction of oxygen catalyzed by Mb. Thus, electrochemically-driven styrene oxidation with these films proceeds by a 'doubly catalytic' electrode-driven reduction-oxidation pathway. Ferrylmyoglobin formation during electrolysis of Mb-DNA films in aerobic solutions was much faster, and styrene oxidation occurred with less Mb decomposition compared to the Mb-AQ films. The better performance of Mb-DNA films is correlated with a larger fraction of electroactive Mb and better stability than for the Mb-AQ films.

Animals↗
PubMed1999

Direct electron transfer for hemoglobin in biomembrane-like dimyristoyl phosphatidylcholine films on pyrolytic graphite electrodes.

Stable thin films made from dimyristoyl phosphatidylcholine (DMPC) with incorporated hemoglobin (Hb) on pyrolytic graphite (PG) electrodes were characterized by electrochemical and other techniques. Cyclic voltammetry (CV) of Hb-DMPC films showed a pair of well-defined and nearly reversible peaks at about -0.27 V vs. saturated calomel electrode (SCE) at pH 5.5, characteristic of Hb heme Fe(III)/Fe(II) redox couple. The electron transfer between Hb and PG electrodes was greatly facilitated in DMPC films. Apparent heterogeneous rate constants (ks) were estimated by fitting square wave voltammograms of Hb-DMPC films to a model featuring thin layer behavior and dispersion of formal potentials for redox center. The formal potential of Hb heme Fe(III)/Fe(II) couple in DMPC films shifted linearly between pH 4.5 to 11 with a slope of -48 mV pH-1, suggesting that one proton is coupled to each electron transfer in the electrochemical reaction. Soret absorption band positions suggest that Hb retains a near native conformation in DMPC films at medium pH. Differential scanning calorimetry (DSC) showed the phase transition for DMPC and Hb-DMPC films, suggesting DMPC has an ordered multibilayer structure. Trichloroacetic acid (TCA) was catalytically reduced by Hb-DMPC films with significant decreases in the electrode potential required.

Algorithms↗
PubMed1999

Fast reversible electron transfer for photosynthetic reaction center from wild type Rhodobacter sphaeroides re-constituted in polycation sandwiched monolayer film.

Direct reversible electron transfer for photosynthetic reaction center from wild type Rhodobacter sphaeroides re-constituted in polycation sandwiched monolayer film was observed in this work. The redox potential E0' = 0.46 V vs. NHE for first primary donor redox couple P/P+ was accurately measured from reversible CV or SWV peaks, which were quite close to those obtained from optic redox titration method. Reaction center (RC) in film was found re-constituted in such an ordered way that the orientation of RC favored the electron transfer in film. Thus, the protein electroactivity seems to be turned on in this artificial biomimic thin film. Furthermore, RC in the film features a photo-induced redox-peak fluctuation, suggesting an intact and functional state for RC in such film. Redox peaks were also found dependent of pH, implying a proton-coupled electron transfer occurring in film. Charge recombination was observed accompanied with change of electrochemical driving force. Electrochemical model assuming several classes of electroactive sites in the films on the electrode with a dispersion of standard potentials successfully fits SWV experimental data at different pulse height and frequency.

Electrochemistry↗
PubMed2003

Preparation of flat carbon support films.

Wrinkling of carbon support films is known to limit the resolution of electron microscopy images of protein two-dimensional crystals. The origin of carbon wrinkling during preparation of the support films was investigated by reflected light microscopy. We observed that carbon films go through several states during their preparation. While dried carbon films have a tendency to be wrinkled, a flat state is observed transiently before complete drying. This state could be stabilized by the addition of sugars or tannic acid to the embedding medium. An alternative method for preparing flat carbon films was developed, in which a sandwich is formed by two symmetrical carbon films positioned on both sides of a grid. The formation of sandwiched carbon films was facilitated by the use of grids with thin bars. The carbon sandwich films were flat, stable, and easily and reproducibly prepared.

Carbohydrates↗
PubMedDate not supplied

Nanotribological characterization of molecularly thick lubricant films for applications to MEMS/NEMS by AFM.

Molecularly thick perfluoropolyether (PFPE) films are considered to be good protective films for micro/nanoelectromechanical systems (MEMS/NEMS) to reduce stiction, friction, and improve their durability. Understanding the nanotribological performance and mechanisms of these films are quite important for efficient lubrication for MEMS/NEMS devices. These devices are used in various operating environments and their effect on friction, adhesion and durability needs to be clarified. For this purpose, mobile and chemically bonded PFPE films were deposited by dip coating technique. The friction and adhesion properties of these films were characterized by atomic force microscopy (AFM). The effect of rest time, velocity, relative humidity, and temperature on nanotribological properties of these films was studied. Durability of these films was also measured by repeated cycling tests. The adhesion, friction mechanisms of PFPE at molecular scale, and the mechanisms of the effect of operating environment and durability are subject of this paper. This study found that adsorption of water, formation of meniscus and its change during sliding, viscosity, and surface chemistry properties play a big role on the friction, adhesion, and durability of the lubricant films.

