Science.gov

Sample records for implanted glassy carbon

  1. Diamond film growth on Ti-implanted glassy carbon

    NASA Astrophysics Data System (ADS)

    Brewer, M. A.; Brown, I. G.; Evans, P. J.; Hoffman, A.

    1993-09-01

    The growth of diamond thin films on glassy carbon substrates has been investigated as a function of deposition time for different surface treatments. Implantation of Ti to a dose of 1.7 x 10 exp 17/sq cm and abrasion with diamond powder have both been examined to determine their effect on film nucleation and growth. At the shorter deposition times studied, diamond nucleation was observed on all test samples with those subjected to the abrasive pretreatment exhibiting the higher growth rates. However, the adhesion and uniformity of films on unimplanted glassy carbon were found to deteriorate significantly following deposition runs of 14 and 21 h duration. This was attributed to a destabilization of the underlying surface caused by plasma erosion.

  2. Annealing effects on the migration of ion-implanted cadmium in glassy carbon

    NASA Astrophysics Data System (ADS)

    Hlatshwayo, T. T.; Sebitla, L. D.; Njoroge, E. G.; Mlambo, M.; Malherbe, J. B.

    2017-03-01

    The migration behaviour of cadmium (Cd) implanted into glassy carbon and the effects of annealing on radiation damage introduced by ion implantation were investigated. The glassy carbon substrates were implanted with Cd at a dose of 2 × 1016 ions/cm2 and energy of 360 keV. The implantation was performed at room temperature (RT), 430 °C and 600 °C. The RT implanted samples were isochronally annealed in vacuum at 350, 500 and 600 °C for 1 h and isothermally annealed at 350 °C up to 4 h. The as-implanted and annealed samples were characterized by Raman spectroscopy and Rutherford backscattering spectrometry (RBS). Raman results revealed that implantation at room temperature amorphized the glassy carbon structure while high temperature implantations resulted in slightly less radiation damage. Isochronal annealing of the RT implanted samples resulted in some recrystallization as a function of increasing temperature. The original glassy carbon structure was not achieved at the highest annealing temperature of 600 °C. Diffusion of Cd in glassy carbon was already taking place during implantation at 430 °C. This diffusion of Cd was accompanied by significant loss from the surface during implantation at 600 °C. Isochronal annealing of the room temperature implanted samples at 350 °C for 1 h caused Cd to diffuse towards the bulk while isothermal annealing at 500 and 600 °C resulted in the migration of implanted Cd toward the surface accompanied by a loss of Cd from the surface. Isothermal annealing at 350 °C for 1 h caused Cd to diffuse towards the bulk while for annealing time >1 h Cd diffused towards the surface. These results were interpreted in terms of trapping and de-trapping of implanted Cd by radiation damage.

  3. Equation of state of heated glassy carbon

    NASA Technical Reports Server (NTRS)

    Sekine, Toshimori; Ahrens, Thomas J.

    1991-01-01

    New Hugoniot data are presented for glassy carbon preheated to 1550 K and shocked to 20 GPa. The high-temperature Hugoniot is very similar to the principal Hugoniot. This results argues against the diffusional mechanism for the shock-induced transformaton of amorphous carbon to diamond, although the present results are obviously limited to below 20 GPa. This study provides the first Higoniot data for carbon preheated to significantly high temperatures.

  4. Wafer-level microstructuring of glassy carbon

    NASA Astrophysics Data System (ADS)

    Hans, Loïc. E.; Prater, Karin; Kilchoer, Cédric; Scharf, Toralf; Herzig, Hans Peter; Hermerschmidt, Andreas

    2014-03-01

    Glassy carbon is used nowadays for a variety of applications because of its mechanical strength, thermal stability and non-sticking adhesion properties. One application is glass molding that allows to realize high resolution diffractive optical elements on large areas and at affordable price appropriate for mass production. We study glassy carbon microstructuring for future precision compression molding of low and high glass-transition temperature. For applications in optics the uniformity, surface roughness, edge definition and lateral resolution are very important parameters for a stamp and the final product. We study different methods of microstructuring of glassy carbon by etching and milling. Reactive ion etching with different protection layers such as photoresists, aluminium and titanium hard masks have been performed and will be compare with Ion beam etching. We comment on the quality of the structure definition and give process details as well as drawbacks for the different methods. In our fabrications we were able to realize optically flat diffractive structures with slope angles of 80° at typical feature sizes of 5 micron and 700 nm depth qualified for high precision glass molding.

  5. The fabrication of artifacts out of glassy carbon and carbon-fiber-reinforced carbon for biomedical applications.

    PubMed

    Jenkins, G M; Grigson, C J

    1979-05-01

    Polymeric carbons are produced by the carbonization of a wide range of organic polymeric systems. We have concentrated on the fabrication of two types of polymeric carbons, glassy carbon and carbon-fiber-reinforced carbon (CFRC), both involving phenolic resin precursors. We describe herein the technology which enables us to make dental implants and heart valves out of glassy carbon. We also show how carbon-fiber-reinforced carbon can be made in the form of rods and plates for orthopedic use and molded before firing to produce complex, rigid, individually sculptured shapes suitable for maxillofacial bone replacement. The mechanical properties will be discussed in relation to the structure of these various forms of polymeric carbon. The main purpose of the work is to show that the technology of polymeric-carbon manufacture is essentially simple and the manufacturing process is readily carried out in laboratories which have already been equipped to fabricate standard dental prostheses.

  6. How Glassy States Affect Brown Carbon Production?

    NASA Astrophysics Data System (ADS)

    Liu, P.; Li, Y.; Wang, Y.; Bateman, A. P.; Zhang, Y.; Gong, Z.; Gilles, M. K.; Martin, S. T.

    2015-12-01

    Secondary organic material (SOM) can become light-absorbing (i.e. brown carbon) via multiphase reactions with nitrogen-containing species such as ammonia and amines. The physical states of SOM, however, potentially slow the diffusion of reactant molecules in organic matrix under conditions that semisolids or solids prevail, thus inhibiting the browning reaction pathways. In this study, the physical states and the in-particle diffusivity were investigated by measuring the evaporation kinetics of both water and organics from aromatic-derived SOMs using a quartz-crystal-microbalance (QCM). The results indicate that the SOMs derived from aromatic precursors toluene and m-xylene became solid (glassy) and the in particle diffusion was significantly impeded for sufficiently low relative humidity ( < 20% RH) at 293 K. Optical properties and the AMS spectra were measured for toluene-derived SOM after ammonia exposure at varied RHs. The results suggest that the production of light-absorbing nitrogen-containing compounds from multiphase reactions with ammonia was kinetically limited in the glassy organic matrix, which otherwise produce brown carbon. The results of this study have significant implications for production and optical properties of brown carbon in urban atmospheres that ultimately influence the climate and tropospheric photochemistry.

  7. Anodic electrosynthesis of some peroxy compounds on glassy carbon electrodes

    SciTech Connect

    Khomutov, N.E.; Zakhodyakina, N.A.; Svirida, L.V.; Nesvat, N.V.

    1987-11-10

    The authors present the results of a study of the anodic electrosynthesis of hydrogen peroxide and its derivatives on glassy carbon in solutions of sodium carbonate and sodium carbonate with sodium borate. We studied the kinetics of anodic processes on glassy carbon with the aid of polarization measurements and a method for determining the concentrations of active oxygen in the anolyte and the current efficiency. The current efficiencies with respect to active oxygen obtained on glassy carbon in the mixed solution of sodium borate and sodium carbonate are close to the current efficiencies which are observed on platinum anodes in the industrial electrosynthesis of perborates.

  8. Shock-wave studies of anomalous compressibility of glassy carbon

    SciTech Connect

    Molodets, A. M. Golyshev, A. A.; Savinykh, A. S.; Kim, V. V.

    2016-02-15

    The physico-mechanical properties of amorphous glassy carbon are investigated under shock compression up to 10 GPa. Experiments are carried out on the continuous recording of the mass velocity of compression pulses propagating in glassy carbon samples with initial densities of 1.502(5) g/cm{sup 3} and 1.55(2) g/cm{sup 3}. It is shown that, in both cases, a compression wave in glassy carbon contains a leading precursor with amplitude of 0.135(5) GPa. It is established that, in the range of pressures up to 2 GPa, a shock discontinuity in glassy carbon is transformed into a broadened compression wave, and shock waves are formed in the release wave, which generally means the anomalous compressibility of the material in both the compression and release waves. It is shown that, at pressure higher than 3 GPa, anomalous behavior turns into normal behavior, accompanied by the formation of a shock compression wave. In the investigated area of pressure, possible structural changes in glassy carbon under shock compression have a reversible character. A physico-mechanical model of glassy carbon is proposed that involves the equation of state and a constitutive relation for Poisson’s ratio and allows the numerical simulation of physico-mechanical and thermophysical properties of glassy carbon of different densities in the region of its anomalous compressibility.

  9. Transparent, superhard amorphous carbon phase from compressing glassy carbon

    NASA Astrophysics Data System (ADS)

    Yao, Mingguang; Xiao, Junping; Fan, Xianhong; Liu, Ran; Liu, Bingbing

    2014-01-01

    Raman spectroscopy has been used to study the transformations of glassy carbon (GC) under high pressure. A GC sphere has been observed to transform into a transparent carbon phase above 33 GPa. The transformation is associated with a change in bonding character of carbon from sp2 to sp3 hybridization and an increase in hardness. The yield strength of the GC sphere reaches a value of 120 GPa at a confining pressure of 62 GPa, which is comparable to that of diamond at ambient conditions. The stress induced by the pressure medium is important for the observed transformations of GC under pressure.

  10. Morphology and formation process of diamond from glassy carbon

    NASA Astrophysics Data System (ADS)

    Miyamoto, Manabu; Akaishi, Minoru; Ohsawa, Toshikazu; Yamaoka, Shinobu; Fukunaga, Osamu

    1989-10-01

    Under static high pressure conditions in the presence of a catalyst metal, a diamond formation process was studied using glassy carbon as a starting source, which was prepared by pyrolysis of furfuryl alcohol resin. Above 1200 °C of the pyrolysis temperature, diamond formation was clearly observed in Ni, Fe, Co and their alloy catalysts. The hydrogen content in the starting carbon has a drastic effect on the diamond formation. The maximum content of the hydrogen in the glassy carbon had to be between 1200 and 2200 ppm to see diamond formation. In the Fe-rich catalyst, a characteristic needle-like diamond was formed due to the texture of the carbon source and the nature of the catalyst.

  11. Ultrasonic treatment of glassy carbon for nanoparticle preparation.

    PubMed

    Levêque, Jean-Marc; Duclaux, Laurent; Rouzaud, Jean-Noël; Reinert, Laurence; Komatsu, Naoki; Desforges, Alexandre; Afreen, Sadia; Sivakumar, Manickam; Kimura, Takahide

    2017-03-01

    Glassy carbon particles (millimetric or micrometric sizes) dispersions in water were treated by ultrasound at 20kHz, either in a cylindrical reactor, or in a "Rosette" type reactor, for various time lengths ranging from 3h to 10h. Further separations sedimentation allowed obtaining few nanoparticles of glassy carbon in the supernatant (diameter <200nm). Thought the yield of nanoparticle increased together with the sonication time at high power, it tended to be nil after sonication in the cylindrical reactor. The sonication of glassy carbon micrometric particles in water using "Rosette" instead of cylindrical reactor, allowed preparing at highest yield (1-2wt%), stable suspensions of carbon nanoparticles, easily separated from the sedimented particles. Both sediment and supernatant separated by decantation of the sonicated dispersions were characterized by laser granulometry, scanning electron microscopy, X-ray microanalysis, and Raman and infrared spectroscopies. Their multiscale organization was investigated by transmission electron microscopy as a function of the sonication time. For sonication longer than 10h, these nanoparticles from supernatant (diameter <50nm) are aggregated. Their structures are more disordered than the sediment particles showing typical nanometer-sized aromatic layer arrangement of glassy carbon, with closed mesopores (diameter ∼3nm). Sonication time longer than 5h has induced not only a strong amorphization (subnanometric and disoriented aromatic layer) but also a loss of the mesoporous network nanostructure. These multi-scale organizational changes took place because of both cavitation and shocks between particles, mainly at the particle surface. The sonication in water has induced also chemical effects, leading to an increase in the oxygen content of the irradiated material together with the sonication time.

  12. Uniaxial-stress-driven transformation in cold compressed glassy carbon

    NASA Astrophysics Data System (ADS)

    Yao, Mingguang; Fan, Xianhong; Zhang, Weiwei; Bao, Yongjun; Liu, Ran; Sundqvist, Bertil; Liu, Bingbing

    2017-09-01

    We show that transformation of glassy carbon (GC) into a translucent superhard carbon phase by cold-compression is obtained in the presence of a uniaxial stress field. This transition accompanies with sp2 to sp3 bonding change in GC, and it is found that the uniaxial stress strongly favors this bonding transition. The transformation of GC causes photoluminescence and significantly increases light transmissivity. Upon decompression, the high pressure phase can be maintained under large uniaxial stress at a chamber pressure even down to ˜10 GPa. We discuss possible mechanisms of these transitions by a distinct bonding process that occurs in noncrystalline carbon.

  13. Magnetoresistance, electrical conductivity, and Hall effect of glassy carbon

    SciTech Connect

    Baker, D.F.

    1983-02-01

    These properties of glassy carbon heat treated for three hours between 1200 and 2700/sup 0/C were measured from 3 to 300/sup 0/K in magnetic fields up to 5 tesla. The magnetoresistance was generally negative and saturated with reciprocal temperature, but still increased as a function of magnetic field. The maximum negative magnetoresistance measured was 2.2% for 2700/sup 0/C material. Several models based on the negative magnetoresistance being proportional to the square of the magnetic moment were attempted; the best fit was obtained for the simplest model combining Curie and Pauli paramagnetism for heat treatments above 1600/sup 0/C. Positive magnetoresistance was found only in less than 1600/sup 0/C treated glassy carbon. The electrical conductivity, of the order of 200 (ohm-cm)/sup -1/ at room temperature, can be empirically written as sigma = A + Bexp(-CT/sup -1/4) - DT/sup -1/2. The Hall coefficient was independent of magnetic field, insensitive to temperature, but was a strong function of heat treatment temperature, crossing over from negative to positive at about 1700/sup 0/C and ranging from -0.048 to 0.126 cm/sup 3//coul. The idea of one-dimensional filaments in glassy carbon suggested by the electrical conductivity is compatible with the present consensus view of the microstructure.

  14. Nanocrystalline hexagonal diamond formed from glassy carbon

    NASA Astrophysics Data System (ADS)

    Shiell, Thomas. B.; McCulloch, Dougal G.; Bradby, Jodie E.; Haberl, Bianca; Boehler, Reinhard; McKenzie, David. R.

    2016-11-01

    Carbon exhibits a large number of allotropes and its phase behaviour is still subject to significant uncertainty and intensive research. The hexagonal form of diamond, also known as lonsdaleite, was discovered in the Canyon Diablo meteorite where its formation was attributed to the extreme conditions experienced during the impact. However, it has recently been claimed that lonsdaleite does not exist as a well-defined material but is instead defective cubic diamond formed under high pressure and high temperature conditions. Here we report the synthesis of almost pure lonsdaleite in a diamond anvil cell at 100 GPa and 400 °C. The nanocrystalline material was recovered at ambient and analysed using diffraction and high resolution electron microscopy. We propose that the transformation is the result of intense radial plastic flow under compression in the diamond anvil cell, which lowers the energy barrier by “locking in” favourable stackings of graphene sheets. This strain induced transformation of the graphitic planes of the precursor to hexagonal diamond is supported by first principles calculations of transformation pathways and explains why the new phase is found in an annular region. Our findings establish that high purity lonsdaleite is readily formed under strain and hence does not require meteoritic impacts.

  15. Nanocrystalline hexagonal diamond formed from glassy carbon.

    PubMed

    Shiell, Thomas B; McCulloch, Dougal G; Bradby, Jodie E; Haberl, Bianca; Boehler, Reinhard; McKenzie, David R

    2016-11-29

    Carbon exhibits a large number of allotropes and its phase behaviour is still subject to significant uncertainty and intensive research. The hexagonal form of diamond, also known as lonsdaleite, was discovered in the Canyon Diablo meteorite where its formation was attributed to the extreme conditions experienced during the impact. However, it has recently been claimed that lonsdaleite does not exist as a well-defined material but is instead defective cubic diamond formed under high pressure and high temperature conditions. Here we report the synthesis of almost pure lonsdaleite in a diamond anvil cell at 100 GPa and 400 °C. The nanocrystalline material was recovered at ambient and analysed using diffraction and high resolution electron microscopy. We propose that the transformation is the result of intense radial plastic flow under compression in the diamond anvil cell, which lowers the energy barrier by "locking in" favourable stackings of graphene sheets. This strain induced transformation of the graphitic planes of the precursor to hexagonal diamond is supported by first principles calculations of transformation pathways and explains why the new phase is found in an annular region. Our findings establish that high purity lonsdaleite is readily formed under strain and hence does not require meteoritic impacts.

  16. Nanocrystalline hexagonal diamond formed from glassy carbon

    SciTech Connect

    Shiell, Thomas. B.; McCulloch, Dougal G.; Bradby, Jodie E.; Haberl, Bianca; Boehler, Reinhard; McKenzie, David. R.

    2016-11-29

    Carbon exhibits a large number of allotropes and its phase behaviour is still subject to signifcant uncertainty and intensive research. The hexagonal form of diamond, also known as lonsdaleite, was discovered in the Canyon Diablo meteorite where its formation was attributed to the extreme conditions experienced during the impact. However, it has recently been claimed that lonsdaleite does not exist as a well-defned material but is instead defective cubic diamond formed under high pressure and high temperature conditions. Here we report the synthesis of almost pure lonsdaleite in a diamond anvil cell at 100GPa and 400 C. The nanocrystalline material was recovered at ambient and analysed using difraction and high resolution electron microscopy. We propose that the transformation is the result of intense radial plastic fow under compression in the diamond anvil cell, which lowers the energy barrier by locking in favourable stackings of graphene sheets. This strain induced transformation of the graphitic planes of the precursor to hexagonal diamond is supported by frst principles calculations of transformation pathways and explains why the new phase is found in an annular region. Furthermore, our findings establish that high purity lonsdaleite is readily formed under strain and hence does not require meteoritic impacts.

  17. Nanocrystalline hexagonal diamond formed from glassy carbon

    PubMed Central

    Shiell, Thomas. B.; McCulloch, Dougal G.; Bradby, Jodie E.; Haberl, Bianca; Boehler, Reinhard; McKenzie, David. R.

    2016-01-01

    Carbon exhibits a large number of allotropes and its phase behaviour is still subject to significant uncertainty and intensive research. The hexagonal form of diamond, also known as lonsdaleite, was discovered in the Canyon Diablo meteorite where its formation was attributed to the extreme conditions experienced during the impact. However, it has recently been claimed that lonsdaleite does not exist as a well-defined material but is instead defective cubic diamond formed under high pressure and high temperature conditions. Here we report the synthesis of almost pure lonsdaleite in a diamond anvil cell at 100 GPa and 400 °C. The nanocrystalline material was recovered at ambient and analysed using diffraction and high resolution electron microscopy. We propose that the transformation is the result of intense radial plastic flow under compression in the diamond anvil cell, which lowers the energy barrier by “locking in” favourable stackings of graphene sheets. This strain induced transformation of the graphitic planes of the precursor to hexagonal diamond is supported by first principles calculations of transformation pathways and explains why the new phase is found in an annular region. Our findings establish that high purity lonsdaleite is readily formed under strain and hence does not require meteoritic impacts. PMID:27897174

  18. Nanocrystalline hexagonal diamond formed from glassy carbon

    DOE PAGES

    Shiell, Thomas. B.; McCulloch, Dougal G.; Bradby, Jodie E.; ...

    2016-11-29

    Carbon exhibits a large number of allotropes and its phase behaviour is still subject to signifcant uncertainty and intensive research. The hexagonal form of diamond, also known as lonsdaleite, was discovered in the Canyon Diablo meteorite where its formation was attributed to the extreme conditions experienced during the impact. However, it has recently been claimed that lonsdaleite does not exist as a well-defned material but is instead defective cubic diamond formed under high pressure and high temperature conditions. Here we report the synthesis of almost pure lonsdaleite in a diamond anvil cell at 100GPa and 400 C. The nanocrystalline materialmore » was recovered at ambient and analysed using difraction and high resolution electron microscopy. We propose that the transformation is the result of intense radial plastic fow under compression in the diamond anvil cell, which lowers the energy barrier by locking in favourable stackings of graphene sheets. This strain induced transformation of the graphitic planes of the precursor to hexagonal diamond is supported by frst principles calculations of transformation pathways and explains why the new phase is found in an annular region. Furthermore, our findings establish that high purity lonsdaleite is readily formed under strain and hence does not require meteoritic impacts.« less

  19. Evidence for a glassy state in strongly driven carbon

    NASA Astrophysics Data System (ADS)

    Brown, C. R. D.; Gericke, D. O.; Cammarata, M.; Cho, B. I.; Döppner, T.; Engelhorn, K.; Förster, E.; Fortmann, C.; Fritz, D.; Galtier, E.; Glenzer, S. H.; Harmand, M.; Heimann, P.; Kugland, N. L.; Lamb, D. Q.; Lee, H. J.; Lee, R. W.; Lemke, H.; Makita, M.; Moinard, A.; Murphy, C. D.; Nagler, B.; Neumayer, P.; Plagemann, K.-U.; Redmer, R.; Riley, D.; Rosmej, F. B.; Sperling, P.; Toleikis, S.; Vinko, S. M.; Vorberger, J.; White, S.; White, T. G.; Wünsch, K.; Zastrau, U.; Zhu, D.; Tschentscher, T.; Gregori, G.

    2014-06-01

    Here, we report results of an experiment creating a transient, highly correlated carbon state using a combination of optical and x-ray lasers. Scattered x-rays reveal a highly ordered state with an electrostatic energy significantly exceeding the thermal energy of the ions. Strong Coulomb forces are predicted to induce nucleation into a crystalline ion structure within a few picoseconds. However, we observe no evidence of such phase transition after several tens of picoseconds but strong indications for an over-correlated fluid state. The experiment suggests a much slower nucleation and points to an intermediate glassy state where the ions are frozen close to their original positions in the fluid.

  20. Evidence for a glassy state in strongly driven carbon.

    PubMed

    Brown, C R D; Gericke, D O; Cammarata, M; Cho, B I; Döppner, T; Engelhorn, K; Förster, E; Fortmann, C; Fritz, D; Galtier, E; Glenzer, S H; Harmand, M; Heimann, P; Kugland, N L; Lamb, D Q; Lee, H J; Lee, R W; Lemke, H; Makita, M; Moinard, A; Murphy, C D; Nagler, B; Neumayer, P; Plagemann, K-U; Redmer, R; Riley, D; Rosmej, F B; Sperling, P; Toleikis, S; Vinko, S M; Vorberger, J; White, S; White, T G; Wünsch, K; Zastrau, U; Zhu, D; Tschentscher, T; Gregori, G

    2014-06-09

    Here, we report results of an experiment creating a transient, highly correlated carbon state using a combination of optical and x-ray lasers. Scattered x-rays reveal a highly ordered state with an electrostatic energy significantly exceeding the thermal energy of the ions. Strong Coulomb forces are predicted to induce nucleation into a crystalline ion structure within a few picoseconds. However, we observe no evidence of such phase transition after several tens of picoseconds but strong indications for an over-correlated fluid state. The experiment suggests a much slower nucleation and points to an intermediate glassy state where the ions are frozen close to their original positions in the fluid.

  1. Evidence for a glassy state in strongly driven carbon

    SciTech Connect

    Brown, C. R. D.; Gericke, D. O.; Cammarata, M.; Cho, B. I.; Gwangju Inst. of Science and Technology, Gwangju; Inst. for Basic Science, Gwangju ; Döppner, T.; Engelhorn, K.; Förster, E.; Fortmann, C.; Fritz, D.; Galtier, E.; Glenzer, S. H.; Harmand, M.; Heimann, P.; Kugland, N. L.; Lamb, D. Q.; Lee, H. J.; Lee, R. W.; Lemke, H.; Makita, M.; Moinard, A.; Murphy, C. D.; Nagler, B.; Neumayer, P.; Plagemann, K. -U.; Redmer, R.; Riley, D.; Rosmej, F. B.; Sperling, P.; Toleikis, S.; Vinko, S. M.; Vorberger, J.; White, S.; White, T. G.; Wünsch, K.; Zastrau, U.; Zhu, D.; Tschentscher, T.; Gregori, G.

    2014-06-09

    Here, we report results of an experiment creating a transient, highly correlated carbon state using a combination of optical and x-ray lasers. Scattered x-rays reveal a highly ordered state with an electrostatic energy significantly exceeding the thermal energy of the ions. Strong Coulomb forces are predicted to induce nucleation into a crystalline ion structure within a few picoseconds. However, we observe no evidence of such phase transition after several tens of picoseconds but strong indications for an over-correlated fluid state. The experiment suggests a much slower nucleation and points to an intermediate glassy state where the ions are frozen close to their original positions in the fluid.

  2. Surface treatment of Glassy Polymeric Carbon artifacts for medical applications

    SciTech Connect

    Rodrigues, M. G.; Zimmerman, R. L.; Rezende, M. C.

    1999-06-10

    Glassy Polymeric Carbon (GPC) has been used for mechanical cardiac valves. GCP valves are chemically biocompatible and durable, but less thromboresistant than biological valves. Enhanced thromboresistance of mechanical cardiac components with porous surface has been demonstrated. The endothelialized tissue blood-contacting surface adheres to the porous prosthetic component and decreases the formation of thrombus. Our experience has shown that the porosity of GPC can be increased and controlled by MeV ion bombardment. We report here that the surface roughness of heat-treated GPC bombarded with C, O, Si and Au is also enhanced. The surface roughness of the ion-bombarded samples is on a smaller scale than those roughened by sand blasting (measurements made with Perthomete S and P). The roughness decreases slightly after heat treatment, in linear proportion to the shrinkage of the test piece. Possible beneficial effects of the imbedded ions on tissue adherence and thromboresistance must be determined by in vivo animal experiments.

  3. Evidence for a glassy state in strongly driven carbon

    PubMed Central

    Brown, C. R. D.; Gericke, D. O.; Cammarata, M.; Cho, B. I.; Döppner, T.; Engelhorn, K.; Förster, E.; Fortmann, C.; Fritz, D.; Galtier, E.; Glenzer, S. H.; Harmand, M.; Heimann, P.; Kugland, N. L.; Lamb, D. Q.; Lee, H. J.; Lee, R. W.; Lemke, H.; Makita, M.; Moinard, A.; Murphy, C. D.; Nagler, B.; Neumayer, P.; Plagemann, K.-U.; Redmer, R.; Riley, D.; Rosmej, F. B.; Sperling, P.; Toleikis, S.; Vinko, S. M.; Vorberger, J.; White, S.; White, T. G.; Wünsch, K.; Zastrau, U.; Zhu, D.; Tschentscher, T.; Gregori, G.

    2014-01-01

    Here, we report results of an experiment creating a transient, highly correlated carbon state using a combination of optical and x-ray lasers. Scattered x-rays reveal a highly ordered state with an electrostatic energy significantly exceeding the thermal energy of the ions. Strong Coulomb forces are predicted to induce nucleation into a crystalline ion structure within a few picoseconds. However, we observe no evidence of such phase transition after several tens of picoseconds but strong indications for an over-correlated fluid state. The experiment suggests a much slower nucleation and points to an intermediate glassy state where the ions are frozen close to their original positions in the fluid. PMID:24909903

  4. Evidence for a glassy state in strongly driven carbon

    DOE PAGES

    Brown, C. R. D.; Gericke, D. O.; Cammarata, M.; ...

    2014-06-09

    Here, we report results of an experiment creating a transient, highly correlated carbon state using a combination of optical and x-ray lasers. Scattered x-rays reveal a highly ordered state with an electrostatic energy significantly exceeding the thermal energy of the ions. Strong Coulomb forces are predicted to induce nucleation into a crystalline ion structure within a few picoseconds. However, we observe no evidence of such phase transition after several tens of picoseconds but strong indications for an over-correlated fluid state. The experiment suggests a much slower nucleation and points to an intermediate glassy state where the ions are frozen closemore » to their original positions in the fluid.« less

  5. Electrochemical Determination of Albendazole at Glassy Carbon Electrode.

    PubMed

    Gowda, Jayant I; Kantikar, Rahul B; Harakuni, Devaraddi G; Jadhav, Kirankumar Y; Chanagoudar, Vinay C; Nandibewoor, Sharanappa T

    2016-11-01

    In this article, the electrochemical behavior on a glassy carbon electrode (GCE) was investigated and the electrochemical parameters of albendazole (ALB) were calculated. ALB effectively accumulated on the GCE surface and caused a pair of redox peaks at around 1.095 V and 1.028 V and an oxidation peak at 0.844 V (versus saturated calomel electrode) in 0.2 M phosphate buffer solution (pH 3.0). Under optimized conditions, the anodic peak current was linear to the ALB concentration the range of 1.5 × 10(-7) M to 4.0 × 10(-5) M. The regression equation was: Ipa (10(-6) A) = 0.79 [ALB] (μM) + 0.84 (R2 = 0.982). The detection limit 6.08 × 10(-8) M was obtained. The proposed method was successfully used to determine ALB content in tablet samples, with satisfactory results.

  6. Surface treatment of Glassy Polymeric Carbon artifacts for medical applications

    NASA Astrophysics Data System (ADS)

    Rodrigues, M. G.; Ila, D.; Rezende, M. C.; Damiao, A.; Zimmerman, R. L.

    1999-06-01

    Glassy Polymeric Carbon (GPC) has been used for mechanical cardiac valves. GCP valves are chemically biocompatible and durable, but less thromboresistant than biological valves. Enhanced thromboresistance of mechanical cardiac components with porous surface has been demonstrated. The endothelialized tissue blood-contacting surface adheres to the porous prosthetic component and decreases the formation of thrombus. Our experience has shown that the porosity of GPC can be increased and controlled by MeV ion bombardment. We report here that the surface roughness of heat-treated GPC bombarded with C, O, Si and Au is also enhanced. The surface roughness of the ion-bombarded samples is on a smaller scale than those roughened by sand blasting (measurements made with Perthomete S&P). The roughness decreases slightly after heat treatment, in linear proportion to the shrinkage of the test piece. Possible beneficial effects of the imbedded ions on tissue adherence and thromboresistance must be determined by in vivo animal experiments.

  7. Poly(4-vinylpyridine)-coated glassy carbon flow detectors

    SciTech Connect

    Wang, J.; Golden, T.; Tuzhi, P.

    1987-03-01

    The performance of a thin-layer flow detector with a glassy carbon electrode coated with a film of protonated poly(4-vinylpyridine) is described. Substantial improvement in the selectivity of amperometric detection for liquid chromatography and flow injection systems is observed as a result of excluding cationic species from the surface. The detector response was evaluated with respect to flow rate, solute concentration, coating scheme, film-to-film reproducibility, and other variables. Despite the increase in diffusional resistance, low detection limits of ca. 0.04 and 0.10 ng of ascorbic acid and uric acid, respectively, are maintained. Protection from organic surfactants can be coupled to the charge exclusion effect by using a bilayer coating, with a cellulose acetate film atop the poly(4-vinylpyridine) layer. Applicability to urine sample is demonstrated.

  8. Au nanoparticles and graphene quantum dots co-modified glassy carbon electrode for catechol sensing

    NASA Astrophysics Data System (ADS)

    Zhao, Xuan; He, Dawei; Wang, Yongsheng; Hu, Yin; Fu, Chen

    2016-03-01

    In this letter, the gold nanoparticles and graphene quantum dots were applied to the modification of glassy carbon electrode for the detection of catechol. The synergist cooperation between gold nanoparticles and graphene quantum dots can increase specific surface area and enhance electronic and catalytic properties of glassy carbon electrode. The detection limit of catechol is 0.869 μmol/L, demonstrating the superior detection efficiency of the gold nanoparticles and graphene quantum dots co-modified glassy carbon electrode as a new sensing platform.

  9. Carbonization Studies of Glassy Carbon Derived from Bis-Ortho-Diynylarenes (BODA) (Postprint)

    DTIC Science & Technology

    2007-02-26

    Derived from Bis-Ortho-Diynylarenes ( BODA ) (Postprint) 5b. GRANT NUMBER 5c. PROGRAM ELEMENT NUMBER 6. AUTHOR(S) Scott T. Iacono, Mark W. Perpall...have demonstrated bis-ortho-diynylarene ( BODA ) monomers undergo Bergman cyclopolymerizations to form hyper-branched, rigid naphthalene networks that...Std. 239.18 CARBONIZATION STUDIES OF GLASSY CARBON DERIVED FROM BIS-ORTHO-DIYNYLARENES ( BODA ) Scott T. Iacono1, Mark W. Perpall1, Wesley P

  10. Redox behavior of biofilm on glassy carbon electrode.

    PubMed

    Sridharan, D; Manoharan, S P; Palaniswamy, N

    2011-10-01

    Marine and freshwater biofilm usually shift the open circuit potential (OCP) of stainless steel towards the electropositive direction by +450 mV vs SCE. The nature of oxide film and bacterial metabolism were also correlated with ennoblement process by various investigators. Glassy carbon electrode (GCE) was used in the present study and a shifting of potential in the positive side (+450 mV) was noticed. It indicates that biofilm contributes to the ennoblement process without any n/p-type semiconducting oxide film. The nature of the cathodic curve for the biofilm covered GCE is compared with the previous literature on the electrochemical behavior of stainless steel. The present study explains the oxidation and reduction peaks of biofilm covered GCE by cyclic voltammetry. Electrochemical impedance result reveals the diffusion process within the manganese biofilm. The present study confirms the previous investigations that the manganese biofilm rules the electrochemical behavior of materials and suggests that oxide film is not necessary to assist the ennoblement process.

  11. Surface micro-structuring of glassy carbon for precision glass molding of diffractive optical elements

    NASA Astrophysics Data System (ADS)

    Prater, Karin; Dukwen, Julia; Scharf, Toralf; Herzig, Hans Peter; Hermerschmidt, Andreas

    2014-09-01

    Glassy carbon is used nowadays for a variety of applications because of its mechanical strength, thermal stability and non-sticking adhesion properties. This makes it also a suitable candidate as mold material for precision compression molding of low and high glass-transition temperature materials. To fabricate molds for diffractive optics a highresolution structuring technique is needed. We introduce a process that allows the micro-structuring of glassy carbon by reactive ion etching. Key parameters such as uniformity, surface roughness, edge definition and lateral resolution are discussed. They are the most relevant parameters for a stamp in optical applications. The use of titanium as a hard mask makes it possible to achieve a reasonable selectivity of 4:1, which has so far been one of the main problems in microstructuring of glassy carbon. We investigate the titanium surface structure with its 5-10 nm thick layer of TiO2 grains and its influence on the shape of the hard mask. In our fabrication procedure we were able to realize optically flat diffractive structures with slope angles of more than 80° at typical feature sizes of 5 μm and at 700 nm depth. The fabricated glassy carbon molds were applied to thermal imprinting onto different glasses. Glassy carbon molds with 1 mm thickness were tested with binary optical structures. Our experiments show the suitability of glassy carbon as molds for cost efficient mass production with a high quality.

  12. Ion Beam Optimized Mechanical Characteristics of Glassy Polymeric Carbon for Medical Applications

    SciTech Connect

    Rodrigues, M.G.; Cruz, N.C. da; Rangel, E.C.; Zimmerman, R.L.; Ila, D.; Poker, D.B.; Hensley, D.K.

    2003-08-26

    Glassy Polymeric Carbon (GPC) has medical applications owing to its inertness and biocompatible characteristics. Commercial GPC prosthetics include mitral, aortic and hydrocephalic valves. Surface treatment of GPC increases the adhesion of endothelic tissue on GPC and avoids the occurrence of thrombus in cardiac implant. In this work, ion beam was used to improve the mechanical characteristics of GPC surface. Hardness was measured as a function of depth in precursor and GPC samples heat treated from 300 to 2500 deg. C before and after bombardment with energetic ions of silicon, carbon, oxygen and gold at energies of 5, 6, 8 and 10 MeV and fluences between 1.0x1013 and 1.0x1016 ions/cm2. Comparison shows that hardness increases of the bombarded samples depend on heat treatment temperature. We verify that ion bombardment promotes carbonization due to an increased linkage between the chains of the polymeric material in lateral groups that are more numerous for samples heat treated to 700 deg. C.

  13. Nanoindentation mechanical properties characterization of glassy polymeric carbon treated with ion beam

    NASA Astrophysics Data System (ADS)

    Rodrigues, M. G.; da Cruz, N. C.; Rangel, E. C.; Zimmerman, R. L.; Ila, D.; Poker, D. B.; Hensley, D. K.

    2002-05-01

    Phenolic resins when heat treated in inert atmosphere up to 1000 °C become glassy polymeric carbon (GPC), a chemically inert and biocompatible material useful for medical applications, such as in the manufacture of heart valves and prosthetic devices. In earlier work we have shown that ion bombardment can modify the surface of GPC, increasing its roughness. The enhanced roughness, which depends on the species, energy and fluence of the ion beam, can improve the biocompatibility of GPC prosthetic artifacts. In this work, ion bombardment was used to make a layer of implanted ions under the surface to avoid the propagation of microcracks in regions where cardiac valves should have pins for fixation of the leaflets. GPC samples prepared at 700 and 1500 °C were bombarded with ions of silicon, carbon, oxygen and gold at energies of 5, 6, 8 and 10 MeV, respectively, and fluences between 1.0×10 13 and 1.0×10 16 ions/cm 2. Nanoindentation hardness characterization was used to compare bombarded with non-bombarded samples prepared at temperatures up to 2500 °C. The results with samples not bombarded showed that the hardness of GPC increases strongly with the heat treatment temperature. Comparison with ion bombarded samples shows that the hardness changes according to the ion used, the energy and fluence.

  14. Sensitive Electrochemical Detection of Enzymatically-generated Thiocholine at Carbon Nanotube Modified Glassy Carbon Electrode

    SciTech Connect

    Liu, Guodong; Riechers, Shawn L.; Mellen, Maria C.; Lin, Yuehe

    2005-11-01

    A carbon nanotube modified glassy-carbon (CNT/GC) electrode was used for enhancing the sensitivity of electrochemical measurements of enzymatically-generated thiocholine. Cyclic voltammetric and amperometric characteristics of thiocholine at CNT/GC, glassy carbon, carbon paste, and gold electrodes were compared. The CNT layer leads to a greatly improved anodic detection of enzymatically generated thiocholine product including lower oxidation overpotential (0.15 V) and higher sensitivity because of its electrocatalytic activity, fast electron transfer and large surface area. The sensor performance was optimized with respect to the operating conditions. Under the optimal batch conditions, a detection limit of 5 ?10 -6 mol/L was obtained with good precision (RSD = 5.2%, n=10). Furthermore, the attractive response of thiocholine on a CNT/GC electrode has allowed it to be used for constant-potential flow injection analysis. The detection limit was greatly improved to 0.3 ?10-6 mol/L. The high sensitivity electrochemical detection of enzymatically generated thiocholine with a CNT sensing platform holds great promise to prepare an acetylcholinesterase biosensor for monitoring organophosphate pesticides and nerve agents.

  15. Direct proteins electrochemistry based on ionic liquid mediated carbon nanotube modified glassy carbon electrode.

    PubMed

    Zhao, Qiang; Zhan, Dongping; Ma, Hongyang; Zhang, Meiqin; Zhao, Yifang; Jing, Ping; Zhu, Zhiwei; Wan, Xinhua; Shao, Yuanhua; Zhuang, Qiankun

    2005-01-01

    A novel glassy carbon electrode modified by a gel containing multi-walled carbon nanotubes (MWNTs) and ionic liquid of 1-butyl-3-methylimidazolium hexafluorophosphate (BMIPF6) is reported. The gel is formed by grinding of MWNTs and BMIPF6. Such gel is then coated on the surface of a glassy carbon electrode. We have employed scanning electron microscopy, Fourier transform infrared spectrometry (FTIR) and cyclic voltammetry to characterize the modified electrode. The direct electron transfers of hemoglobin and catalase on the modified electrode have been observed and studied in detail electrochemically. Hemoglobin is verified to be adsorbed on the modified electrode with the retention of conformation, which has been proved by microscopic FTIR. The electrochemical response of the adsorbed hemoglobin on the modified electrode is very stable, and shows repeated changes in the different pH solutions. It also has shown electrocatalysis to the reduction of oxygen and trichloroacetic acid. Catalase adsorbed on the gel modified electrode still keep activity to hydrogen peroxide. This work provides a simple and easy approach to construct biosensors based on the carbon nanotubes and ionic liquids.