Journal Article↗
PubMed2000

Investigation of thermoelectric silicide thin films by means of analytical transmission electron microscopy

The microstructure of rhenium silicide thin films and its progress by annealing were investigated by means of analytical transmission electron microscopy. Sputtered amorphous films were characterised by analysis of the radial distribution function (RDF). The position of the first maximum of RDF represents the most probable distance between neighbouring atoms and decreases from 2.75 to 2.62 A in films with an increasing Si-content from 60 to 75 at%. This decrease correlates with the change of the temperature coefficient (TC) of the electrical resistivity. During in situ annealing, the formation of nanocrystals in films with different Si-contents was observed. In thin films with 64 at% the quantity of nanocrystals increases after 1 h at 900 K whereas their sizes remain unchanged. The crystallisation in Re-rich thin films proceeds lower and produces larger crystals than in films near to the ReSi1.75 stoichiometry. Sputtered epitaxial ReSi1.75 films on Si (1 0 0) consist of crystals with nanometer size and an azimuthal torsion of 45 degrees.

Journal Article↗
PubMed1999

Non-traditional plasticization of polymeric films.

The objective of this study was to investigate the influence of methylparaben, ibuprofen, chlorpheniramine maleate and theophylline on the thermal and mechanical properties of polymeric films of Eudragit RS 30 D. The effects of methylparaben and ibuprofen in the film coating on the rate of drug release from Eudragit RS 30 D coated beads were also studied. The physical and mechanical properties of the cast films and coated beads were investigated using thermal analysis, tensile testing, X-ray diffraction analysis and dissolution testing. The results demonstrated that the glass transition temperature of the Eudragit RS 30 D decreased with increasing levels of methylparaben, ibuprofen and chlorpheniramine maleate in the film. Theophylline exerted no influence on the thermal properties of the polymer. The higher levels of the ibuprofen and methylparaben incorporated into the film resulted in a decrease in the tensile strength of the film. The decrease in Young's modulus of Eudragit RS 30 D coated beads was attributed to an increase in the flexibility of the polymeric films when the level of methylparaben or ibuprofen in the polymeric dispersion was increased. The dissolution data demonstrated that the rate of release of the ibuprofen from coated beads was decreased by increasing the amount of ibuprofen and methylparaben in the polymeric film coating.

Chlorpheniramine↗
PubMed1999

Surface free energy of ethylcellulose films and the influence of plasticizers.

The surface free energy parameters of ethylcellulose (EC) films were determined using the Lifshitz-van der Waals/acid-base approach and the influence of plasticizers on their surface energetics was assessed. Films were prepared by dip-coating glass slides in organic solvents containing EC and the advancing angles of drops of pure liquids on the EC films were measured with a contact angle goniometer using the captive drop technique. EC has lower surface free energy than cellulose. The acid-base (AB) term made only a slight contribution to the total surface free energy and the surfaces exhibited predominantly monopolar electron-donicity. The addition of plasticizer (dibutyl sebacate or dibutyl phthalate) resulted in a small decrease in the total surface free energy. The effects of film forming variables, including solvent system, concentration and post-formation treatment (annealing), on the surface free energy parameters of EC films were also investigated. These data were then used to analyze how the surface energetics affect the interaction of the EC films with other surfaces based on interfacial tension, work of adhesion and spreading coefficient calculations. Lifshitz-van der Waals (LW) interactions provided the major contribution to the work of adhesion for EC with all of the solid substrates analyzed. However, the AB interactions contributed significantly to the work of adhesion for EC with 'bipolar' substrates and to the spreading coefficients of EC over substrates. The consideration of work of adhesion and spreading coefficient based on surface free energy parameters may have potential use in evaluating factors affecting film adhesion and, furthermore, in optimizing pharmaceutical film coating processes.

Cellulose↗
PubMed2001

Investigation of thin films formed from liposome suspensions on quartz substrate.