  16. Carbon Fiber Biocompatibility for Implants

    PubMed Central

    Petersen, Richard

    2016-01-01

    Carbon fibers have multiple potential advantages in developing high-strength biomaterials with a density close to bone for better stress transfer and electrical properties that enhance tissue formation. As a breakthrough example in biomaterials, a 1.5 mm diameter bisphenol-epoxy/carbon-fiber-reinforced composite rod was compared for two weeks in a rat tibia model with a similar 1.5 mm diameter titanium-6-4 alloy screw manufactured to retain bone implants. Results showed that carbon-fiber-reinforced composite stimulated osseointegration inside the tibia bone marrow measured as percent bone area (PBA) to a great extent when compared to the titanium-6-4 alloy at statistically significant levels. PBA increased significantly with the carbon-fiber composite over the titanium-6-4 alloy for distances from the implant surfaces of 0.1 mm at 77.7% vs. 19.3% (p < 10−8) and 0.8 mm at 41.6% vs. 19.5% (p < 10−4), respectively. The review focuses on carbon fiber properties that increased PBA for enhanced implant osseointegration. Carbon fibers acting as polymer coated electrically conducting micro-biocircuits appear to provide a biocompatible semi-antioxidant property to remove damaging electron free radicals from the surrounding implant surface. Further, carbon fibers by removing excess electrons produced from the cellular mitochondrial electron transport chain during periods of hypoxia perhaps stimulate bone cell recruitment by free-radical chemotactic influences. In addition, well-studied bioorganic cell actin carbon fiber growth would appear to interface in close contact with the carbon-fiber-reinforced composite implant. Resulting subsequent actin carbon fiber/implant carbon fiber contacts then could help in discharging the electron biological overloads through electrochemical gradients to lower negative charges and lower concentration. PMID:26966555

  17. Carbon Fiber Biocompatibility for Implants.

    PubMed

    Petersen, Richard

    Carbon fibers have multiple potential advantages in developing high-strength biomaterials with a density close to bone for better stress transfer and electrical properties that enhance tissue formation. As a breakthrough example in biomaterials, a 1.5 mm diameter bisphenol-epoxy/carbon-fiber-reinforced composite rod was compared for two weeks in a rat tibia model with a similar 1.5 mm diameter titanium-6-4 alloy screw manufactured to retain bone implants. Results showed that carbon-fiber-reinforced composite stimulated osseointegration inside the tibia bone marrow measured as percent bone area (PBA) to a great extent when compared to the titanium-6-4 alloy at statistically significant levels. PBA increased significantly with the carbon-fiber composite over the titanium-6-4 alloy for distances from the implant surfaces of 0.1 mm at 77.7% vs. 19.3% (p < 10(-8)) and 0.8 mm at 41.6% vs. 19.5% (p < 10(-4)), respectively. The review focuses on carbon fiber properties that increased PBA for enhanced implant osseointegration. Carbon fibers acting as polymer coated electrically conducting micro-biocircuits appear to provide a biocompatible semi-antioxidant property to remove damaging electron free radicals from the surrounding implant surface. Further, carbon fibers by removing excess electrons produced from the cellular mitochondrial electron transport chain during periods of hypoxia perhaps stimulate bone cell recruitment by free-radical chemotactic influences. In addition, well-studied bioorganic cell actin carbon fiber growth would appear to interface in close contact with the carbon-fiber-reinforced composite implant. Resulting subsequent actin carbon fiber/implant carbon fiber contacts then could help in discharging the electron biological overloads through electrochemical gradients to lower negative charges and lower concentration.

  18. SUPERNOVA SHOCK-WAVE-INDUCED CO-FORMATION OF GLASSY CARBON AND NANODIAMOND

    SciTech Connect

    Stroud, Rhonda; Chisholm, Matthew F; Heck, Phillipp; Alexander, Conel; Nittler, Larry

    2011-01-01

    Nanodiamond (ND) was the first extrasolar dust phase to be identified in meteorites. However, the 2 nm average size of the NDs precludes isotopic analysis of individual particles, and thus their origin(s) remains controversial. Using electron microscopy with subnanometer resolution, we show that ND separates from the Allende and Murchison meteorites are actually a two-phase mixture of ND and glassy carbon. This phase mixture is likely the product of supernova shock-wave transformation of pre-formed organics in the interstellar medium (ISM). The glassy carbon ND mixture is also a plausible contributor to the 2175 extinction feature in the diffuse ISM.

  19. Electrochemical reduction of nalidixic acid at glassy carbon electrode modified with multi-walled carbon nanotubes.

    PubMed

    Patiño, Yolanda; Pilehvar, Sanaz; Díaz, Eva; Ordóñez, Salvador; De Wael, Karolien

    2017-02-05

    The aqueous phase electrochemical degradation of nalidixic acid (NAL) is studied in this work, using cyclic voltammetry (CV) and differential pulse voltammetry (DPV) as instrumental techniques. The promotional effect of multi-walled carbon nanotubes (MWCNT) on the performance of glassy carbon electrodes is demonstrated, being observed that these materials catalyze the NAL reduction. The effect of surface functional groups on MWCNT -MWCNT-COOH and MWCNT-NH2-was also studied. The modification of glassy carbon electrode (GCE) with MWCNT leads to an improved performance for NAL reduction following the order of MWCNT>MWCNT-NH2>MWCNT-COOH. The best behavior at MWCNT-GCE is mainly due to both the increased electrode active area and the enhanced MWCNT adsorption properties. The NAL degradation was carried out under optimal conditions (pH=5.0, deposition time=20s and volume of MWCNT=10μL) using MWCNT-GCE obtaining an irreversible reduction of NAL to less toxic products. Paramaters as the number of DPV cycles and the volume/area (V/A) ratio were optimized for maximize pollutant degradation. It was observed that after 15 DPV scans and V/A=8, a complete reduction was obtained, obtaining two sub-products identified by liquid chromatography-mass spectrometry (LC-MS).

  20. In-Vivo Characterization of Glassy Carbon Micro-Electrode Arrays for Neural Applications and Histological Analysis of the Brain Tissue

    NASA Astrophysics Data System (ADS)

    Vomero, Maria

    The aim of this work is to fabricate and characterize glassy carbon Microelectrode Arrays (MEAs) for sensing and stimulating neural activity, and conduct histological analysis of the brain tissue after the implant to determine long-term performance. Neural applications often require robust electrical and electrochemical response over a long period of time, and for those applications we propose to replace the commonly used noble metals like platinum, gold and iridium with glassy carbon. We submit that such material has the potential to improve the performances of traditional neural prostheses, thanks to better charge transfer capabilities and higher electrochemical stability. Great interest and attention is given in this work, in particular, to the investigation of tissue response after several weeks of implants in rodents' brain motor cortex and the associated materials degradation. As part of this work, a new set of devices for Electrocorticography (ECoG) has been designed and fabricated to improve durability and quality of the previous generation of devices, designed and manufactured by the same research group in 2014. In-vivo long-term impedance measurements and brain activity recordings were performed to test the functionality of the neural devices. In-vitro electrical characterization of the carbon electrodes, as well as the study of the adhesion mechanisms between glassy carbon and different substrates is also part of the research described in this book.

  1. A novel pattern transfer technique for mounting glassy carbon microelectrodes on polymeric flexible substrates

    NASA Astrophysics Data System (ADS)

    Vomero, Maria; van Niekerk, Pieter; Nguyen, Vivian; Gong, Nick; Hirabayashi, Mieko; Cinopri, Alessio; Logan, Kyle; Moghadasi, Ali; Varma, Priya; Kassegne, Sam

    2016-02-01

    We present a novel technology for transferring glassy carbon microstructures, originally fabricated on a silicon wafer through a high-temperature process, to a polymeric flexible substrate such as polyimide. This new transfer technique addresses a major barrier in Carbon-MEMS technology whose widespread use so has been hampered by the high-temperature pyrolysis process (⩾900 °C), which limits selection of substrates. In the new approach presented, patterning and pyrolysis of polymer precursor on silicon substrate is carried out first, followed by coating with a polymer layer that forms a hydrogen bond with glassy carbon and then releasing the ensuing glassy carbon structure; hence, transferring it to a flexible substrate. This enables the fabrication of a unique set of glassy carbon microstructures critical in applications that demand substrates that conform to the shape of the stimulated/actuated or sensed surface. Our findings based on Fourier transform infared spectroscopy on the complete electrode set demonstrate—for the first time—that carbonyl groups on polyimide substrate form a strong hydrogen bond with hydroxyl groups on glassy carbon resulting in carboxylic acid dimers (peaks at 2660 and 2585 cm-1). This strong bond is further confirmed by a tensile test that demonstrated an almost perfect bond between these materials that behave as an ideal composite material. Further, mechanical characterization shows that ultimate strain for such a structure is as high as 15% with yield stress of ~20 MPa. We propose that this novel technology not only offers a compelling case for the widespread use of carbon-MEMS, but also helps move the field in new and exciting directions.

  2. Preparation and characterization of dense graphite/glassy carbon composite coating for sealing application

    NASA Astrophysics Data System (ADS)

    Wang, Yang; Chen, Zhaofeng; Yu, Shengjie; Pan, Ning; Liao, Jiahao

    2017-09-01

    Glassy carbon (GC), characterized by a homogeneous structure and glass-like fracture surface once broken, has attracted increasing attention because of its excellent performance. In this paper, a dense graphite/glassy carbon composite coating with low gas permeability was introduced. In this composite coating, small graphite particles acting as second phase were wrapped by glassy carbon matrix. The composite coatings with different mass fractions of graphite particles were prepared. The mass loss of phenolic resin was determined by TG (thermogravimetry) analysis to determine the pyrolysis process. Raman spectrum analysis indicates that graphite content in composite coatings affected the G/D ratio significantly. The permeability of composite coatings with 50% and 100% graphite particles was almost same, which was ranged from 6  ×  10‑13 m3 · µm/m2 · s · Pa to 3  ×  10‑13 m3 · µm/m2 · s · Pa within the differential pressure from 100 kPa to 70 kPa. While the composite coating with 150% graphite particles had higher gas permeability due to the tiny micro-cracks and micro-pores produced. What was more, the densification mechanism of graphite/glassy carbon composite coating was also discussed in detail.

  3. Electrochemical Determination of Glycoalkaloids Using a Carbon Nanotubes-Phenylboronic Acid Modified Glassy Carbon Electrode

    PubMed Central

    Wang, Huiying; Liu, Mingyue; Hu, Xinxi; Li, Mei; Xiong, Xingyao

    2013-01-01

    A versatile strategy for electrochemical determination of glycoalkaloids (GAs) was developed by using a carbon nanotubes-phenylboronic acid (CNTs-PBA) modified glassy carbon electrode. PBA reacts with α-solanine and α-chaconine to form a cyclic ester, which could be utilized to detect GAs. This method allowed GA detection from 1 μM to 28 μM and the detection limit was 0.3 μM. Affinity interaction of GAs and immobilized PBA caused an essential change of the peak current. The CNT-PBA modified electrodes were sensitive for detection of GAs, and the peak current values were in quite good agreement with those measured by the sensors. PMID:24287539

  4. Amperometric biosensor based on glassy carbon electrode modified with long-length carbon nanotube and enzyme

    NASA Astrophysics Data System (ADS)

    Furutaka, Hajime; Nemoto, Kentaro; Inoue, Yuki; Hidaka, Hiroki; Muguruma, Hitoshi; Inoue, Hitoshi; Ohsawa, Tatsuya

    2016-05-01

    An amperometric biosensor based on a glassy carbon electrode modified with long-length multiwalled carbon nanotubes (MWCNTs) and enzyme nicotinamide-adenine-dinucleotide-dependent glucose dehydrogenase (GDH) is presented. We demonstrate the effect of the MWCNT length on the amperometric response of the enzyme biosensor. The long length of MWCNT is 200 µm (average), whereas the normal length of MWCNT is 1 µm (average). The response of the long MWCNT-GDH electrode is 2 times more sensitive than that of the normal-length MWCNT-GDH electrode in the concentration range from 0.25-35 mM. The result of electrochemical impedance spectroscopy measurements suggest that the long-length MWCNT-GDH electrode formed a better electron transfer network than the normal-length one.

  5. Electrochemical determination of glycoalkaloids using a carbon nanotubes-phenylboronic acid modified glassy carbon electrode.

    PubMed

    Wang, Huiying; Liu, Mingyue; Hu, Xinxi; Li, Mei; Xiong, Xingyao

    2013-11-27

    A versatile strategy for electrochemical determination of glycoalkaloids (GAs) was developed by using a carbon nanotubes-phenylboronic acid (CNTs-PBA) modified glassy carbon electrode. PBA reacts with α-solanine and α-chaconine to form a cyclic ester, which could be utilized to detect GAs. This method allowed GA detection from 1 μM to 28 μM and the detection limit was 0.3 μM. Affinity interaction of GAs and immobilized PBA caused an essential change of the peak current. The CNT-PBA modified electrodes were sensitive for detection of GAs, and the peak current values were in quite good agreement with those measured by the sensors.

  6. Evaluation in a Dog Model of Three Antimicrobial Glassy Coatings: Prevention of Bone Loss around Implants and Microbial Assessments.

    PubMed

    López-Píriz, Roberto; Solá-Linares, Eva; Rodriguez-Portugal, Mercedes; Malpica, Beatriz; Díaz-Güemes, Idoia; Enciso, Silvia; Esteban-Tejeda, Leticia; Cabal, Belén; Granizo, Juan José; Moya, José Serafín; Torrecillas, Ramón

    2015-01-01

    The aim of the present study is to evaluate, in a ligature-induced peri-implantitis model, the efficacy of three antimicrobial glassy coatings in the prevention of biofilm formation, intrasulcular bacterial growth and the resulting peri-implant bone loss. Mandibular premolars were bilaterally extracted from five beagle dogs. Four dental implants were inserted on each hemiarch. Eight weeks after, one control zirconia abutment and three with different bactericidal coatings (G1n-Ag, ZnO35, G3) were connected. After a plaque control period, bacterial accumulation was allowed and biofilm formation on abutments was observed by Scanning Electron Microscopy (SEM). Peri-implantitis was induced by cotton ligatures. Microbial samples and peri-implant crestal bone levels of all implant sites were obtained before, during and after the breakdown period. During experimental induce peri-implantitis: colony forming units counts from intrasulcular microbial samples at implants with G1n-Ag coated abutment remained close to the basal inoculum; G3 and ZnO35 coatings showed similar low counts; and anaerobic bacterias counts at control abutments exhibited a logarithmic increase by more than 2. Bone loss during passive breakdown period was no statistically significant. Additional bone loss occurred during ligature-induce breakdown: 0.71 (SD 0.48) at G3 coating, 0.57 (SD 0.36) at ZnO35 coating, 0.74 (SD 0.47) at G1n-Ag coating, and 1.29 (SD 0.45) at control abutments; and statistically significant differences (p<0.001) were found. The lowest bone loss at the end of the experiment was exhibited by implants dressing G3 coated abutments (mean 2.1; SD 0.42). Antimicrobial glassy coatings could be a useful tool to ward off, diminish or delay peri-implantitis progression.

  7. Evaluation in a Dog Model of Three Antimicrobial Glassy Coatings: Prevention of Bone Loss around Implants and Microbial Assessments

    PubMed Central

    López-Píriz, Roberto; Solá-Linares, Eva; Rodriguez-Portugal, Mercedes; Malpica, Beatriz; Díaz-Güemes, Idoia; Enciso, Silvia; Esteban-Tejeda, Leticia; Cabal, Belén; Granizo, Juan José; Moya, José Serafín; Torrecillas, Ramón

    2015-01-01

    Objectives The aim of the present study is to evaluate, in a ligature-induced peri-implantitis model, the efficacy of three antimicrobial glassy coatings in the prevention of biofilm formation, intrasulcular bacterial growth and the resulting peri-implant bone loss. Methods Mandibular premolars were bilaterally extracted from five beagle dogs. Four dental implants were inserted on each hemiarch. Eight weeks after, one control zirconia abutment and three with different bactericidal coatings (G1n-Ag, ZnO35, G3) were connected. After a plaque control period, bacterial accumulation was allowed and biofilm formation on abutments was observed by Scanning Electron Microscopy (SEM). Peri-implantitis was induced by cotton ligatures. Microbial samples and peri-implant crestal bone levels of all implant sites were obtained before, during and after the breakdown period. Results During experimental induce peri-implantitis: colony forming units counts from intrasulcular microbial samples at implants with G1n-Ag coated abutment remained close to the basal inoculum; G3 and ZnO35 coatings showed similar low counts; and anaerobic bacterias counts at control abutments exhibited a logarithmic increase by more than 2. Bone loss during passive breakdown period was no statistically significant. Additional bone loss occurred during ligature-induce breakdown: 0.71 (SD 0.48) at G3 coating, 0.57 (SD 0.36) at ZnO35 coating, 0.74 (SD 0.47) at G1n-Ag coating, and 1.29 (SD 0.45) at control abutments; and statistically significant differences (p<0.001) were found. The lowest bone loss at the end of the experiment was exhibited by implants dressing G3 coated abutments (mean 2.1; SD 0.42). Significance Antimicrobial glassy coatings could be a useful tool to ward off, diminish or delay peri-implantitis progression. PMID:26489088

  8. Elastic Properties of 4-6 nm-thick Glassy Carbon Thin Films

    NASA Astrophysics Data System (ADS)

    Manoharan, M. P.; Lee, H.; Rajagopalan, R.; Foley, H. C.; Haque, M. A.

    2010-09-01

    Glassy carbon is a disordered, nanoporous form of carbon with superior thermal and chemical stability in extreme environments. Freestanding glassy carbon specimens with 4-6 nm thickness and 0.5 nm average pore size were synthesized and fabricated from polyfurfuryl alcohol precursors. Elastic properties of the specimens were measured in situ inside a scanning electron microscope using a custom-built micro-electro-mechanical system. The Young's modulus, fracture stress and strain values were measured to be about 62 GPa, 870 MPa and 1.3%, respectively; showing strong size effects compared to a modulus value of 30 GPa at the bulk scale. This size effect is explained on the basis of the increased significance of surface elastic properties at the nanometer length-scale.

  9. Electrochemical synthesis of gold nanoparticles on the surface of multi-walled carbon nanotubes with glassy carbon electrode and their application

    NASA Astrophysics Data System (ADS)

    Song, Y. Z.; Li, X.; Song, Y.; Cheng, Z. P.; Zhong, H.; Xu, J. M.; Lu, J. S.; Wei, C. G.; Zhu, A. F.; Wu, F. Y.; Xu, J.

    2013-01-01

    Gold nanoparticles on the surface of multi-walled carbon nanotubes with glassy carbon electrode were prepared using electrochemical synthesis method. The thin films of gold Nanoparticles/multi-walled carbon nanotubes were characterized by scanning electron microscopy, powder X-ray diffraction, and cyclic voltammetry. Electrochemical behavior of adrenaline hydrochloride at gold nanoparticles/multi-walled carbon nanotube modified glassy carbon electrode was investigated. A simple, sensitive, and inexpensive method for determination of adrenaline hydrochloride was proposed.

  10. Electrochemical determination of gatifloxacin, moxifloxacin and sparfloxacin fluoroquinolonic antibiotics on glassy carbon electrode in pharmaceutical formulations.

    PubMed

    Radi, Abd-Elgawad; Wahdan, Tarek; Anwar, Zeinab; Mostafa, Hend

    2010-08-01

    Three fluoroquinolones; gatifloxacin (GAT), moxifloxacin (MOX) and sparfloxacin (SPAR) were electrochemically studied in various buffer systems at different pH values, using a glassy carbon electrode. The three fluoroquinolones were electrochemically oxidized at potential range (0.65-1.1 V) vs Ag-AgCl-KCl. The oxidation was irreversible and exhibited adsorption-controlled process behavior at all pH values and buffers studied. An electroanalytical methodology based on the adsorptive behavior of fluoroquinolones on glassy carbon electrode (GCE) and according to the linear relation between peak current and concentration using differential pulse voltammetry (DPV) method was successfully applied to the determination of the three fluoroquinolones in bulk and tablets. The proposed methods were statistically in agreement with that obtained by spectrophotometric comparison method. Copyright © 2010 John Wiley & Sons, Ltd.

  11. Low substrate temperature deposition of diamond coatings derived from glassy carbon

    DOEpatents

    Holcombe, C.E. Jr.; Seals, R.D.

    1995-09-26

    A process is disclosed for depositing a diamond coating on a substrate at temperatures less than about 550 C. A powder mixture of glassy carbon and diamond particles is passed through a high velocity oxy-flame apparatus whereupon the powders are heated prior to impingement at high velocity against the substrate. The powder mixture contains between 5 and 50 powder volume percent of the diamond particles, and preferably between 5 and 15 powder volume percent. The particles have a size from about 5 to about 100 micrometers, with the diamond particles being about 5 to about 30 micrometers. The flame of the apparatus provides a velocity of about 350 to about 1000 meters per second, with the result that upon impingement upon the substrate, the glassy carbon is phase transformed to diamond as coaxed by the diamond content of the powder mixture. 2 figs.

  12. Low substrate temperature deposition of diamond coatings derived from glassy carbon

    DOEpatents

    Holcombe, Jr., Cressie E.; Seals, Roland D.

    1995-01-01

    A process for depositing a diamond coating on a substrate at temperatures less than about 550.degree. C. A powder mixture of glassy carbon and diamond particles is passed through a high velocity oxy-flame apparatus whereupon the powders are heated prior to impingement at high velocity against the substrate. The powder mixture contains between 5 and 50 powder volume percent of the diamond particles, and preferably between 5 and 15 powder volume percent. The particles have a size from about 5 to about 100 micrometers, with the diamond particles being about 5 to about 30 micrometers. The flame of the apparatus provides a velocity of about 350 to about 1000 meters per second, with the result that upon impingement upon the substrate, the glassy carbon is phase transformed to diamond as coaxed by the diamond content of the powder mixture.

  13. Electrochemiluminescence of luminol at the titanate nanotubes modified glassy carbon electrode.

    PubMed

    Xu, Guifang; Zeng, Xiaoxue; Lu, Shuangyan; Dai, Hong; Gong, Lingshan; Lin, Yanyu; Wang, Qingping; Tong, Yuejin; Chen, Guonan

    2013-01-01

    A new strategy for the construction of a sensitive and stable electrochemiluminescent platform based on titanate nanotubes (TNTs) and Nafion composite modified electrode for luminol is described, TNTs contained composite modified electrodes that showed some photocatalytic activity toward luminol electrochemiluminescence emission, and thus could dramatically enhance luminol light emission. This extremely sensitive and stable platform allowed a decrease of the experiment electrochemiluminescence luminol reagent. In addition, in luminol solution at low concentrations, we compared the capabilities of a bare glassy carbon electrode with the TNT composite modified electrode for hydrogen peroxide detection. The results indicated that compared with glassy carbon electrode this platform was extraordinarily sensitive to hydrogen peroxide. Therefore, by combining with an appropriate enzymatic reaction, this platform would be a sensitive matrix for many biomolecules.

  14. Cytochrome c dynamics at gold and glassy carbon surfaces monitored by in situ scanning tunnel microscopy

    NASA Astrophysics Data System (ADS)

    Andersen, Jens E. T.; Møller, Per; Pedersen, Marianne V.; Ulstrup, Jens

    1995-02-01

    We have investigated the absorption of cytochrome c on gold and glassy carbon substrates by in situ scanning tunnel microscopy under potentiostatic control of both substrate and tip. Low ionic strength and potential ranges where no Faradaic current flows were used. Cyt c aggregates into flat composite structures of about 50 nm lateral extension at gold surfaces. The aggregates evolve in time, and structures resembling individual cyt c molecules can be distinguished in the space between the 50 nm structures. Cyt c aggregates also form at glassy carbon but have a different, unbroken character where cyt c both sticks well to the surface and exhibits notable mobility. The observations suggest that characteristic surface specific, internally mobile protein aggregates are formed at both surfaces and that in situ molecular resolution of the STM pictures may have been achieved.

  15. Kinetics of phase transformation of carbon nanotubes containing Se85Te10Ag5 glassy composites

    NASA Astrophysics Data System (ADS)

    Upadhyay, A. N.; Singh, Kedar

    2016-12-01

    Carbon nanotubes (CNTs) containing glassy composites [(Se85Te10Ag5)100-X(CNT)X] (X = 0, 3 and 5) have been prepared by the melt-quenching technique. The differential scanning calorimetry (DSC) technique was used to study changes in the kinetics of phase transformations of [(Se85Te10Ag5)100-X(CNT)X] (X = 0, 3 and 5) after the incorporation of CNTs under non-isothermal conditions at different heating rates (5, 10, 15 and 20 K min-1). The calculated values of the activation energy of crystallization (E c) and the Avrami index (n) decrease whereas the activation energy of the glass transition (E g) increases for CNTs containing glass composites; such effects are explained on the basis of effective CNTs mediating through a cross-link with the pure-Se85Te10Ag5 glassy matrix. The superiority of the CNT-Se85Te10Ag5 glassy composite over the pure glassy alloy have also been briefly mentioned in regard to electrical, thermal and mechanical properties at room temperature.

  16. Growth of InP single crystals by liquid encapsulated Czochralski (LEC) using glassy-carbon crucibles

    SciTech Connect

    Oliveira, C.E.M. de; Miskys, C.R.; Carvalho, M.M.G. de

    1996-12-31

    Using a high pressure puller and Glassy-Carbon crucibles, undoped InP single crystals weighing 100g and with 25 mm diameter were grown in the <100> direction. The residual carrier concentration of samples, measure by the Van der Pauw method at 300K, was about 5 {times} 10{sup 15}cm{sup {minus}3}, result as good as those obtained with Quartz crucibles with the advantage that Glassy-Carbon crucibles are fully reusable.

  17. Glassy carbon as an absolute intensity calibration standard for small-angle scattering.

    SciTech Connect

    Zhang, F.; Ilavsky, J.; Long, G.; Allen, A.; Quintana, J.; Jemian, P.; NIST

    2010-05-01

    Absolute calibration of small-angle scattering (SAS) intensity data (measured in terms of the differential scattering cross section per unit sample volume per unit solid angle) is essential for many important aspects of quantitative SAS analysis, such as obtaining the number density, volume fraction, and specific surface area of the scatterers. It also enables scattering data from different instruments (light, X-ray, or neutron scattering) to be combined, and it can even be useful to detect the existence of artifacts in the experimental data. Different primary or secondary calibration methods are available. In the latter case, absolute intensity calibration requires a stable artifact with the necessary scattering profile. Glassy carbon has sometimes been selected as this intensity calibration standard. Here we review the spatial homogeneity and temporal stability of one type of commercially available glassy carbon that is being used as an intensity calibration standard at a number of SAS facilities. We demonstrate that glassy carbon is sufficiently homogeneous and stable during routine use to be relied upon as a suitable standard for absolute intensity calibration of SAS data.

  18. Thermal and elastic characterization of glassy carbon thin films by photoacoustic measurements

    NASA Astrophysics Data System (ADS)

    Markushev, D. D.; Ordonez-Miranda, J.; Rabasović, M. D.; Chirtoc, M.; Todorović, D. M.; Bialkowski, S. E.; Korte, D.; Franko, M.

    2017-01-01

    A portable photoacoustic device is designed and applied to measure thermal diffusivity and linear thermal expansion coefficient of glassy carbon by means of the standard photoacoustic model involving both the thermal diffusion and thermoelastic contributions. This is done by measuring the evolution of the open-cell photoacoustic signal within the modulation frequency interval of 20 Hz-10 kHz, for four samples with thicknesses of 180μm, 140μm, 100μm, and 60μm. A proper fitting procedure of the theoretical amplitude and phase to their corresponding experimental counterparts yielded an average thermal diffusivity of 0.68mm^2·s^-1 and expansion coefficient of 4.3× 10^{-6} K-1 which are in good agreement with their values reported in the literature for glassy carbon. Furthermore, we demonstrate that the theoretical amplitude does not properly describe the thermoelastic behavior of the samples thinner than l ≤ 100 μm, due to their strong bending and vibrations driven by the highly disordered fullerene microstructure of glassy carbon followed by the increasing non-homogeneity effects violating 1D heat conduction.

  19. Gold nanoparticles directly modified glassy carbon electrode for non-enzymatic detection of glucose

    NASA Astrophysics Data System (ADS)

    Chang, Gang; Shu, Honghui; Ji, Kai; Oyama, Munetaka; Liu, Xiong; He, Yunbin

    2014-01-01

    This work describes controllable preparation of gold nanoparticles on glassy carbon electrodes by using the seed mediated growth method, which contains two steps, namely, nanoseeds attachment and nanocrystals growth. The size and the dispersion of gold nanoparticles grown on glassy carbon electrodes could be easily tuned through the growth time based on results of field-emission scanning electron microscopy. Excellent electrochemical catalytic characteristics for glucose oxidation were observed for the gold nanoparticles modified glassy carbon electrodes (AuNPs/GC), resulting from the extended active surface area provided by the dense gold nanoparticles attached. It exhibited a wide linear range from 0.1 mM to 25 mM with the sensitivity of 87.5 μA cm-2 mM-1 and low detection limit down to 0.05 mM for the sensing of glucose. The common interfering species such as chloride ion, ascorbic acid, uric acid and 4-acetamidophenol were verified having no interference effect on the detection of glucose. It is demonstrated that the seed mediated method is one of the facile approaches for fabricating Au nanoparticles modified substrates, which could work as one kind of promising electrode materials for the glucose nonenzymatic sensing.

  20. Flow injection catalase activity measurement based on gold nanoparticles/carbon nanotubes modified glassy carbon electrode.

    PubMed

    El Nashar, Rasha Mohamed

    2012-07-15

    Amperometric flow injection method of hydrogen peroxide analysis was developed based on catalase enzyme (CAT) immobilization on a glassy carbon electrode (GC) modified with electrochemically deposited gold nanoparticles on a multiwalled carbon nanotubes/chitosan film. The resulting biosensor was applied to detect hydrogen peroxide with a linear response range 1.0×10(-7)-2.5×10(-3)M with a correlation coefficient 0.998 and response time less than 10s. The optimum conditions of film deposition such as potential applied, deposition time and pH were tested and the flow injection conditions were optimized to be: flow rate of 3ml/min, sample volume 75μl and saline phosphate buffer of pH 6.89. Catalase enzyme activity was successfully determined in liver homogenate samples of rats, raised under controlled dietary plan, using a flow injection analysis system involving the developed biosensor simultaneously with spectrophotometric detection, which is the common method of enzymatic assay. Copyright © 2011. Published by Elsevier B.V.

  1. A Reliable Homemade Electrode Based on Glassy Polymeric Carbon

    ERIC Educational Resources Information Center

    Santos, Andre L.; Takeuchi, Regina M.; Oliviero, Herilton P.; Rodriguez, Marcello G.; Zimmerman, Robert L.

    2004-01-01

    The production of a GPC-based material by submitting a cross-linked resin precursor to control thermal conditions is discussed. The precursor material is prepolymerized at 60-degree Celsius in a mold and is carbonized in inert atmosphere by slowly raising the temperature, the rise is performed to avoid change in the shape of the carbonization…

  2. A Reliable Homemade Electrode Based on Glassy Polymeric Carbon

    ERIC Educational Resources Information Center

    Santos, Andre L.; Takeuchi, Regina M.; Oliviero, Herilton P.; Rodriguez, Marcello G.; Zimmerman, Robert L.

    2004-01-01

    The production of a GPC-based material by submitting a cross-linked resin precursor to control thermal conditions is discussed. The precursor material is prepolymerized at 60-degree Celsius in a mold and is carbonized in inert atmosphere by slowly raising the temperature, the rise is performed to avoid change in the shape of the carbonization…

  3. Direct electrochemistry and electrocatalysis of hemoglobin in nafion/carbon nanochip film on glassy carbon electrode.

    PubMed

    George, Sini; Lee, Hian Kee

    2009-11-26

    The use of heat treated carbon nanofibers, known as carbon nanochips (CNCs) for the studies of the direct electrochemistry and electrocatalytic properties of heme proteins, is demonstrated. A glassy carbon electrode (GCE) was modified with CNCs, and hemoglobin (Hb) was immobilized on the modified electrode surface by casting a film of Hb. Nafion was employed to fix the CNCs and Hb tightly on the surface of the GCE. The modified electrode was characterized by scanning electron microscopy. Ultraviolet-visible and Fourier transform infrared spectroscopy showed that Hb immobilized in the CNC film remained in its native structure. Electrochemical impedance spectroscopy and cyclic voltammetry (CV) were employed for electrochemical studies. The results showed that the presence of CNCs in the film can greatly enhance the electrochemical response of Hb. A pair of well-defined reversible CV peaks was observed, and the formal potential of the heme Fe(III)/Fe(II) redox couple was found to be -253 mV [vs Ag/AgCl (saturated KCl)]. The apparent heterogeneous electron-transfer rate constant (k(s)) was estimated as 2.54 s(-1). The modified electrode showed excellent electrocatalytic behavior to hydrogen peroxide (H(2)O(2)), trichloroacetic acid, and sodium nitrite. H(2)O(2) had a linear current response from 0.5 to 30 microM (R(2) = 0.9997; n = 5) with a detection limit of 0.05 microM when the signal-to-noise ratio was 3 and the apparent Michaelis-Menten constant (K(m)(app)) was 21.55 microM. These values suggest that CNCs are the best matrix described so far for the development of biosensors, far superior to untreated carbon nanofibers. The direct immobilization of proteins onto the surface of CNCs is shown to be a highly efficient method for the development of a new class of very sensitive, stable, and reproducible electrochemical biosensors.

  4. Voltammetric oxidation and determination of cinnarizine at glassy carbon electrode modified with multi-walled carbon nanotubes.

    PubMed

    Hegde, Rajesh N; Hosamani, Ragunatharaddi R; Nandibewoor, Sharanappa T

    2009-09-01

    The voltammetric oxidation of cinnarizine was investigated. In pH 2.5 Britton-Robinson buffer, cinnarizine shows an irreversible oxidation peak at about 1.20 V at a multi-walled carbon nanotube (MWCNT)-modified glassy carbon electrode. The cyclic voltammetric results indicate that MWCNT-modified glassy carbon electrode can remarkably enhance electrocatalytic activity towards the oxidation of cinnarizine. The electrocatalytic behavior was further exploited as a sensitive detection scheme for the cinnarizine determination by differential-pulse voltammetry. Under optimized conditions, the concentration range and detection limit are 9.0x10(-8) to 6.0x10(-6) M and 2.58x10(-9) M, respectively for cinnarizine. The proposed method was successfully applied to cinnarizine determination in pharmaceutical samples. The analytical performance of this sensor has been evaluated for the detection of analyte in urine as a real sample.

  5. Reactive Carbon Nano-Onion Modified Glassy Carbon Surfaces as DNA Sensors for Human Papillomavirus Oncogene Detection with Enhanced Sensitivity.

    PubMed

    Bartolome, Joanne P; Echegoyen, Luis; Fragoso, Alex

    2015-07-07

    Glassy carbon electrodes were modified with small carbon nano-onions (CNOs) and activated by electrografting of diazonium salts bearing terminal carboxylic acid and maleimide groups. The CNO-modified surfaces were characterized by ESEM and AFM microscopy as well as by electrochemical techniques. The modified electrodes were used for the amperometric detection of a model DNA target sequence associated with the human papillomavirus by immobilizing short recognition sequences by amidation or thiol-maleimide reactions. The analytical parameters of the developed biosensors were compared with glassy carbon electrodes without CNOs. In both cases, the incorporation of CNOs resulted in an enhancement in sensitivity and a decrease in detection limits ascribed to a combination of large surface areas and enhanced electron transfer properties of the CNO-modified electrodes. These results offer promise for the construction of other CNO-based biomolecule detection platforms with enhanced sensitivities.

  6. Laser micromilling of convex microfluidic channels onto glassy carbon for glass molding dies

    NASA Astrophysics Data System (ADS)

    Tseng, Shih-Feng; Chen, Ming-Fei; Hsiao, Wen-Tse; Huang, Chien-Yao; Yang, Chung-Heng; Chen, Yu-Sheng

    2014-06-01

    This study reports the fabrication of convex microfluidic channels on glassy carbon using an ultraviolet laser processing system to produce glass molding dies. The laser processing parameters, including various laser fluences and scanning speeds of galvanometers, were adjusted to mill a convex microchannel on a glassy carbon substrate to identify the effects of material removal. The machined glassy carbon substrate was then applied as a glass molding die to fabricate a glass-based microfluidic biochip. The surface morphology, milled width and depth, and surface roughness of the microchannel die after laser micromilling were examined using a three-dimensional confocal laser scanning microscope. This study also investigates the transcription rate of microchannels after the glass molding process. To produce a 180 μm high microchannel on the GC substrate, the optimal number of milled cycles, laser fluence, and scanning speed were 25, 4.9 J/cm2, and 200 mm/s, respectively. The width, height, and surface roughness of milled convex microchannels were 119.6±0.217 μm, 180.26±0.01 μm, and 0.672±0.08 μm, respectively. These measured values were close to the predicted values and suitable for a glass molding die. After the glass molding process, a typical glass-based microchannel chip was formed at a molding temperature of 660 °C and the molding force of 0.45 kN. The transcription rates of the microchannel width and depth were 100% and 99.6%, respectively. Thus, the proposed approach is suitable for performing in chemical, biochemical, or medical reactions.

  7. An impedance study of the adsorption of nucleic acid bases at glassy carbon electrodes.

    PubMed

    Oliveira-Brett, A M; Brett, C M A; Silva, L A

    2002-05-15

    Electrochemical impedance has been used to study the adsorption at glassy carbon electrodes of guanine, its corresponding nucleoside, guanosine, and adenine. Impedance studies at different concentrations and applied potentials show clearly that all three bases are adsorbed on the electrode, blocking the surface. Irradiating the electrode with low-frequency (20 kHz) ultrasound whilst recording the impedance spectra increased transport of molecules to the electrode surface with cavitation cleaning the surface and removing strongly adsorbed molecules of bases. In this way, sonoelectrochemical experiments enabled the electrode processes to be studied in the absence of adsorption.

  8. Glucose biosensor based on a glassy carbon electrode modified with polythionine and multiwalled carbon nanotubes.

    PubMed

    Tang, Wenwei; Li, Lei; Wu, Lujun; Gong, Jiemin; Zeng, Xinping

    2014-01-01

    A novel glucose biosensor was fabricated. The first layer of the biosensor was polythionine, which was formed by the electrochemical polymerisation of the thionine monomer on a glassy carbon electrode. The remaining layers were coated with chitosan-MWCNTs, GOx, and the chitosan-PTFE film in sequence. The MWCNTs embedded in FAD were like "conductive wires" connecting FAD with electrode, reduced the distance between them and were propitious to fast direct electron transfer. Combining with good electrical conductivity of PTH and MWCNTs, the current response was enlarged. The sensor was a parallel multi-component reaction system (PMRS) and excellent electrocatalytic performance for glucose could be obtained without a mediator. The glucose sensor had a working voltage of -0.42 V, an optimum working temperature of 25°C, an optimum working pH of 7.0, and the best percentage of polytetrafluoroethylene emulsion (PTFE) in the outer composite film was 2%. Under the optimised conditions, the biosensor displayed a high sensitivity of 2.80 µA mM(-1) cm(-2) and a low detection limit of 5 µM (S/N = 3), with a response time of less than 15 s and a linear range of 0.04 mM to 2.5 mM. Furthermore, the fabricated biosensor had a good selectivity, reproducibility, and long-term stability, indicating that the novel CTS+PTFE/GOx/MWCNTs/PTH composite is a promising material for immobilization of biomolecules and fabrication of third generation biosensors.

  9. Glucose Biosensor Based on a Glassy Carbon Electrode Modified with Polythionine and Multiwalled Carbon Nanotubes

    PubMed Central

    Tang, Wenwei; Li, Lei; Wu, Lujun; Gong, Jiemin; Zeng, Xinping

    2014-01-01

    A novel glucose biosensor was fabricated. The first layer of the biosensor was polythionine, which was formed by the electrochemical polymerisation of the thionine monomer on a glassy carbon electrode. The remaining layers were coated with chitosan-MWCNTs, GOx, and the chitosan-PTFE film in sequence. The MWCNTs embedded in FAD were like “conductive wires” connecting FAD with electrode, reduced the distance between them and were propitious to fast direct electron transfer. Combining with good electrical conductivity of PTH and MWCNTs, the current response was enlarged. The sensor was a parallel multi-component reaction system (PMRS) and excellent electrocatalytic performance for glucose could be obtained without a mediator. The glucose sensor had a working voltage of −0.42 V, an optimum working temperature of 25°C, an optimum working pH of 7.0, and the best percentage of polytetrafluoroethylene emulsion (PTFE) in the outer composite film was 2%. Under the optimised conditions, the biosensor displayed a high sensitivity of 2.80 µA mM−1 cm−2 and a low detection limit of 5 µM (S/N = 3), with a response time of less than 15 s and a linear range of 0.04 mM to 2.5 mM. Furthermore, the fabricated biosensor had a good selectivity, reproducibility, and long-term stability, indicating that the novel CTS+PTFE/GOx/MWCNTs/PTH composite is a promising material for immobilization of biomolecules and fabrication of third generation biosensors. PMID:24816121

  10. Glassy Carbons

    DTIC Science & Technology

    1975-02-01

    the layer plane spacing, d002; the in plane spacing, dll 0 , and the line broadening parameters, Lc and La, there is an experimentally significant...developed graphitic structure. The structure is certainly planar, with a near perfect graphitic spacing wi+hin planes. The line broadening parameters, Lc ...phase) Peak NVS: "Not Very Smooth" Peak 2P: Ŗ Phase" Peak 3P: ŗ Phase" Peak (002) Temp. Peak Sample Des,.qnation (rC) Type d(002) Lc d(10) La Graphite

  11. Electrochemical reduction of Brønsted acids by glassy carbon in acetonitrile-implications for electrocatalytic hydrogen evolution.

    PubMed

    McCarthy, Brian D; Martin, Daniel J; Rountree, Eric S; Ullman, Alexander C; Dempsey, Jillian L

    2014-08-18

    Molecular catalysts for electrochemically driven hydrogen evolution are often studied in acetonitrile with glassy carbon working electrodes and Brønsted acids. Surprisingly, little information is available regarding the potentials at which acids are directly reduced on glassy carbon. This work examines acid electroreduction in acetonitrile on glassy carbon electrodes by cyclic voltammetry. Reduction potentials, spanning a range exceeding 2 V, were found for 20 acids. The addition of 100 mM water was not found to shift the reduction potential of any acid studied, although current enhancement was observed for some acids. The data reported provides a guide for selecting acids to use in electrocatalysis experiments such that direct electrode reduction is avoided.