The stability of thin wetting films formed from 0.15 M NaCl solutions containing small unilamellar dimyristoylphosphatidylcholine (DMPC) vesicles of different concentrations on quartz surface has been investigated by the microinterferometric method. The intensity of monochromatic light reflected from both film surfaces has been recorded as a function of the time of film thinning. Two temperatures were used in the experiments (20 and 35 degrees C). Films containing 10(-3), 5x10(-3) and 10(-2) mg/ml DMPC were unstable and ruptured, while films with 10(-1) and 1 mg/ml DMPC were stable. Film stability was explained on the basis of hydrophobic interactions. Film thickness dependence on time was calculated. The kinetics of film thinning did not obey Reynolds equation and a linearization was observed in co-ordinates ln(h) as a function of time. This phenomenon was explained by a non-homogeneous thinning process, which might be due to the existence of some areas of different structure of the DMPC adsorption layers.

Journal Article↗
PubMed2002

Self-adhesive thin films for topical delivery of 5-aminolevulinic acid.

Self-adhesive thin-films have been developed as a topical delivery system for 5-aminolevulinic acid (ALA). The thin films are suitable for use during the photodynamic therapy of epithelial skin tumors. They are composed of a combination of the lipophilic polymer Eudragit NE and the lipophilic plasticiser acetyl tributyl citrate (ATBC). Because of its hydrophilicity, ALA forms suspension systems within these thin films, as evidenced by light microscopy. ALA release measured using Franz cells is very rapid from a Eudragit NE thin film loaded with 10% w/w ALA (200 microg ALA after 2.5 h), and even higher when ATBC is included. A Eudragit NE/ATBC (1: 2) thin film loaded with 20% w/w ALA releases 2000 microg ALA after 3.5 h. Combined release/permeation of ALA through excised membranes of human stratum corneum plus epidermis yielded fluxes of 50-100 microg ALA within 5 h for the Eudragit NE/ATBC (1: 2) thin film. The ATBC acts as a permeation enhancer for ALA. Scanning electron microscopy of the thin film surface shows protruding ALA particles which rapidly dissolve on contact with an aqueous medium. This surface dissolution mechanism is the cause of the rapid ALA release and hence also the high skin permeation in vitro. The mechanical properties of the thin films were also briefly examined. Adhesive strength increases with higher ATBC loading and decreases with higher ALA loading. Internal cohesion decreases with greater ATBC loading and increases with higher ALA loading. As part of this project, an improved derivatisation assay for gradient HPLC of ALA with 9Fluorenylmethyloxycarbonylchloride is also presented.

Adhesives↗
PubMed2003

Use of xylan, an agricultural by-product, in wheat gluten based biodegradable films: mechanical, solubility and water vapor transfer rate properties.

The possibility of using xylan, as an agricultural by-product, for production of composite films in combinations with wheat gluten was investigated. Different levels of xylan (0-40% w/w) were incorporated into wheat gluten to form biodegradable composite films. Films were prepared at pH 4 and 11, and dried at either uncontrolled or controlled conditions. The mechanical properties, solubilities and water vapour transfer rate (WVTR) of the composite films were studied. Films were obtained with added xylan without decreasing film-forming quality. Xylan can be used as an additive, as much as 40% (w/w), in wheat gluten films. Changing pH, wheat gluten/xylan ratio, xylan type and drying conditions affected mechanical and solubility properties, however, WVTR was not affected by xylan additions. Wheat gluten/xylan composite films having different characteristics can be produced depending on xylan type, composition and process conditions.

Agriculture↗
PubMed2003

Raman spectroscopic investigation of the single-monolayer Langmuir-Blodgett film of C16NaphOH and C10AzoNaphC4N-SDS.

Raman spectra were measured for Langmuir-Blodgett (LB) films of C(16)NaphOH and C(10)AzoNaphC(4)N-SDS on Calcium Fluorite substrate for the first time. In order to find out favorable excitation condition, Raman spectra of the single and multi-monolayer LB films excited at different lines at 244, 514, 633 and 778 nm are recorded and compared in the present study. Raman spectrum of the monolayer LB film of C(16)NaphOH excited by 244 nm demonstrate that excellent signal to noise is achieved even for one monolayer LB film with an extremely short integrating time as 60 s because of being resonantly enhanced, while no meaningful spectra were recorded under the same condition for the monolayer LB film of C(10)AzoNaphC(4)N-SDS because of burning. Using a HeNe 633 nm excitation the problem with strong substrate fluorescence was partially solved, since under these conditions this fluorescence is mainly outside the fingerprint region of the LB film molecules (1000-2000 cm(-1)). Therefore by using the HeNe laser excitation, Raman spectra with high signal to noise ratio of LB films of C(16)NaphOH were collected and shown in this paper. These findings stress again the necessity to define an appropriate Raman system for this special application of LB film diagnosis.