  12. Voltammetric Detection of Oxalic Acid by Using Glassy Carbon Electrodes with Covalently Attached Nitrogen-containing Functional Groups.

    PubMed

    Matsuura, Hiroaki; Akabe, Syuhei; Kitamura, Tsubasa; Takahashi, Takuto; Uchiyama, Shunichi

    2015-01-01

    We report on a novel voltammetric detection of oxalic acid by using glassy carbon electrodes with covalently attached nitrogen-containing functional groups prepared by stepwise electrolysis. A glassy carbon electrode electrooxidized in an ammonium carbamate solution was electroreduced at -1.0 V (vs. Ag/AgCl) in 1.0 M sulfuric acid for a long time. We found that the electrocatalytic oxidation wave of oxalic acid obtained by this modified glassy carbon electrode was moved to a more negative potential region than that obtained by a platinum electrode in an acidic medium. A good linearity for the peak current signals was observed in the concentration range from 0.1 to 50 mM.

  13. Magnetite-platinum nanoparticles-modified glassy carbon electrode as electrochemical detector for nitrophenol isomers.

    PubMed

    Gerent, Giles G; Spinelli, Almir

    2017-05-15

    A glassy carbon electrode was modified with magnetite and platinum nanoparticles stabilized with 3-n-propyl-4-picoline silsesquioxane chloride. This chemically-modified electrode is proposed for the first time for the individual or simultaneous electrochemical detection of nitrophenol isomers. Nanoparticles act as catalysts and also increase the surface area. The polymer stabilizes the particles and provides the electrochemical separation of isomers. Under optimized conditions, the reduction peak currents, obtained by differential-pulse voltammetry, of 2-, 3-, and 4-nitrophenol increased linearly with increases in their concentration in the range of 0.1-1.5μmolL(-1). In individual analysis, the detection limits were 33.7nmolL(-1), 45.3nmolL(-1) and 48.2nmolL(-1), respectively. Also, simultaneous analysis was possible for 2-, and 4-nitrophenol. In this case, the separation of the peak potentials was 0.138V and the detection limits were 69.6nmolL(-1) and 58.0nmolL(-1), respectively. These analytical figures of merit evidence the outstanding performance of the modified electrode, which was also successfully applied to the individual determination of isomers in environmental and biological samples. The magnetite and platinum nanoparticles modified glassy carbon electrode was able to detect nitrophenol isomers at the ppm level in rain water and human urine samples.

  14. Study of the electrochemical behavior of isorhamnetin on a glassy carbon electrode and its application.

    PubMed

    Liu, Ai-Lin; Zhang, Shao-Bo; Chen, Wei; Huang, Li-Ying; Lin, Xin-Hua; Xia, Xing-Hua

    2008-10-19

    The electrochemical behavior of isorhamnetin (ISO) at a glassy carbon electrode was studied in a phosphate buffer solution (PBS) of pH 4.0 by cyclic voltammetry (CV) and differential pulse voltammetric method (DPV). A well-defined redox wave of ISO involving one electrons and one proton appeared. The electrode reaction is a reactant weak adsorption-controlled process with a charge transfer coefficient (alpha) of 0.586. Based on the understanding of the electrochemical process of ISO at the glassy carbon electrode, analysis of ISO can be realized. Under optimal conditions, the oxidation peak current showed linear dependence on the concentration of ISO in the range of 1.0x10(-8) to 4.0x10(-7)M and 1.0x10(-6) to 1.0x10(-5)M. The detection limit is 5.0x10(-9)M. This method has been successfully applied to the detection of ISO in tablets.

  15. Electrochemical behavior of triflusal, aspirin and their metabolites at glassy carbon and boron doped diamond electrodes.

    PubMed

    Enache, Teodor Adrian; Fatibello-Filho, Orlando; Oliveira-Brett, Ana Maria

    2010-08-01

    The electrochemical behavior of triflusal (TRF) and aspirin (ASA), before and after hydrolysis in water and in alkaline medium using two different electrode surfaces, glassy carbon and boron doped diamond, was study by differential pulse voltammetry over a wide pH range. The hydrolysis products are 2-(hydroxyl)-4-(trifluoromethyl)-benzoic acid (HTB) for triflusal and salicylic acid (SA) for aspirin, which in vivo represent their main metabolites. The hydrolysis processes were also followed by spectrophotometry. The UV results showed complete hydrolysis after one hour for TRF and after two hours for ASA in alkaline solution. The glassy carbon electrode enables only indirect determination of TRF and ASA through the electrochemical detection of their hydrolysis products HTB and SA, respectively. The oxidation processes of HTB and SA are pH dependent and involve different numbers of electrons and protons. Moreover, the difference between the oxidation peak potential of SA and HTB was equal to 100 mV in the studied pH range from 1 to 8 due to the CF3 of the aromatic ring of HTB molecule. Due to its wider oxidation potential range, the boron doped diamond electrode was used to study the direct oxidation of TRF and ASA, as well as of their respective metabolites HTB and SA.

  16. Mediatorless solar energy conversion by covalently bonded thylakoid monolayer on the glassy carbon electrode.

    PubMed

    Lee, Jinhwan; Im, Jaekyun; Kim, Sunghyun

    2016-04-01

    Light reactions of photosynthesis that take place in thylakoid membranes found in plants or cyanobacteria are among the most effective ways of utilizing light. Unlike most researches that use photosystem I or photosystem II as conversion units for converting light to electricity, we have developed a simple method in which the thylakoid monolayer was covalently immobilized on the glassy carbon electrode surface. The activity of isolated thylakoid membrane was confirmed by measuring evolving oxygen under illumination. Glassy carbon surfaces were first modified with partial or full monolayers of carboxyphenyl groups by reductive C-C coupling using 4-aminobenzoic acid and aniline and then thylakoid membrane was bioconjugated through the peptide bond between amine residues of thylakoid and carboxyl groups on the surface. Surface properties of modified surfaces were characterized by cyclic voltammetry, contact angle measurements, and electrochemical impedance spectroscopy. Photocurrent of 230 nA cm(-2) was observed when the thylakoid monolayer was formed on the mixed monolayer of 4-carboxylpheny and benzene at applied potential of 0.4V vs. Ag/AgCl. A small photocurrent resulted when the 4-carboxyphenyl full monolayer was used. This work shows the possibility of solar energy conversion by directly employing the whole thylakoid membrane through simple surface modification.

  17. Nanoshaping field emitters from glassy carbon sheets: a new functionality induced by H-plasma etching.

    PubMed

    Gay, S; Orlanducci, S; Passeri, D; Rossi, M; Terranova, M L

    2016-09-14

    This paper reports on the morphological and electrical characterization at the nanometer scale and the investigation of the field emission characteristics of glassy carbon (GC) plates which underwent H-induced physical/chemical processes occurring in a dual-mode MW-RF plasma reactor. Plasma treatment produced on the GC surface arrays of vertically aligned conically shaped nanostructures, with density and height depending on the plasma characteristics. Two kinds of samples obtained under two different bias regimes have been deeply analyzed using an AFM apparatus equipped with tools for electric forces and surface potential measurements. The features of electron emission via the Field Emission (FE) mechanism have been correlated with the morphology and the structure at the nanoscale of the treated glassy carbon samples. The measured current density and the characteristics of the emission, which follow the Fowler-Nordheim law, indicate that the plasma-based methodology utilized for the engineering of the GC surfaces is able to turn conventional GC plates into efficient emission devices. The outstanding properties of GC suggest the use of such nanostructured materials for the assembling of cold cathodes to be used in a harsh environment and under extreme P/T conditions.

  18. Electrochemical behavior of an antiviral drug acyclovir at fullerene-C(60)-modified glassy carbon electrode.

    PubMed

    Shetti, Nagaraj P; Malode, Shweta J; Nandibewoor, Sharanappa T

    2012-12-01

    Electrochemical oxidation of acyclovir at fullerene-C(60)-modified glassy carbon electrode has been investigated using cyclic and differential pulse voltammetry. In pH 7.4 phosphate buffer, acyclovir showed an irreversible oxidation peak at about 0.96V. The cyclic voltammetric results showed that fullerene-C(60)-modified glassy carbon electrode can remarkably enhance electrocatalytic activity towards the oxidation of acyclovir. The electrocatalytic behavior was further exploited as a sensitive detection scheme for the acyclovir determination by differential pulse voltammetry. Effects of anodic peak potential (E(p)/V), anodic peak current (I(p)/μA) and heterogeneous rate constant (k(0)) have been discussed. Under optimized conditions, the concentration range and detection limit were 9.0×10(-8) to 6.0×10(-6)M and 1.48×10(-8)M, respectively. The proposed method was applied to acyclovir determination in pharmaceutical samples and human biological fluids such as urine and blood plasma as a real sample. This method can also be employed in quality control and routine determination of drugs in pharmaceutical formulations.

  19. Multilevel micro-structuring of glassy carbon for precision glass molding of diffractive optical elements

    NASA Astrophysics Data System (ADS)

    Prater, Karin; Dukwen, Julia; Scharf, Toralf; Herzig, Hans Peter; Plöger, Sven; Hermerschmidt, Andreas

    2015-03-01

    A consumer market for diffractive optical elements in glass can only be created if high efficient elements are available at affordable prices. In diffractive optics the efficiency and optical properties increases with the number of levels used, but in the same way the costs are multiplied by the number if fabrication steps. Replication of multilevel diffractive optical elements in glass would allow cost efficient fabrication but a suitable mold material is needed. Glassy carbon shows a high mechanical strength, thermal stability and non-sticking adhesion properties, which makes it an excellent candidate as mold material for precision compression molding of low and high glass-transition temperature materials. We introduce an 8 level micro structuring process for glassy carbon molds with standard photolithography and a Ti layer as hard mask for reactive ion etching. The molds were applied to thermal imprinting onto low and high transition temperature glass. Optical performance was tested for the molded samples with different designs for laser beamsplitters. The results show a good agreement to the design specification. Our result allow us to show limitations of our fabrication technique and we discussed the suitability of precision glass molding for cost efficient mass production with a high quality.

  20. Electrochemical Determination of Caffeine Content in Ethiopian Coffee Samples Using Lignin Modified Glassy Carbon Electrode.

    PubMed

    Amare, Meareg; Aklog, Senait

    2017-01-01

    Lignin film was deposited at the surface of glassy carbon electrode potentiostatically. In contrast to the unmodified glassy carbon electrode, an oxidative peak with an improved current and overpotential for caffeine at modified electrode showed catalytic activity of the modifier towards oxidation of caffeine. Linear dependence of peak current on caffeine concentration in the range 6 × 10(-6) to 100 × 10(-6) mol L(-1) with determination coefficient and method detection limit (LoD = 3 s/slope) of 0.99925 and 8.37 × 10(-7) mol L(-1), respectively, supplemented by recovery results of 93.79-102.17% validated the developed method. An attempt was made to determine the caffeine content of aqueous coffee extracts of Ethiopian coffees grown in four coffee cultivating localities (Wonbera, Wolega, Finoteselam, and Zegie) and hence to evaluate the correlation between users preference and caffeine content. In agreement with reported works, caffeine contents (w/w%) of 0.164 in Wonbera coffee; 0.134 in Wolega coffee; 0.097 in Finoteselam coffee; and 0.089 in Zegie coffee were detected confirming the applicability of the developed method for determination of caffeine in a complex matrix environment. The result indicated that users' highest preference for Wonbera and least preference for Zegie cultivated coffees are in agreement with the caffeine content.

  1. Tellurium-nanowire-coated glassy carbon electrodes for selective and sensitive detection of dopamine.

    PubMed

    Tsai, Hsiang-Yu; Lin, Zong-Hong; Chang, Huan-Tsung

    2012-05-15

    Tellurium-nanowire-coated glassy carbon electrodes (TNGCEs) have been fabricated and employed for selective and sensitive detection of dopamine (DA). TNGCEs were prepared by direct deposition of tellurium nanowires, 600 ± 150 nm in length and 16 ± 3 nm in diameter, onto glassy carbon electrodes, which were further coated with Nafion to improve their selectivity and stability. Compared to the GCE, the TNGCE is more electroactive (by approximately 1.9-fold) for DA, and its selectivity toward DA over ascorbic acid (AA) and uric acid (UA) is also greater. By applying differential pulse voltammetry, at a signal-to-noise ratio of 3, the TNGCE provides a limit of detection of 1 nM for DA in the presence of 0.5mM AA and UA. Linearity (R(2)=0.9955) of the oxidation current at 0.19 V against the concentration of DA is found over the range 5 nM-1 μM. TNGCEs have been applied to determine the concentration of dopamine to be 0.59 ± 0.07 μM in PC12 cells.

  2. Electrochemical study of functionalization on the surface of a chitin/platinum-modified glassy carbon paste electrode.

    PubMed

    Sugawara, Kazuharu; Yugami, Asako; Terui, Norifumi; Kuramitz, Hideki

    2009-11-01

    To functionalize chitin surfaces using proteins, we developed a glucose oxidase (GOD)-chitin/platinum-modified glassy carbon paste electrode (GCPE) as a model. In a weakly acidic solution, negatively charged GOD were immobilized by the protonated acetylamide groups on chitin. When the electrode was immersed in a solution containing GOD, the enzyme was readily immobilized due to the electrostatic interaction. In addition, measurements were performed using electrodes made with powders of different sizes because sensor performance depends on the particle sizes of glassy carbon powder.

  3. Nucleation and growth of thin films of the organic conductor TTF-iodide over glassy carbon. Electrochemical and spectroelectrochemical study.

    PubMed

    Gómez, L; Rodríguez-Amaro, R

    2009-04-21

    On the basis of the electrochemical and spectroelectrochemical behavior of thin films of TTF over a glassy carbon electrode in iodide media, a new, more complete mechanism for the electrode processes involved is proposed. The voltammetric and chronoamperometric results for the films can be explained in light of a recently developed nucleation-growth model involving a layer-by-layer mechanism. Also, their in situ UV-vis spectral data expand the available knowledge about the overall mechanism and the nature of the compound formed over the glassy carbon electrode.

  4. Detection of lead ions in picomolar concentration range using underpotential deposition on silver nanoparticles-deposited glassy carbon electrodes.

    PubMed

    Sivasubramanian, R; Sangaranarayanan, M V

    2011-09-30

    The efficacy of silver-deposited glassy carbon electrode for the determination of lead ions at the sub-nanomolar concentration ranges is investigated. The silver nanoparticles are electrodeposited on glassy carbon electrode using chronoamperometry and the electrode surface is characterized using SEM. Lead ions are detected in the region of underpotential deposition. The analysis is performed in square wave mode in the stripping voltammetry without the removal of oxygen. The detection limit of 10 pM has been obtained with a constant potential of -0.7 V during the electrodeposition step for a period of 50s. The interference of surfactants in the detection of lead ions is also studied.

  5. Anomalous Capacitance Maximum of the Glassy Carbon-Ionic Liquid Interface through Dilution with Organic Solvents.

    PubMed

    Bozym, David J; Uralcan, Betül; Limmer, David T; Pope, Michael A; Szamreta, Nicholas J; Debenedetti, Pablo G; Aksay, Ilhan A

    2015-07-02

    We use electrochemical impedance spectroscopy to measure the effect of diluting a hydrophobic room temperature ionic liquid with miscible organic solvents on the differential capacitance of the glassy carbon-electrolyte interface. We show that the minimum differential capacitance increases with dilution and reaches a maximum value at ionic liquid contents near 5-10 mol% (i.e., ∼1 M). We provide evidence that mixtures with 1,2-dichloroethane, a low-dielectric constant solvent, yield the largest gains in capacitance near the open circuit potential when compared against two traditional solvents, acetonitrile and propylene carbonate. To provide a fundamental basis for these observations, we use a coarse-grained model to relate structural variations at the double layer to the occurrence of the maximum. Our results reveal the potential for the enhancement of double-layer capacitance through dilution.

  6. An agglomeration induced glassy magnetic state in a carbon nanotube/NiO nanocomposite system.

    PubMed

    Chattopadhyay, S; Jana, S; Giri, S; Majumdar, S

    2012-10-31

    A series of nanocomposite materials were synthesized using multi-walled carbon nanotubes (MWCNTs) and NiO nanoparticles by varying the concentration of NiO in the MWCNT host matrix. Such an increment in the NiO particle density actually tunes the degree of isolation among the magnetic nanoparticles. Careful investigation by transmission electron microscopy shows that particle agglomeration increases substantially with NiO particle density. Field dependence of magnetization measurements depict a gradual enhancement of coercivity with increasing NiO concentration, signifying the enhancement of magnetic anisotropy in this nanocomposite system. Furthermore, field cooled and zero field cooled memory effect as well as magnetization relaxation measurements show that a glassy magnetic state gradually develops when the concentration increases. Analysis based on the result of high resolution transmission electron microscopy along with the magnetization data reveals that interparticle magnetic exchange interaction in the presence of interfacial disorders plays the major role in the emergence of the glassy magnetic state in this nanocomposite system.

  7. [Fusion implants of carbon fiber reinforced plastic].

    PubMed

    Früh, H J; Liebetrau, A; Bertagnoli, R

    2002-05-01

    Carbon fiber reinforced plastics (CFRP) are used in the medical field when high mechanical strength, innovative design, and radiolucency (see spinal fusion implants) are needed. During the manufacturing process of the material CFRP carbon fibers are embedded into a resin matrix. This resin material could be thermoset (e.g., epoxy resin EPN/DDS) or thermoplastic (e.g., PEAK). CFRP is biocompatible, radiolucent, and has higher mechanical capabilities compared to other implant materials. This publication demonstrates the manufacturing process of fusion implants made of a thermoset matrix system using a fiber winding process. The material has been used clinically since 1994 for fusion implants of the cervical and lumbar spine. The results of the fusion systems CORNERSTONE-SR C (cervical) and UNION (lumbar) showed no implant-related complications. New implant systems made of this CFRP material are under investigation and are presented.

  8. Electrochemical behavior and voltammetric determination of norfloxacin at glassy carbon electrode modified with multi walled carbon nanotubes/Nafion.

    PubMed

    Huang, Ke-Jing; Liu, Xue; Xie, Wan-Zhen; Yuan, Hong-Xia

    2008-07-15

    A simple and rapid electrochemical method is developed for the determination of trace-level norfloxacin, based on the excellent properties of multi-walled carbon nanotubes (MWCNTs). The MWCNTs/Nafion film-coated glassy carbon electrode (GCE) is constructed and the electrochemical behavior of norfloxacin at the electrode is investigated in detail. The results indicate that MWCNTs modified glassy carbon electrode exhibited efficiently electrocatalytic oxidation for norfloxacin (NFX) with relatively high sensitivity, stability and life time. Under conditions of cyclic voltammetry, the current for oxidation of selected analyte is enhanced significantly in comparison to the bare GCE. The electrocatalytic behavior is further exploited as a sensitive detection scheme for the analyte determinations by linear sweep voltammetry (LSV). Under optimized condition in voltammetric method the concentration calibration range and detection limit (S/N=3) are 0.1-100 micromol/L and 5 x 10(-8)mol/L for NFX. The proposed method was successfully applied to NFX determination in tablets. The analytical performance of this sensor has been evaluated for detection of the analyte in urine as a real sample.

  9. Determination of s-triazines with copper and glassy carbon electrodes. Flow injection analysis of aziprotryne in water samples.

    PubMed

    Zapardiel, A; Bermejo, E; Pérez, J A; Chicharro, M

    2000-07-01

    The detection and determination of s-triazines, atrazine-desethyl and aziprotryne by cyclic voltammetry and an amperometric method using a metallic copper electrode and a glassy carbon electrode are described. The concentrations of atrazine-desethyl and aziprotryne in 0.1 M NaOH solutions were determined using the oxidation signal corresponding to the Cu(0)/Cu(I) redox process. The detection level calculated for these s-triazines were 0.3 and 0.5 microg/mL of analyte, respectively. The glassy carbon electrode was shown to give sensitive reduction response to aziprotryne in flow injection mode. No special activation was required for the glassy carbon electrode. A detection limit of 0.2 microg/mL (20 ng aziprotryne) was obtained for a sample loop of 0.1 mL at a fixed potential of -1.0 V (vs. Ag/AgCl) in 0.1 M HCl and a flow rate of 3.5 mL/min. Furthermore, the glassy carbon electrode showed stable response in such a system, and the relative standard deviation was only 2.7% using the same surface, and 6.3% using different surfaces. The method developed was applied to the determination of aziprotryne in environmental and tap water samples; using a prior solid-phase extraction step, aziprotryne concentrations lower than 1.0 ng/mL could be measured.