Alkanes↗
PubMed2003

Electrochemical and electrocatalytic properties of myoglobin and hemoglobin incorporated in carboxymethyl cellulose films.

Protein-CMC films were made by casting a solution of myoglobin (Mb) or hemoglobin (Hb) and carboxymethyl cellulose (CMC) on pyrolytic graphite electrodes. In pH 7.0 buffers, Mb and Hb incorporated in CMC films gave a pair of well-defined and quasi-reversible cyclic voltammetric peaks at about -0.34 V vs. SCE, respectively, characteristic of heme Fe(III)/Fe(II) redox couples of the proteins. The electrochemical parameters such as apparent standard heterogeneous electron transfer rate constants (k(s)) and formal potentials (E degrees ') were estimated by square wave voltammetry with nonlinear regression analysis. In aqueous solution, stable CMC films absorbed large amounts of water and formed hydrogel. Scanning electron microscopy of the films showed that interaction between Mb or Hb and CMC would make the morphology of dry protein-CMC films different from the CMC films alone. Positions of Soret absorbance band suggest that Mb and Hb in CMC films retain their secondary structure similar to the native states in the medium pH range. Trichloroacetic acid, nitrite, oxygen, and hydrogen peroxide were catalytically reduced at protein-CMC film electrodes.

Carboxymethylcellulose Sodium↗
PubMed2000

Standard electrochemical behavior of high-quality, boron-doped polycrystalline diamond thin-film electrodes

Standard electrochemical data for high-quality, boron-doped diamond thin-film electrodes are presented. Films from two different sources were compared (NRL and USU) and both were highly conductive, hydrogen-terminated, and polycrystalline. The films are acid washed and hydrogen plasma treated prior to use to remove nondiamond carbon impurity phases and to hydrogen terminate the surface. The boron-doping level of the NRL film was estimated to be in the mid 1019 B/cm3 range, and the boron-doping level of the USU films was approximately 5 x 10(20) B/cm(-3) based on boron nuclear reaction analysis. The electrochemical response was evaluated using Fe-(CN)6(3-/4-), Ru(NH3)6(3+/2+), IrCl6(2-/3-), methyl viologen, dopamine, ascorbic acid, Fe(3+/2+), and chlorpromazine. Comparisons are made between the apparent heterogeneous electron-transfer rate constants, k0(app), observed at these high-quality diamond films and the rate constants reported in the literature for freshly activated glassy carbon. Ru(NH3)6(3+/2+), IrCl6(2-/3-), methyl viologen, and chlorpromazine all involve electron transfer that is insensitive to the diamond surface microstructure and chemistry with k0(app) in the 10(-2)-10(-1) cm/s range. The rate constants are mainly influenced by the electronic properites of the films. Fe(CN)6(3-/4-) undergoes electron transfer that is extremely sensitive to the surface chemistry with k0(app) in the range of 10(-2)-10(-1) cm/s at the hydrogen-terminated surface. An oxygen surface termination severely inhibits the rate of electron transfer. Fe(3+/2+) undergoes slow electron transfer at the hydrogen-terminated surface with k0(app) near 10(-5) cm/s. The rate of electron transfer at sp2 carbon electrodes is known to be mediated by surface carbonyl functionalities; however, this inner-sphere, catalytic pathway is absent on diamond due to the hydrogen termination. Dopamine, like other catechol and catecholamines, undergoes sluggish electron transfer with k0(app) between 10(-4) and 10(-5) cm/s. Converting the surface to an oxygen termination has little effect on k0(app). The slow kinetics may be related to weak adsorption of these analytes on the diamond surface. Ascorbic acid oxidation is very sensitive to the surface termination with the most negative Ep(ox) observed at the hydrogen-terminated surface. An oxygen surface termination shifts Ep(ox) positive by some 250 mV or more. An interfacial energy diagram is proposed to explain the electron transfer whereby the midgap density of states results primarily from the boron doping level and the lattice hydrogen. The films were additionally characterized by scanning electron microscopy and micro-Raman imaging spectroscopy. The cyclic voltammetric and kinetic data presented can serve as a benchmark for research groups evaluating the electrochemical properties of semimetallic (i.e., conductive), hydrogen-terminated, polycrystalline diamond.

Journal Article↗
PubMed2000

Orientations of liquid crystals on mechanically rubbed films of bovine serum albumin: a possible substrate for biomolecular assays based on liquid crystals.