  10. Determination of Norfloxacin by square-wave adsorptive voltammetry on a glassy carbon electrode.

    PubMed

    Ghoneim, M M; Radi, A; Beltagi, A M

    2001-05-01

    The adsorptive and electrochemical behavior of norfloxacin on a glassy carbon electrode were investigated by cyclic and square-wave voltammetry. Cyclic voltammetric studies indicated that the process was irreversible and fundamentally controlled by adsorption. To obtain a good sensitivity, the solution conditions and instrumental parameters were studied using square-wave voltammetry. In acetate buffer of pH 5.0, norfloxacin gave a sensitive adsorptive oxidative peak at 0.920 V (versus Ag-AgCl). Applicability to measurement of norfloxacin at submicromolar levels in urine samples was illustrated. The peak current was linear with the norfloxacin concentration in the range 5-50 microg ml(-1) urine. The detection limit was 1.1 microg ml(-1) urine.

  11. An electrochemically aminated glassy carbon electrode for simultaneous determination of hydroquinone and catechol.

    PubMed

    Wang, Xiuyun; Xi, Min; Guo, Mengmeng; Sheng, Fangmeng; Xiao, Guang; Wu, Shuo; Uchiyama, Shunichi; Matsuura, Hiroaki

    2016-02-07

    In this contribution, a very simple and reliable strategy based on the easy modification of a glassy carbon electrode (GCE) by pre-electrolyzing GCE in ammonium carbamate aqueous solution was employed for the simultaneous determination of hydroquinone (HQ) and catechol (CC). Compared with bare GCE, the incorporation of nitrogen into the GCE surface structure improved the electrocatalytic properties of GCE towards the electro-oxidation of HQ and CC. The nitrogen-introduced GCE (N-GCE) was evaluated for the simultaneous detection of HQ and CC and the linear ranges for HQ and CC were both from 5 to 260 μM. Their detection limits were both evaluated to be 0.2 μM (S/N = 3). The present method was applied for the determination of HQ and CC in real river water samples with recoveries of 95.0-102.1%. In addition, a possible detection mechanism of HQ and CC was discussed.

  12. Voltammetric Determination of Dopamine in Human Serum with Amphiphilic Chitosan Modified Glassy Carbon Electrode

    PubMed Central

    Wang, Cheng Yin; Wang, Zhi Xian; Zhu, Ai Ping; Hu, Xiao Ya

    2006-01-01

    An improvement of selectivity for electrochemical detection of dopamine (DA) with differential pulse voltammetry is achieved by covalently modifying a glassy carbon electrode (GCE) with O-carboxymethylchitosan (OCMCS). The amphiphilic chitosan provides electrostatic accumulation of DA onto the electrode surface. In a phosphate buffer solution (pH 6.0), a pair of well-defined reversible redox waves of DA was observed at the OCMCS/GCE with a ΔEp of 52 mV. The anodic peak current obtained from the differential pulse voltammetry of dopamine was linearly dependent on its concentration in the range of 6.0 × 10-8 to 7.0 × 10-6 M, with a correlation coefficient of 0.998. The detection limit (S/N = 3) was found to be 1.5 × 10-9 M. The modified electrode had been applied to the determination of DA in human serum samples with satisfactory results.

  13. Voltammetric Determination of Flunixin on Molecularly Imprinted Polypyrrole Modified Glassy Carbon Electrode

    PubMed Central

    Radi, Abd-Elgawad; Abd El-Ghany, Nadia; Wahdan, Tarek

    2016-01-01

    A novel electrochemical sensing approach, based on electropolymerization of a molecularly imprinted polypyrrole (MIPpy) film onto a glassy carbon electrode (GCE) surface, was developed for the detection of flunixin (FXN). The sensing conditions and the performance of the constructed sensor were assessed by cyclic, differential pulse and (DPV) square wave voltammetry (SWV). The sensor exhibited high sensitivity, with linear responses in the range of 5.0 to 50.0 µM with detection limits of 1.5 and 1.0 µM for DPV and SWV, respectively. In addition, the sensor showed high selectivity towards FXN in comparison to other interferents. The sensor was successfully utilized for the direct determination of FXN in buffalo raw milk samples. PMID:27242945

  14. Polymer modified glassy carbon electrode for the electrochemical determination of caffeine in coffee.

    PubMed

    Amare, Meareg; Admassie, Shimelis

    2012-05-15

    4-Amino-3-hydroxynaphthalene sulfonic acid (AHNSA) was electropolymerized on a glassy carbon electrode. The deposited film showed electrocatalytic activity towards the oxidation of caffeine. The polymer-modified electrode showed high sensitivity, selectivity and stability in the determination of caffeine in coffee. The peak current increased linearly with the concentration of caffeine in the range of 6 × 10(-8) to 4 × 10(-5) mol L(-1), with a detection limit of 1.37 × 10(-7) mol L(-1) (LoD = 3δ/slope). Analysis of caffeine in coffee was affected neither by sample matrices nor by structurally similar compounds. Recoveries ranging between 93.75 ± 2.32 and 100.75 ± 3.32 were achieved from coffee extracts indicating the applicability of the developed method for real sample analyses.

  15. X-ray parabolic lenses made from glassy carbon by means of laser

    NASA Astrophysics Data System (ADS)

    Artemiev, A.; Snigirev, A.; Kohn, V.; Snigireva, I.; Artemiev, N.; Grigoriev, M.; Peredkov, S.; Glikin, L.; Levtonov, M.; Kvardakov, V.; Zabelin, A.; Maevskiy, A.

    2006-06-01

    Parabolic planar compound refractive lenses (CRLs) made from glassy carbon by means of laser ablation are presented. They have radii of curvatures of 5 and 200μm and geometric apertures of 40 and 900μm, respectively. The numbers of biconcave elements in the CRLs were 4, 7, and 200. The planar lenses allow formation of a linear focus of length comparable with the depths of their profiles. Usage of two CRLs in a crossed geometry provides formation of two-dimensional focus. The lenses were tested at the European Synchrotron Radiation Facility at the bending magnet beam line BM-5. The minimum experimental size of the focus has been achieved as 1.4μm.

  16. Voltammetric Determination of Flunixin on Molecularly Imprinted Polypyrrole Modified Glassy Carbon Electrode.

    PubMed

    Radi, Abd-Elgawad; Abd El-Ghany, Nadia; Wahdan, Tarek

    2016-01-01

    A novel electrochemical sensing approach, based on electropolymerization of a molecularly imprinted polypyrrole (MIPpy) film onto a glassy carbon electrode (GCE) surface, was developed for the detection of flunixin (FXN). The sensing conditions and the performance of the constructed sensor were assessed by cyclic, differential pulse and (DPV) square wave voltammetry (SWV). The sensor exhibited high sensitivity, with linear responses in the range of 5.0 to 50.0 µM with detection limits of 1.5 and 1.0 µM for DPV and SWV, respectively. In addition, the sensor showed high selectivity towards FXN in comparison to other interferents. The sensor was successfully utilized for the direct determination of FXN in buffalo raw milk samples.

  17. A novel nitrite sensor based on graphene/polypyrrole/chitosan nanocomposite modified glassy carbon electrode.

    PubMed

    Ye, Daixin; Luo, Liqiang; Ding, Yaping; Chen, Qiang; Liu, Xiao

    2011-11-07

    A novel nitrite sensor was fabricated based on a graphene/polypyrrole/chitosan nanocomposite film modified glassy carbon electrode. The nanocomposite film was characterized by scanning electron microscopy, Fourier transform infrared spectroscopy and Raman spectroscopy. The electron transfer behaviour of the modified electrodes was investigated in [Fe(CN)(6)](3-)/(4-) redox probe using cyclic voltammetry and electrochemical impedance spectroscopy. Differential pulse voltammetry and amperometry were used to study the electrochemical properties of the proposed sensor. Under optimum conditions, the sensor exhibited good reproducibility and stability for nitrite determination. Linear response was obtained in the range of 0.5-722 μM with a detection limit of 0.1 μM (S/N = 3) for nitrite determination.

  18. Toward the Control of the Creation of Mixed Monolayers on Glassy Carbon Surfaces by Amine Oxidation.

    PubMed

    Groppi, Jessica; Bartlett, Philip N; Kilburn, Jeremy D

    2016-01-18

    A versatile and simple methodology for the creation of mixed monolayers on glassy carbon (GC) surfaces was developed, using an osmium-bipyridyl complex and anthraquinone as model redox probes. The work consisted in the electrochemical grafting on GC of a mixture of mono-protected diamine linkers in varying ratios which, after attachment to the surface, allowed orthogonal deprotection. After optimisation of the deprotection conditions, it was possible to remove one of the protecting groups selectively, couple a suitable osmium complex and cap the residual free amines. The removal of the second protecting group allowed the coupling of anthraquinone. The characterisation of the resulting surfaces by cyclic voltammetry showed the variation of the surface coverage of the two redox centres in relation to the initial ratio of the linking amine in solution.

  19. Fast Electrocatalytic Determination of Methimazole at an Activated Glassy Carbon Electrode

    PubMed Central

    Jalali, Fahimeh; Hatami, Zahra

    2016-01-01

    A fast and simple voltammetric method for the determination of methimazole in pharmaceutical products was reported. A glassy carbon electrode was pretreated by anodization at +1.75 V (vs. SCE) for 5 min, followed by potential cycling in the range of 0.3-1.3 V (20 cycles). The pretreated electrode showed an excellent electrocatalytic effect on the oxidation of methimazole. Compared with untreated electrode, a large decrease (~300 mV) in the oxidation peak of methimazole was observed. The oxidation peak current at the new potential (0.4 V vs. SCE) was linearly dependent on the concentration of methimazole in the range of 7.0 - 130 μM with a detection limit of 3.7 μM (S/N = 3). The method was successfully used in the determination of methimazole in thyramozol tablets. Due to the simple and fast electrode preparation, there is no need for electrode cleaning or storage. PMID:28243269

  20. Amperometric ascorbic acid sensor based on doped ferrites nanoparticles modified glassy carbon paste electrode.

    PubMed

    Dimitrijević, Teodora; Vulić, Predrag; Manojlović, Dragan; Nikolić, Aleksandar S; Stanković, Dalibor M

    2016-07-01

    In this study, a novel electrochemical sensor for quantification of ascorbic acid with amperometric detection in physiological conditions was constructed. For this purpose, cobalt and nickel ferrites were synthesized using microwave and ultrasound assistance, characterized by scanning electron microscopy (SEM), Fourier transform infrared (FTIR) spectroscopy, and X-ray powder diffraction (XRPD), and used for modification of glassy carbon paste electrode (GCPE). It was shown that introducing these nanoparticles to the structure of GCPE led to increasing analytical performance. Co ferrite modified GCPE (CoFeGCPE) showed better characteristics toward ascorbic acid sensing. The limit of detection (LOD) obtained by sensor was calculated to be 0.0270 mg/L, with linear range from 0.1758 to 2.6010 mg/L. This sensor was successfully applied for practical analysis, and the obtained results demonstrated that the proposed procedure could be a promising replacement for the conventional electrode materials and time-consuming and expensive separation methods.

  1. Amperometric sensing of hydrogen peroxide using glassy carbon electrode modified with copper nanoparticles

    SciTech Connect

    Sophia, J.; Muralidharan, G.

    2015-10-15

    In this paper, fabrication of glassy carbon electrode (GCE) modified with nano copper particles is discussed. The modified electrode has been tested for the non-enzymatic electrochemical detection of hydrogen peroxide (H{sub 2}O{sub 2}). The copper nanoparticles (Cu NPs) were prepared employing a simple chemical reduction method. The presence of Cu NPs was confirmed through UV–visible (UV–vis) absorption spectroscopy and X-ray diffraction (XRD) analysis. The size and morphology of the particles were investigated using transmission electron microscopy (TEM). The electrochemical properties of the fabricated sensor were studied via cyclic voltammetry (CV), chronoamperometry and electrochemical impedance spectroscopy (EIS). The electrochemical sensor displayed excellent performance features towards H{sub 2}O{sub 2} detection exhibiting wide linear range, low detection limit, swift response time, good reproducibility and stability.

  2. Multilevel micro-structuring of glassy carbon molds for precision glass molding

    NASA Astrophysics Data System (ADS)

    Prater, Karin; Dukwen, Julia; Scharf, Toralf; Herzig, Hans Peter; Plöger, Sven; Hermerschmidt, Andreas

    2015-09-01

    Replication techniques for diffractive optical elements (DOEs) in soft materials such as plastic injection molding are state of the art. For precision glass molding in glasses with high transition temperatures, molds with extreme thermal resistivity, low chemical reactivity and high mechanical strength are needed. Glassy Carbon can be operated up to 2000°C making it possible to mold almost all glasses including Fused Silica with a transition temperatures above 1060°C. For the structuring of Glassy Carbon wafers photolithography and a RIE process is used. We have developed a process using Si as a hard mask material. If the flow rates of the etching gases O2 and SF6 are chosen properly, high selectivity of GC to Si 19:1 can be achieved, which provides excellent conditions to realize high resolution elements with feature size down to 1 micron and fulfills requirements for optical applications. We fabricated several multilevel GC molds with 8 levels of structuring. Two different optical functionalities were implemented: 6x6 array beamsplitter and 1x4 linear beamsplitter. The molds were applied for precision glass molding of a low Tg glass L-BAL 42 (from Ohara) with a transition temperature of 565°C. Their optical performance was measured. A more detailed analysis of the impact of mold fabrication defects on optical performance is done. Rigorous coupled wave analysis simulations are performed, where we included fabrication constrains such as duty cycle, edge depth errors, wall verticality and misalignment errors. We will compare the results with the design specifications and discuss the influence of fabrication errors introduced during the different process steps.

  3. Gold nanoparticle/multi-walled carbon nanotube modified glassy carbon electrode as a sensitive voltammetric sensor for the determination of diclofenac sodium.

    PubMed

    Afkhami, Abbas; Bahiraei, Atousa; Madrakian, Tayyebeh

    2016-02-01

    A simple and highly sensitive sensor for the determination of diclofenac sodium based on gold nanoparticle/multi-walled carbon nanotube modified glassy carbon electrode is reported. Scanning electron microscopy along with energy dispersive X-ray spectroscopy, electrochemical impedance spectroscopy, cyclic voltammetry and square wave voltammetry was used to characterize the nanostructure and performance of the sensor and the results were compared with those obtained at the multi-walled carbon nanotube modified glassy carbon electrode and bare glassy carbon electrode. Under the optimized experimental conditions diclofenac sodium gave linear response over the range of 0.03-200μmolL(-1). The lower detection limits were found to be 0.02μmolL(-1). The effect of common interferences on the current response of DS was investigated. The practical application of the modified electrode was demonstrated by measuring the concentration of diclofenac sodium in urine and pharmaceutical samples. This revealed that the gold nanoparticle/multiwalled carbon nanotube modified glassy carbon electrode shows excellent analytical performance for the determination of diclofenac sodium in terms of a very low detection limit, high sensitivity, very good accuracy, repeatability and reproducibility. Copyright © 2015 Elsevier B.V. All rights reserved.

  4. Structural Modifications And Mechanical Degradation Of Ion Irradiated Glassy Polymer Carbon

    NASA Astrophysics Data System (ADS)

    Abunaemeh, Malek; Seif, Mohamed; Elsamadicy, Abdalla; Muntele, Claudiu; Ila, Daryush

    2011-06-01

    The TRISO fuel has been used in some of the Generation IV nuclear reactor designs. It consists of a fuel kernel of UOx coated with several layers of materials with different functions. Pyrolytic carbon (PyC) is one of the materials in the layers. In this study we investigate the possibility of using Glassy Polymeric Carbon (GPC) as an alternative to PyC. GPC is used for artificial heart valves, heat-exchangers, and other high-tech products developed for the space and medical industries. This lightweight material can maintain dimensional and chemical stability in adverse environment and very high temperatures (up to 3000 °C). In this work, we are comparing the changes in physical and microstructure properties of GPC after exposure to irradiation fluence of 5 MeV Ag equivalent to a 1 displacement per atom (dpa) at samples prepared at 1000, 1500 and 2000 °C. The GPC material is manufactured and tested at the Center for Irradiation Materials (CIM) at Alabama A&M University. Transmission electron microscopy (TEM) and Raman spectroscopy were used for analysis.

  5. Electrochemical determination of nitrite and iodate based on Pt nanoparticles self-assembled on a chitosan modified glassy carbon electrode.

    PubMed

    Li, Yongxin; Zhou, Yuan; Xian, Hongying; Wang, Lun; Huo, Jianqiang

    2011-01-01

    A promising electrochemical sensor was fabricated by the self-assembling of Pt nanoparticles (nano-Pts) on a chitosan (CS) modified glassy carbon electrode (GCE). A field-emission scanning electron microscope (FE-SEM), transmission electron microscopy (TEM) and electrochemical techniques were used for characterization of these composites. It has been found that nano-Pts are inserted into the CS layer uniformly, and have a larger surface area compared to the chitosan modified glassy carbon electrode. Electrocatalytic experiments for the oxidation of nitrite and the reduction of iodate have shown that nano-Pts/CS/GCE can decrease the over-potential and increase the faradic current, which can be used for the sensitive determination of nitrite and iodate. Moreover, the prepared modified electrode exhibits good reproducibility and stability, and it is possible that this novel electrochemical sensor can be applied in the sensing and/or biosensing field.

  6. Effects of Ion Beam on Nanoindentation Characteristics of Glassy Polymeric Carbon Surface

    SciTech Connect

    Rodrigues, M. G.; Da Cruz, N. C.; Rangel, E. C.; Zimmerman, R. L.; Ila, Dr. Daryush; Poker, David B; Hensley, Dale K

    2005-01-01

    Glassy polymeric carbon (GPC) is a useful material for medical applications due to its chemical inertness and biocompatible characteristics. Mitral and aortic and hydrocephalic valves are examples of GPC prosthetic devices that have been fabricated and commercialized in Brazil. In this work, ion beam was used to improve the mechanical characteristics of GPC surface and therefore to avoid the propagation of microcracks where the cardiac valves are more fragile. A control group of phenolic resin samples heat-treated at 300, 400, 700, 1000, 1500, and 2500 C was characterized by measuring their hardness and Young's reduced elastic modulus with the depth of indentation. The control group was compared to results obtained with samples heat-treated at 700, 1000, and 1500 C and bombarded with energetic ions of silicon, carbon, oxygen, and gold at energies of 5, 6, 8, and 10 MeV, respectively, with fluences between 1.0 x 10{sup 13} and 1.0 x 10{sup 16} ions/cm{sup 2}. GPC nonbombarded samples showed that hardness depends on the heat treatment temperature (HTT), with a maximum hardness for heat treatment at 1000 C. The comparison between the control group and bombarded group also showed that hardness, after bombardment, had a greater increase for samples prepared at 700 C than for samples prepared at higher temperatures. The Young's elastic modulus presents an exponential relationship with depth. The parameters obtained by fitting depend on the HTT and on the ion used in the bombardment more than on energy and fluence. The hardness results show clearly that bombardment can promote carbonization, increase the linkage between the chains of the polymeric material, and promote recombination of broken bonds in lateral groups that are more numerous for samples heat-treated at 700 C.

  7. Effect of the glassy carbon structure on the aspect ratio of micropoints of matrix field-emission cathodes prepared by thermochemical etching

    NASA Astrophysics Data System (ADS)

    Pleshkova, L. S.; Shesterkin, V. I.

    2016-11-01

    The application of thermochemical etching technology makes it possible to reveal and investigate the structure of SU-2000 glassy carbon using electron microscopy. The glassy carbon structure at the microscopic and nanoscopic levels is inhomogeneous and consists of pockets with an irregular cross section separated by partitions. This structure sets the limits on the aspect ratio of geometrical sizes and micropoint packing density in the matrix prepared by thermochemical etching.

  8. Electrocatalytic behaviour and application of manganese porphyrin/gold nanoparticle- surface modified glassy carbon electrodes

    NASA Astrophysics Data System (ADS)

    Sebarchievici, I.; Tăranu, B. O.; Birdeanu, M.; Rus, S. F.; Fagadar-Cosma, E.

    2016-12-01

    The main purpose of this research was to obtain manganese porphyrin/gold nanoparticle-modified glassy carbon electrodes and to use them for the detection of H2O2. Two sets of modified electrodes were prepared by drop-cast deposition of 5,10,15,20-tetra(4-methyl-phenyl)porphyrinato manganese(III) chloride alone and of the same Mn-porphyrin and gold-colloid solution and comparatively characterized by Raman, UV-vis, ellipsometry, AFM and TEM microscopy, XPS and cyclic voltammetry. XPS spectrum recorded for GC_MnP_nAu modified electrode displayed the characteristic signals of gold nanoparticles. The optical parameters have greater values for GC_MnP_nAu in comparison with GC_MnP, due to increasing charge transfer efficiency. The MnP_nAu film mediates the electron transfer between H2O2 and GC, evidenced by an increase in the current intensity of the anodic peak, and facilitates the electrochemical regeneration of oxidized H2O2 at cathodic potentials. From the cyclic voltammetry experiments a linear relationship between H2O2 concentration vs oxidation and reduction currents was observed. The linear dependence between density of current and the square root of the scan rate indicates that the oxidation and reduction processes of H2O2 are diffusion controlled. The GC_MnP_nAu modified electrode shows great potential as electrochemical sensor for determination of hydrogen peroxide.

  9. Electrochemical investigation of methyl parathion at gold-sodium dodecylbenzene sulfonate nanoparticles modified glassy carbon electrode.

    PubMed

    Li, Chunya; Wang, Zhengguo; Zhan, Guoqin

    2011-01-01

    A gold/sodium dodecylbenzene sulfonate nanoparticles modified glassy carbon electrode (nano-Au/SDBS/GCE) was electrochemically fabricated with a constant potential at -0.4V. The obtained nano-Au/SDBS/GCE was characterized with scanning electronic microscopy, X-ray photoelectron spectroscopy and electrochemical techniques. Electrochemical behaviors of methyl parathion at the nano-Au/SDBS/GCE were thoroughly investigated. Compared to the unmodified electrode, the peak current obviously increased and the oxidation peak potential negatively shifted. These changes indicated that the composite nanoparticles possess good electrocatalytic performance on the electrochemical reaction of methyl parathion. Experimental parameters such as deposition time, pH value and accumulation conditions were optimized. Under optimum conditions, the peak current corresponding to the oxidation of the hydroxylamine group was found in a good linear relationship with the methyl parathion concentration. In addition, a calibration curve with excellent linearity was obtained in the concentration range from 5.0×10(-7)molL(-1) to 1.0×10(-4)molL(-1) with an estimated detection limit of 8.6×10(-8)molL(-1) (S/N=3). The successful determination of methyl parathion in real samples demonstrated the usefulness and potential applications of this method.

  10. The Enhanced Photo-Electrochemical Detection of Uric Acid on Au Nanoparticles Modified Glassy Carbon Electrode

    NASA Astrophysics Data System (ADS)

    Shi, Yuting; Wang, Jin; Li, Shumin; Yan, Bo; Xu, Hui; Zhang, Ke; Du, Yukou

    2017-07-01

    In this work, a sensitive and novel method for determining uric acid (UA) has been developed, in which the glassy carbon electrode (GCE) was modified with electrodeposition Au nanoparticles and used to monitor the concentration of UA with the assistant of visible light illumination. The morphology of the Au nanoparticles deposited on GCE surface were characterized by scanning electron microscope (SEM) and the nanoparticles were found to be well-dispersed spheres with the average diameter approaching 26.1 nm. A series of cyclic voltammetry (CV) and differential pulse voltammetry (DPV) measurements have revealed that the introduction of visible light can greatly enhance both the strength and stability of response current due to the surface plasmon resonance (SPR). Specifically, the DPV showed a linear relationship between peak current and UA concentration in the range of 2.8 to 57.5 μM with the equation of I pa (μA) = 0.0121 c UA (μM) + 0.3122 ( R 2 = 0.9987). Herein, the visible light illuminated Au/GCE possesses a potential to be a sensitive electrochemical sensor in the future.

  11. Development of a new separation media using ultra-thin glassy carbon film modified silica.

    PubMed

    Wang, Hui; Olesik, Susan V

    2015-01-30

    A self-polymerizable octatetrayne, 1,8-dialdehydebenzyl-1,3,5,7-octatetrayne, is synthesized and covalently attached to an amino-functionalized surface of silica particles. The silica particles with a monolayer coverage of octatetrayne were then thermally processed to various final temperatures of 200, 400 and 700°C. The amino-functionalization, covalent attachment of octatetrayne and thermal process of silica particles were monitored by scanning electron microscopy (SEM), infrared (IR) spectroscopy and thermogravimetric analysis (TGA). The thermally processed particles were then packed into a capillary column and evaluated as a stationary phase for HPLC. After chromatographic evaluation, the optimized temperature for thermal processing was determined to be 400°C, which provides the best modified silica particles SiO2-OCT-T400 with an ultra-thin glassy carbon film coating. The linear solvation energy relationship model indicated that the primary contributors in retention are dispersion and H-bond basicity. The application of SiO2-OCT-T400 as a stationary phase was further demonstrated by successful separation of nonpolar hydrocarbons mixture and a nucleosides mixture.

  12. Electrochemistry of raloxifene on glassy carbon electrode and its determination in pharmaceutical formulations and human plasma.

    PubMed

    Bagheri, Akbar; Hosseini, Hadi

    2012-12-01

    The electrochemical behavior of raloxifene (RLX) on the surface of a glassy carbon electrode (GCE) has been studied by cyclic voltammetry (CV). The CV studies were performed in various supporting electrolytes, wide range of potential scan rates, and pHs. The results showed an adsorption-controlled and quasi-reversible process for the electrochemical reaction of RLX, and a probable redox mechanism was suggested. Under the optimum conditions, differential pulse voltammetry (DPV) was applied for quantitative determination of the RLX in pharmaceutical formulations. The DPV measurements showed that the anodic peak current of the RLX was linear to its concentration in the range of 0.2-50.0μM with a detection limit of 0.0750μM, relative standard deviation (RSD %) below 3.0%, and a good sensitivity. The proposed method was successfully applied for determination of the RLX in pharmaceutical and human plasma samples with a good selectivity and suitable recovery. Copyright © 2012 Elsevier B.V. All rights reserved.

  13. Corrosion of glassy carbon neural electrodes under electrical stimulation and chemical exposure

    NASA Astrophysics Data System (ADS)

    Gong, Nick Thomas

    Advances in research of neural prosthetics have led to the development of novel materials used for neural stimulation applications. Glassy carbon (GC) has demonstrated promise as a novel and robust material that can be used in such applications. This study focused on reporting the in-vitro testing of GC microelectrodes under stimulation and chemical exposure to simulate an in-vivo environment, and to determine corrosion. Microelectrode arrays were fabricated and tested for an electrochemical (EC) setup for long-term corrosion tests. GC electrode pillars were used to test the testing apparatus, and confirm its ability to stimulate the GC microelectrodes. Electrode stimulation was conducted over 7 and 14 day time periods in phosphate buffer saline (PBS) with two different types of hydrogen peroxide (H2O2), USP and ACS. Corrosion of GC neural microelectrode arrays was monitored by physical, chemical, and electrochemical characterization methods. GC corrosion was characterized and evaluated over the duration of this study. Both GC and platinum microelectrode arrays were subjected to the same parameters. USP H2O2 did not corrode GC electrodes and characterization revealed that a protective layer can be preventing further electrode degradation. ACS H2O2 corroded GC electrodes. Implications of this work have given insights and new directions on testing neural prosthetic microelectrode arrays for stimulation applications.

  14. Preparation of aminylferrocene/nanogold modified glassy carbon electrode and its electrocatalysis on dopamine.

    PubMed

    Wang, Cong; Wang, Guangfeng; Jiao, Shoufeng; Guo, Zhihua; Fang, Bin

    2007-01-01

    Aminylferrocene(FcAI)-Nanogold(NG) modified glassy carbon electrode (FcAI/NG/GCE) was prepared by the Au-N bond between Au and FcAI. Electrochemical impedance spectroscopy (EIS) was employed to study the surface of the modified electrode. The electrochemical behavior of dopamine (DA) on the modified electrode was investigated and it was found that the modified electrode had an obvious electrocatalytic effect on DA. Compared with a bare GCE, the modified electrode exhibited an apparent shift of the oxidation peak potential in the negative potential direction and a marked enhancement in the current response for DA. We investigated the determination of DA on the modified electrode by differential pulse voltammetry (DPV). Linear calibration curve was obtained in the range of 7.0 x 10(-7) mol/L to 6x10(-4) mol/L of DA in 0.1 mol/L phosphate buffer solution (pH = 7.0) with a correlation coefficient of 0.9989. The detection limit (S/N = 3) of DA was estimated to be 1.0 x 10(-7) mol/L. Especially, by using the modified electrode, we can separate the oxidation peaks of ascorbic acid (AA) and DA in the PBS and it was satisfactory for the determination of DA with the interference of AA.

  15. Construction of Au nanoparticles on choline chloride modified glassy carbon electrode for sensitive detection of nitrite.

    PubMed

    Wang, Po; Mai, Zhibin; Dai, Zong; Li, Yongxin; Zou, Xiaoyong

    2009-07-15

    A promising electrochemical sensor for sensitive determination of nitrite was fabricated by construction of Au nanoparticles on the surface of choline chloride (Ch) modified glassy carbon electrode (GCE). Field emission scanning electron microscope, powder X-ray diffraction, X-ray photoelectron spectroscopy and electrochemical techniques were used for the surface characterization of the modified electrode. It was demonstrated that Ch was covalently immobilized onto the GCE surface forming a planted Ch monolayer, which could provide a suitable supporting material for the construction of Au nanoparticles. As a result, the Au nanoparticles with average size of about 110 nm were assembled to form a flowerlike structure on the surface of Ch monolayer. Moreover, the uniform nano-Au/Ch film exhibited remarkable electrocatalytic activity towards the oxidation of nitrite with obvious reduction of overpotential. Under the optimum conditions, the linear range for the detection of nitrite was 4.0 x 10(-7) to 7.5 x 10(-4)M with a high sensitivity of 0.354 microA microM(-1), and a low detection limit of 1.0 x 10(-7)M. The proposed method was successfully applied in the detection of nitrite in water samples and sausage samples, and the results were consistent with those obtained by ion chromatography and UV-visible spectrophotometric methods.

  16. Behavior of the Ru-bda water oxidation catalyst covalently anchored on glassy carbon electrodes

    SciTech Connect

    Matheu, Roc; Francàs, Laia; Chernev, Petko; Ertem, Mehmed Z.; Batista, Victor; Haumann, Michael; Sala, Xavier; Llobet, Antoni

    2015-05-07

    Electrochemical reduction of the dizaonium complex, [RuII(bda)(NO)(N–N2)2]3+, 23+ (N–N22+ is 4-(pyridin-4-yl) benzenediazonium and bda2– is [2,2'-bipyridine]-6,6'-dicarboxylate), in acetone produces the covalent grafting of this molecular complex onto glassy carbon (GC) electrodes. Multiple cycling voltammetric experiments on the GC electrode generates hybrid materials labeled as GC-4, with the corresponding Ru-aqua complex anchored on the graphite surface. GC-4 has been characterized at pH = 7.0 by electrochemical techniques and X-ray absorption spectroscopy (XAS) and has been shown to act as an active catalyst for the oxidation of water to dioxygen. This new hybrid material has a lower catalytic performance than its counterpart in homogeneous phase and progressively decomposes to form RuO2 at the electrode surface. The resulting metal oxide attached at the GC electrode surface, GC-RuO2, is a very fast and rugged heterogeneous water oxidation catalyst with TOFis of 300 s–1 and TONs >45000. The observed performance is comparable to the best electrocatalysts reported so far, at neutral pH.

  17. Voltammetric determination of TBHQ at a glassy carbon electrode surface activated by in situ chemical oxidation.

    PubMed

    Wang, Zhen; Yang, Feng; Zheng, Hao; Qin, Xianjing; Luo, Jiaojiao; Li, Yue; Xiao, Dan

    2014-07-21

    In this article, a bare glassy carbon electrode (GCE) surface was directly activated by a simple in situ chemical method, which was characterized by scanning electron microscopy (SEM), atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS) and cyclic voltammetry (CV), differential pulse voltammetry (DPV) and electrochemical impedance spectroscopy (EIS). Based on these results, it was found that oxygen-containing functional groups at the modified GCE surface were enhanced with a low damage to the surface state. Hence, the modified GCE exhibited an excellent performance, such as the negatively charged surface, good reproducibility and high selectivity. The resulting electrode was applied as a sensitive sensor for detection of antioxidant tertiary butyl hydroquinone (TBHQ), and a good linear relationship was obtained between the oxidation peak current and the concentration in a broad range of 1.0 μM-1.1 mM, with detection limits of 67 nM (S/N = 3) by DPV. Electrochemical parameters of TBHQ on the resulting GCE were also investigated, suggesting that the modified GCE could promote electron transfer kinetics towards the electrochemical reaction of TBHQ. Besides, the present method was used for determination of TBHQ in jatropha biodiesel with recovery ranging from 95.2% to 103.2%.

  18. On the hybrid glassy carbon electrode/OligoThiophene/Ag(NP) interface.

    PubMed

    Tassinari, Francesco; Tancini, Erik; Innocenti, Massimo; Schenetti, Luisa; Fontanesi, Claudio

    2012-11-06

    GC/OligoThiophene/Ag(NP) hybrid interfaces are synthesized and characterized: GC is the glassy carbon surface; OligoThiophene stands for both an ultrathin bithiophene grafted film and a 4-Br-Bithiophene grafted polymer; Ag(NP) stands for silver nanoparticles. The hybrid interface preparation involves different steps: first, the electrode surface is functionalized through a combination of electrochemically assisted grafting (under reduction regime) and polymerization (under oxidation regime); then, silver nanoparticles are chemisorbed by dipping. In particular, an ultrathin film of grafted bithiophene can be obtained by applying one cyclic voltammetry reduction cycle (GC/BT surface), while subsequent cyclic voltammetry cycling under oxidation regime yields an immobilized 4Br-Bithiophene polymer (GC/4BrBT surface). AFM and TEM images were recorded to investigate the morphology and chemical composition of the Ag(NP). Fe(II)/Fe(III) cyclic voltammetry, Zn underpotential deposition (UPD), XPS, LA-ICP-MS, and Raman techniques were exploited to characterize both the GC/OligoThiophene and GC/OligoThiophene/Ag(NP) interfaces. Theoretical calculation, at the B3LYP/6-311G** level of the theory, enabled rationalization of the electroreduction mechanism and the Raman results.

  19. Transport effects in the electrooxidation of methanol studied on nanostructured Pt/glassy carbon electrodes.

    PubMed

    Seidel, Y E; Schneider, A; Jusys, Z; Wickman, B; Kasemo, B; Behm, R J

    2010-03-02

    Transport effects in the methanol oxidation reaction (MOR) were investigated using nanostructured Pt/glassy carbon (GC) electrodes and, for comparison, a polycrystalline Pt electrode. The nanostructured Pt/GC electrodes, consisting of a regular array of catalytically active cylindrical Pt nanostructures with 55 +/- 10 nm in diameter and different densities supported on a planar GC substrate, were fabricated employing hole-mask colloidal lithography (HCL). The MOR measurements were performed under controlled transport conditions in a thin-layer flow cell interfaced to a differential electrochemical mass spectrometry (DEMS) setup. The measurements reveal a distinct variation in the MOR activity and selectivity (product distribution) with Pt nanostructure density and with electrolyte flow rate, showing an increasing overall activity, reflected by a higher Faradaic reaction current, as well as a pronounced increase of the turnover frequency for CO(2) formation and of the CO(2) current efficiency with decreasing flow rate and increasing Pt coverage. These findings are discussed in terms of the "desorption-readsorption-reaction" model introduced recently (Seidel et al. Faraday Discuss. 2008, 140, 67). Finally, consequences for applications in direct methanol fuel cells are outlined.

  20. Ultrasensitive Determination of Piroxicam at Diflunisal-Derived Gold Nanoparticle-Modified Glassy Carbon Electrode

    NASA Astrophysics Data System (ADS)

    Shaikh, Tayyaba; uddin, SiraJ; Talpur, Farah N.; Khaskeli, Abdul R.; Agheem, Muhammad H.; Shah, Muhammad R.; Sherazi, Tufail H.; Siddiqui, Samia

    2017-10-01

    We present a simple and green approach for synthesis of gold nanoparticles (AuNps) using analgesic drug diflunisal (DF) as capping and stabilizing agent in aqueous solution. Characterization of the synthesized diflunisal-derived gold nanoparticles (DF-AuNps) was performed by ultraviolet-visible (UV-Vis) spectroscopy, revealing the surface plasmon absorption band at 520 nm under optimized experimental conditions. Fourier-transform infrared (FTIR) spectroscopy established the effective interaction of the capping agent with the AuNps. Topographical features of the synthesized DF-AuNps were assessed by atomic force microscopy (AFM), revealing average particle height of 29 nm to 32 nm. X-ray diffractometry was used to study the crystalline nature, revealing that the synthesized DF-AuNps possessed excellent crystalline properties. The synthesized DF-AuNps were employed to modify the surface of glassy carbon electrode (GCE) for selective determination of piroxicam (PX) using differential pulse voltammetry technique. The fabricated Nafion/DF-AuNps/GCE sensor exhibited high sensitivity compared with bare GCE. The current response of the fabricated sensor was found to be linear in the PX concentration range of 0.5 μM to 50 μM, with limit of detection (LOD) and limit of quantification (LOQ) of 50 nM and 150 nM, respectively. The proposed sensor was successfully utilized for sensitive and rapid determination of PX in human serum, urine, and pharmaceutical samples.

  1. Behavior of the Ru-bda water oxidation catalyst covalently anchored on glassy carbon electrodes

    DOE PAGES

    Matheu, Roc; Francàs, Laia; Chernev, Petko; ...

    2015-05-07

    Electrochemical reduction of the dizaonium complex, [RuII(bda)(NO)(N–N2)2]3+, 23+ (N–N22+ is 4-(pyridin-4-yl) benzenediazonium and bda2– is [2,2'-bipyridine]-6,6'-dicarboxylate), in acetone produces the covalent grafting of this molecular complex onto glassy carbon (GC) electrodes. Multiple cycling voltammetric experiments on the GC electrode generates hybrid materials labeled as GC-4, with the corresponding Ru-aqua complex anchored on the graphite surface. GC-4 has been characterized at pH = 7.0 by electrochemical techniques and X-ray absorption spectroscopy (XAS) and has been shown to act as an active catalyst for the oxidation of water to dioxygen. This new hybrid material has a lower catalytic performance than its counterpartmore » in homogeneous phase and progressively decomposes to form RuO2 at the electrode surface. The resulting metal oxide attached at the GC electrode surface, GC-RuO2, is a very fast and rugged heterogeneous water oxidation catalyst with TOFis of 300 s–1 and TONs >45000. The observed performance is comparable to the best electrocatalysts reported so far, at neutral pH.« less

  2. Voltammetric determination of 4-nitrophenol at a sodium montmorillonite-anthraquinone chemically modified glassy carbon electrode.

    PubMed

    Hu, S; Xu, C; Wang, G; Cui, D

    2001-03-30

    A new method for the determination of 4-nitrophenol(4-NP) by differential pulse voltammetry (DPV) based on adsorptive stripping technique was described. Cyclic voltammetry (CV) and linear scan voltammetry (LSV) were used in a comparative investigation into the electrochemical reduction of 4-NP at a Na-montmorillonite(SWy-2) and anthraquione (AQ) modified glassy carbon electrode. With this chemically modified electrode, 4-NP was first irreversibly reduced from phiNO(2) to phiNHOH at -0.78 V. A couple of well-defined redox peaks at +0.22 V (vs. SCE) were responsible for a two-electron redox peak between phiNHOH and phiNO. Studies on the effect of pH on the peak height and peak potential were carried out over the pH range 2.0-9.0 with the phosphate buffer solution. A pH of 3.4 was chosen as the optimum pH. The other experimental parameters, such as film thickness, accumulation time and potential etc. were optimized. Anodic peak currents were found to be linearly related to concentration of 4-NP over the range 0.3-45 mg l(-1), with a detection limit of 0.02 mg l(-1). The interference of organic and inorganic species on the voltammetric response have been studied. This modified electrode can be used to the determination of 4-NP in water samples.

  3. Electrochemical behavior of the antifungal agents itraconazole, posaconazole and ketoconazole at a glassy carbon electrode.

    PubMed

    Knoth, H; Scriba, G K E; Buettner, B

    2015-06-01

    The electrochemical behavior of the azole antifungal agents itraconazole, posaconazole and ketoconazole has been investigated at a glassy carbon working electrode using cyclic voltammetry. All measurements were carried out in a supporting electrolyte solution consisting of a 1:1 (v/v) mixture of 0.1 mol L(-1) sodium phosphate buffers and acetonitrile at various substance concentrations and pH values. An amperometric cell with a three electrode system consisting of a working electrode, a palladium reference electrode and a platinum disk as the auxiliary electrode was used in all experiments. All azoles showed a similar electrochemical behavior involving two reactions. An irreversible oxidation occurred at potentials of about 0.5V. A reduction peak was detected at potentials between -0.28V and -0.14V with an associated oxidation peak, which was observed in consecutive repeated measurements at potentials between -0.03 and 0.28 V. The reduction and corresponding oxidation can be regarded as a quasi-reversible process. The proposed reaction mechanisms are an irreversible oxidation of the piperazine moiety at higher potentials as well as a reduction at lower potentials of the carbonyl group of the triazolone moiety in the case of itraconazole and posaconazole or a reduction of the methoxy group of ketoconazole.