We report the uniform planar anchoring of thermotropic liquid crystals on films of bovine serum albumin (BSA) covalently immobilized on the surface of glass microscope slides and mechanically rubbed using a cloth. The azimuthal orientations of the liquid crystals were measured to be parallel to the direction of rubbing. Following immersion and removal of these rubbed films of BSA from aqueous solutions containing either BSA, fibrinogen, lysozyme, anti-FITC immunoglobulin G (IgG), or antistreptavidin IgG, we measured liquid crystals placed onto these surfaces to largely retain their uniform alignment. In contrast, following immersion of a rubbed film of BSA into an aqueous solution of anti-BSA IgG, we observed liquid crystals on these surfaces to assume nonuniform orientations. We conclude that specific binding of anti-BSA IgG to the film of rubbed BSA erased anisotropy induced within the film of BSA by rubbing. This result suggests that the spatial scale of anisotropy within the rubbed film of BSA is comparable to or smaller than the size of the IgG molecule. Because the anisotropy within a rubbed film of a protein can be erased by specific binding of a second protein, we believe these types of substrates (rubbed films of proteins) have the potential to be useful in a variety of label-free biomolecular assays where specific binding of a target species to its ligand can be imaged through observation of the optical appearance of liquid crystal placed onto the surface.

Adsorption↗
PubMed2003

Thin films of polyelectrolyte-encapsulated catalase microcrystals for biosensing.

Polyelectrolyte (PE)-encapsulated catalase microcrystals were assembled onto gold electrodes by their sequential deposition with oppositely charged PEs, utilizing electrostatic interactions to form enzyme thin films for biosensing. The PE coating around the microcrystals provided a regular surface charge, thus facilitating the stepwise film growth, and it effectively prevented catalase leakage from the assembled films. The encapsulated catalase was shown to retain both its biological and its electrochemical activity. Direct electron transfer between catalase molecules and the gold electrode was achieved without the aid of any electron mediator. In pH 5.0 phosphate buffer solution, the apparent formal potential (E(o)') of catalase was -0.131 V (vs Ag/AgCl). As a H2O2 biosensor, films consisting of one layer of the encapsulated catalase displayed considerably higher (approximately 5-fold) and more stable electrocatalytic responses to the reduction of H2O2 than did corresponding films made of one layer of nonencapsulated catalase or solubilized catalase. An increase in either the number of "precursor" PE layers between the gold electrodes and the catalase microcrystal layers in the film or the number of PE layers encapsulating the catalase microcrystals was found to decrease the electrocatalytic activity of the electrode. At low precursor PE layer numbers (approximately 2) and PE encapsulating layers (approximately 4), the current response was proportional to the H2O2 concentration in the range 3.0 x 10(-6) to 1.0 x 10(-2) M. The overall electroactivity of the multilayer film increased for the first two layers of encapsulated catalase, after which a plateau was observed. This was attributed to the increasing difficulty of electron transfer and substrate diffusion limitations. The current approach of using immobilized PE-encapsulated enzyme microcrystals for biosensing provides a versatile method to prepare high enzyme content films with high and tailored enzyme activities.

Biosensing Techniques↗
PubMed2003

An amperometric detector formed of highly dispersed Ni nanoparticles embedded in a graphite-like carbon film electrode for sugar determination.

We achieved improved detection limits for sugars by developing a novel thin film containing 0.8% highly dispersed Ni nanoparticles in disordered graphite-like carbon (Ni-NDC) as a detection electrode for high-performance liquid chromatography. The Ni-NDC film was prepared in one step by a simple radio frequency (rf) sputtering method at a temperature below 200 degrees C. We characterized the film by XPS, TEM, and AFM analysis and found that the average Ni nanoparticle size was 3 nm and that the film consisted of a mixture of Ni, NiO, Ni2O3, and Ni(OH)2. We studied the electrochemical detection of sugars using the 0.8% Ni-NDC film electrode. The film electrode had excellent electrocatalytic ability and good stability compared with a Ni-bulk electrode with regard to the electrooxidation of sugars. We employed the Ni-NDC film as an HPLC detection electrode. We achieved a good separation of four sugars (glucose, fructose, sucrose, lactose) at a relatively low constant detection potential (0.40 V vs Ag/AgCl) and a linearity of over 3 orders of magnitude. We obtained improved detection limits for the investigated sugars, namely, 20, 25, 50, and 37 nM for glucose, fructose, sucrose, and lactose, respectively. This is at least 1 order of magnitude lower than the detection limits obtained with a Ni-bulk electrode with the same measurement condition. The Ni-NDC film electrode also showed good reproducibility with a relative standard deviation of 1.75% for 40 consecutive injections of glucose in a flow system.

Carbon↗