  4. Graphene nanosheets modified glassy carbon electrode for simultaneous detection of heroine, morphine and noscapine.

    PubMed

    Navaee, Aso; Salimi, Abdollah; Teymourian, Hazhir

    2012-01-15

    In the present study, the graphene nanosheets (GNSs) modified glassy carbon (GC) electrode is employed for simultaneous determination of morphine, noscapine and heroin. To the best of our knowledge this is the first report of the simultaneous determination of these three important opiate drugs based on their direct electrochemical oxidation. Field emission scanning electron microscopy (FESEM) technique is utilized in order to study the surface morphology of the modified electrode. The modified electrode shows excellent electrocatalytic activity toward oxidation of morphine, noscapine and heroin at reduced overpotentials in wide pH range. In the performed experiments, differential pulse voltammetric determination of morphine, noscapine and heroin yields calibration curves with the following characteristics; linear dynamic range up to 65, 40 and 100 μM, sensitivity of 275, 500 and 217 nA μM(-1) cm(-2), and detection limits of 0.4, 0.2 and 0.5 μM at 3S(B), respectively. Fast response time, signal stability, high sensitivity, low cost and ease of preparation method without using any specific electron-transfer mediator or specific reagent are the advantageous of the proposed sensor. The modified electrode can be used for simultaneous or individual detection of three major narcotic components, heroin, noscapine and morphine at micromolar concentration without any separation or pretreatment steps.

  5. Glassy carbon electrodes modified with gold nanoparticles for the simultaneous determination of three food antioxidants.

    PubMed

    Lin, Xiaoyun; Ni, Yongnian; Kokot, Serge

    2013-02-26

    Electrochemical behavior of three antioxidants: butylated hydroxyanisole (BHA), butylated hydroxytoluene (BHT) and butylated hydroquinone (TBHQ), was investigated at a glassy carbon electrode modified with gold nanoparticles (AuNPs/GCE). This electrode was characterized by scanning electron microscopy (SEM). The experimental results indicated that the modified electrode was strongly electroactive during the redox reactions of BHA, BHT and TBHQ, and this was confirmed by the observed increased redox peak currents and shifted potentials; in addition, the oxidation products of BHA and TBHQ were found to be the same. The experimental conditions were optimized and the oxidation peaks of BHA and BHT were clearly separated. Based on this, an electrochemical method was researched and developed for the simultaneous determination of BHA, BHT and TBHQ in mixtures with the use of first derivative voltammetry; the linear concentration ranges were 0.10-1.50 μg mL(-1), 0.20-2.20 μg mL(-1) and 0.20-2.80 μg mL(-1), and detection limits were 0.039, 0.080 and 0.079μgmL(-1), for BHA, BHT and TBHQ, respectively. The proposed method was successfully applied for the analysis of the three analytes in edible oil samples. Copyright © 2012 Elsevier B.V. All rights reserved.

  6. Structure, texture, and properties of superconductive electrolytic niobium coatings on glassy carbon

    NASA Astrophysics Data System (ADS)

    Kolosov, V. N.; Shevyrev, A. A.

    2016-01-01

    Superconductive electrolytic niobium coatings 0.1-100 μm thick are prepared via electrochemical deposition onto SU-2000 glassy carbon substrates in (LiF + NaF + KF)eut-K2NbF7 molten salt. Their structure, texture, and residual stresses are investigated by X-ray diffraction methods. It is shown that, when depositing the coatings, the diffusion superconductive layer of niobium carbide is formed at the substrate-coating interface. The sequence of changes in the axis of the texture of niobium coating from <100> through <211> to a textureless state with an increase in their thickness is established. It is found that, in the interval 0.5-5 μm, the sign of the stress changes (compressive stresses change into tensile stresses) and it reaches its maximum value. With an increase in the coating thickness from 5 to 100 μm, tensile stresses decrease from 345 to 80 MPa. It is shown that the coatings formed can be used as the material for creating a working layer of a superconducting cryogenic gyroscope rotor.

  7. Enhanced electrochemical detection of ketorolac tromethamine at polypyrrole modified glassy carbon electrode.

    PubMed

    Santhosh, Padmanabhan; Senthil Kumar, Nagarajan; Renukadevi, Murugesan; Gopalan, Anantha Iyengar; Vasudevan, Thiyagarajan; Lee, Kwang-Pill

    2007-04-01

    A glassy carbon electrode modified with a coating of polypyrrole (Ppy) exhibited an attractive performance for the detection and determination of a non-steroidal and non-narcotic analgesic compound, ketorolac tromethamine (KT). Cyclic voltammetry, differential pulse and square wave voltammetry were used in a combined way to identify the electrochemical characteristics and to optimize the conditions for detection. For calibrating and estimating KT, square-wave voltammetry was mainly used. The drug shows a well-defined peak at -1.40 V vs. Ag/AgCl in the acetate buffer (pH 5.5). The existence of Ppy on the surface of the electrode gives higher electrochemical active sites at the electrode for the detection of KT and preconcentrate KT by adsorption. The square-wave stripping voltammetric response depends on the excitation signal and the accumulation time. The calibration curve is linear in the range 1 x 10(-11) to 1 x 10(-7) M with a detection limit of 1.0 x 10(-12) M. Applicability to serum samples was also demonstrated. A detection limit of 1.0 ng ml for serum was observed. Square-wave voltammetry shows superior performance over UV spectroscopy and other techniques.

  8. A voltammetric determination of caffeic acid in red wines based on the nitrogen doped carbon modified glassy carbon electrode

    NASA Astrophysics Data System (ADS)

    Karikalan, Natarajan; Karthik, Raj; Chen, Shen-Ming; Chen, Hsi-An

    2017-04-01

    We reported an electrochemical determination of caffeic acid (CA) based on the nitrogen doped carbon (NDC). The described sensor material was prepared by the flame synthesis method, which gave an excellent platform for the synthesis of carbon nanomaterials with the hetero atom dopant. The synthesized material was confirmed by various physical characterizations and it was further characterized by different electrochemical experiments. The NDC modified glassy carbon electrode (NDC/GCE) shows the superior electrocatalytic performance towards the determination of CA with the wide linear concentration range from 0.01 to 350 μM. It achieves the lowest detection limit of 0.0024 μM and the limit of quantification of 0.004 μM. The NDC/GCE-CA sensor reveals the good selectivity, stability, sensitivity and reproducibility which endorsed that the NDC is promising electrode for the determination of CA. In addition, NDC modified electrode is applied to the determination of CA in red wines and acquired good results.

  9. A voltammetric determination of caffeic acid in red wines based on the nitrogen doped carbon modified glassy carbon electrode

    PubMed Central

    Karikalan, Natarajan; Karthik, Raj; Chen, Shen-Ming; Chen, Hsi-An

    2017-01-01

    We reported an electrochemical determination of caffeic acid (CA) based on the nitrogen doped carbon (NDC). The described sensor material was prepared by the flame synthesis method, which gave an excellent platform for the synthesis of carbon nanomaterials with the hetero atom dopant. The synthesized material was confirmed by various physical characterizations and it was further characterized by different electrochemical experiments. The NDC modified glassy carbon electrode (NDC/GCE) shows the superior electrocatalytic performance towards the determination of CA with the wide linear concentration range from 0.01 to 350 μM. It achieves the lowest detection limit of 0.0024 μM and the limit of quantification of 0.004 μM. The NDC/GCE-CA sensor reveals the good selectivity, stability, sensitivity and reproducibility which endorsed that the NDC is promising electrode for the determination of CA. In addition, NDC modified electrode is applied to the determination of CA in red wines and acquired good results. PMID:28378813

  10. Glassy carbon/multi walled carbon nanotube/cadmium sulphide photoanode for light energy storage in vanadium photoelectrochemical cell

    NASA Astrophysics Data System (ADS)

    Peimanifard, Zahra; Rashid-Nadimi, Sahar

    2015-12-01

    The aim of this study is utilizing the artificial photosynthesis, which is an attractive and challenging theme in the photoelectrocatalytic water splitting, to charge the vanadium redox flow battery (VRFB). In this work multi walled carbon nanotube/cadmium sulphide hybrid is employed as a photoanode material to oxidize VO2+ to VO2+ for charging the positive vanadium redox flow battery's half-cell. Characterization studies are also described using the scanning electron microscopic-energy-dispersive X-ray spectroscopy (SEM-EDS), inductively coupled plasma atomic emission spectroscopy (ICP-AES) and UV-Visible methods. The phtoelectrochemical performance is characterized by cyclic voltammetry and chronoamperometry. Applied bias photon-to-current efficiency (ABPE) is achieved for both two and three-electrode configurations. The glassy carbon/multi walled carbon nanotube/cadmium sulphide yields high maximum ABPE of 2.6% and 2.12% in three and two-electrode setups, respectively. These results provide a useful guideline in designing photoelectrochemical cells for charging the vanadium redox flow batteries by sunlight as a low cost, free and abundant energy source, which does not rely on an external power input.

  11. Implantation of carbon in GaAs

    SciTech Connect

    Moll, Amy Jo

    1992-03-01

    Carbon implanted into GaAs and thermally annealed typically exhibits very low (<3%) electrical activity. It has been demonstrated that the electrical activity of C can be significantly enhanced by co-implantation with Ga. Improved activation may result from either additional damage of the crystal lattice or from stoichiometric changes, forcing the C atoms onto As sites. To determine the relative importance of each of these effects, I have undertaken a systematic study of carbon activation in GaAs. A range of co-implants have been used: group III (B, Ga), group V (N, P, As) and noble gases (Ar, Kr). The damage introduced to the substrate will depend on the mass of the ion implanted. The group III and group V co-implants will affect the crystal stoichiometry. The results indicate that both lattice damage and crystal stoichiometry are important for high electrical activity of C. Increasing the damage will increase the activation due to the increased number of As vacancies but maximum activation can be obtained only by a co-implant which not only damages the lattice but also forces the C to occupy an As site.

  12. [Study on implant material of carbon/carbon composites].

    PubMed

    Wang, Guohui; Yu, Shu; Zhu, Shaihong; Liu, Yong; Miu, Yunliang; Huang, Boyun

    2010-12-01

    This study was aimed to evaluate the biocompatibility and mechanical property of carbon/carbon composites. At first, carbon/carbon composites were prepared by chemical vapor deposition, and the mechanical property of carbon/carbon composites was tested. The biocompatibility of carbon/carbon composites was evaluated by cytotoxicity test, sensitization test, micronucleus test and implantation test. Mechanical property test showed such carbon/carbon composites are of good compression property and tension property. Cytotoxicity test showed that the leaching liquor of samples has no effect on the growth and proliferation of L-929 cells. The medullary micronucleus frequency of mouse was 2.3 per thousand +/- 0.7 per thousand in experiment group. The sensitization test showed that the skin of the subjects of experiment group had slight erythema and edema, which was 0.188 +/- 0.40 according to Magnusson and Kligman classification. Implantation test revealed that there was slight inflammation around the tissue after the implantation of sample. At 12 weeks, scanning electron microscopy and histopathological exam indicated that the samples of experiment group were of good histocompatibility; and in comparison with control group, there was no significant differences (P > 0.05). So these kinds of samples have good biocompatibility, mechanical property and prospects of clinical application.

  13. Amperometric sensing of anti-HIV drug zidovudine on Ag nanofilm-multiwalled carbon nanotubes modified glassy carbon electrode.

    PubMed

    Rafati, Amir Abbas; Afraz, Ahmadreza

    2014-06-01

    The zidovudine (ZDV) is the first drug approved for the treatment of HIV virus infection. The detection and determination of this drug are very importance in human serum because of its undesirable effects. A new ZDV sensor was fabricated on the basis of nanocomposite of silver nanofilm (Ag-NF) and multiwalled carbon nanotubes (MWCNTs) immobilized on glassy carbon electrode (GCE). The modified electrodes were characterized by scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), X-ray diffraction (XRD), cyclic voltammetry (CV), and linear sweep voltammetry (LSV) techniques. Results showed that the electrodeposited silver has a nanofilm structure and further electrochemical studies showed that the prepared nanocomposite has high electrocatalytic activity and is appropriate for using in sensors. The amperometric technique under optimal conditions is used for the determination of ZDV ranging from 0.1 to 400ppm (0.37μM-1.5mM) with a low detection limit of 0.04ppm (0.15μM) (S/N=3) and good sensitivity. The prepared sensor possessed accurate and rapid response to ZDV and shows an average recovery of 98.6% in real samples.

  14. A novel enzymatic glucose sensor based on Pt nanoparticles-decorated hollow carbon spheres-modified glassy carbon electrode

    NASA Astrophysics Data System (ADS)

    Luhana, Charles; Bo, Xiang-Jie; Ju, Jian; Guo, Li-Ping

    2012-10-01

    A new glucose biosensor was developed based on hollow carbon spheres decorated with platinum nanoparticles (Pt/HCSs)-modified glassy carbon electrode immobilized with glucose oxidase (GOx) with the help of Nafion. The Pt nanoparticles were well dispersed on the HCSs with an average size of 2.29 nm. The detection of glucose was achieved via electrochemical detection of the enzymatically liberated H2O2 at +0.5 V versus Ag/AgCl at physiologic pH of 7.4. The Pt/HCSs-modified electrode exhibited excellent electrocatalytic activities toward both the oxidation and reduction of H2O2. The glucose biosensor showed good electrocatalytic performance in terms of high sensitivity (4.1 μA mM-1), low detection limit (1.8 μM), fast response time <3 s, and wide linear range (0.04-8.62 mM). The apparent Michaelis-Menten constant ( K m) and the maximum current density ( i max) values for the biosensor were 10.94 mM and 887 μA cm-2 respectively. Furthermore, this biosensor showed an acceptable reproducibility and high stability. The interfering signals from ascorbic acid and uric acid at concentration levels normally found in human blood were not much compared with the response to glucose. Blood serum samples were also tested with this biosensor and a good recovery was achieved for the two spiked serum samples.

  15. Amperometric glucose sensor based on glucose oxidase immobilized on gelatin-multiwalled carbon nanotube modified glassy carbon electrode.

    PubMed

    Periasamy, Arun Prakash; Chang, Yu-Jung; Chen, Shen-Ming

    2011-02-01

    We investigated the direct electrochemistry of glucose oxidase (GOx) at gelatin-multiwalled carbon nanotube (GCNT) modified glassy carbon electrode (GCE). GOx was covalently immobilized onto GCNT modified GCE through the well known glutaraldehyde (GAD) chemistry. The immobilized GOx showed a pair of well-defined reversible redox peaks with a formal potential (E(0)') of -0.40V and a peak to peak separation (ΔE(p)) of 47mV. The surface coverage concentration (Г) of GOx in GCNT/GOx/GAD composite film modified GCE was 3.88×10(-9)mol cm(-2) which indicates the high enzyme loading. The electron transfer rate constant (k(s)) of GOx immobilized onto GCNT was 1.08s(-1) which validates a rapid electron transfer processes. The composite film shows linear response towards 6.30 to 20.09mM glucose. We observed a good sensitivity of 2.47μA mM(-)(1)cm(-2) for glucose at the composite film. The fabricated biosensor displayed two weeks stability. Moreover, it shows no response to 0.5mM of ascorbic acid (AA), uric acid (UA), acetaminophen (AP), pyruvate (PA) and lactate (LA) which shows its potential application in the determination of glucose from human serum samples. The composite film exhibits excellent recovery for glucose in human serum at physiological pH with good practical applicability. Copyright © 2010 Elsevier B.V. All rights reserved.

  16. Determination of oleuropein using multiwalled carbon nanotube modified glassy carbon electrode by adsorptive stripping square wave voltammetry.

    PubMed

    Cittan, Mustafa; Koçak, Süleyman; Çelik, Ali; Dost, Kenan

    2016-10-01

    A multi-walled carbon nanotube modified glassy carbon electrode was used to prepare an electrochemical sensing platform for the determination of oleuropein. Results showed that, the accumulation of oleuropein on the prepared electrode takes place with the adsorption process. Electrochemical behavior of oleuropein was studied by using cyclic voltammetry. Compared to the bare GCE, the oxidation peak current of oleuropein increased about 340 times at MWCNT/GCE. Voltammetric determination of oleuropein on the surface of prepared electrode was studied using square wave voltammetry where the oxidation peak current of oleuropein was measured as an analytical signal. A calibration curve of oleuropein was performed between 0.01 and 0.70µM and a good linearity was obtained with a correlation coefficient of 0.9984. Detection and quantification limits of the method were obtained as 2.73 and 9.09nM, respectively. In addition, intra-day and inter-day precision studies indicated that the voltammetric method was sufficiently repeatable. Finally, the proposed electrochemical sensor was successfully applied to the determination of oleuropein in an olive leaf extract. Microwave-assisted extraction of oleuropein had good recovery values between 92% and 98%. The results obtained with the proposed electrochemical sensor were compared with liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis. Copyright © 2016 Elsevier B.V. All rights reserved.

  17. Development of electrochemical method for the determination of olaquindox using multi-walled carbon nanotubes modified glassy carbon electrode.

    PubMed

    Xu, Tianci; Zhang, Lei; Yang, Jichun; Li, Na; Yang, Lijun; Jiang, Xiaoqing

    2013-05-15

    A simple and highly sensitive method for the electrochemical determination of olaquindox (OLA) was developed, which was carried out on the multi-walled carbon nanotubes (MWCNT) modified glassy carbon electrode (MWCNT/GCE) using cyclic voltammetry (CV) and differential pulse voltammetry (DPV). The results showed that MWCNT remarkably enhanced the reduction of OLA, which improved the cathodic peak current of OLA significantly. Under the optimum condition, the linear range for the calibration curve was 0.3-18.0 μg mL(-1) with a detection limit of 0.26 μg mL(-1). The MWCNT/GCE showed a well reproducibility and the relative standard deviation (R.S.D.) was 3.5% (n=9). And a great anti-interference ability of the MWCNT/GCE was also observed. Finally, the MWCNT/GCE was satisfactorily employed to analyze some synthetic and real water samples. Copyright © 2013 Elsevier B.V. All rights reserved.

  18. Amperometric uric acid biosensor based on poly(vinylferrocene)-gelatin-carboxylated multiwalled carbon nanotube modified glassy carbon electrode.

    PubMed

    Erden, Pınar Esra; Kaçar, Ceren; Öztürk, Funda; Kılıç, Esma

    2015-03-01

    In this study, a new uric acid biosensor was constructed based on ferrocene containing polymer poly(vinylferrocene) (PVF), carboxylated multiwalled carbon nanotubes (c-MWCNT) and gelatin (GEL) modified glassy carbon electrode (GCE). Uricase enzyme (UOx) was immobilized covalently through N-ethyl-N'-(3-dimethyaminopropyl) carbodiimide (EDC) and N-hydroxyl succinimide (NHS) chemistry onto c-MWCNT/GEL/PVF/GCE. The c-MWCNT/GEL/PVF composite was characterized by scanning electron microscopy, cyclic voltammetry and electrochemical impedance spectroscopy. Various experimental parameters such as pH, applied potential, enzyme loading, PVF and c-MWCNT concentration were investigated in detail. Under the optimal conditions the dynamic linear range of uric acid was 2.0×10(-7) M-7.1×10(-4) M (R=0.9993) with the detection limit low to 2.3×10(-8) M. With good selectivity and sensitivity, the biosensor was successfully applied to determine the uric acid in human serum. The results of the biosensor were in good agreement with those obtained from standard method. Therefore, the presented biosensor could be a good promise for practical applications in real samples.

  19. Voltammetric determination of antibacterial drug gemifloxacin in solubilized systems at multi-walled carbon nanotubes modified glassy carbon electrode.

    PubMed

    Jain, Rajeev; Rather, Jahangir Ahmad

    2011-04-01

    A sensitive electroanalytical method for determination of gemifloxacin in pharmaceutical formulation has been investigated on the basis of the enhanced electrochemical response at multi-walled carbon nanotubes modified glassy carbon electrode in the presence of CTAB. Solubilized system of different surfactants including SDS, Tween-20 and CTAB were taken for the study of electrochemical behaviour of gemifloxacin at modified electrode. The reduction peak current increases in the presence of CTAB while other surfactants show opposite effect. The modified electrode exhibits catalytic activity, high sensitivity, stability and is applicable over wide range of concentration for the determination of gemifloxacin. The mechanism of electrochemical reduction of gemifloxacin has been proposed on the basis of CV, SWV, DPV and coulometeric techniques. The proposed squarewave voltammetric method shows linearity over the concentration range 2.47-15.5 μg/mL. The achieved limits of detection (LOD) and quantification (LOQ) are 0.90 ng/mL and 3.0 ng/mL respectively. Crown Copyright © 2010. Published by Elsevier B.V. All rights reserved.

  20. Anodic stripping voltammetric determination of mercury using multi-walled carbon nanotubes film coated glassy carbon electrode.

    PubMed

    Yi, Hongchao

    2003-10-01

    An electrochemical method for the determination of trace levels of mercury based on a multi-walled carbon nanotubes (MWNT) film coated glassy carbon electrode (GCE) is described. In 0.1 mol L(-1) HCl solution containing 0.02 mol L(-1) KI, Hg(2+) was firstly preconcentrated at the MWNT film and then reduced at -0.60 V. During the anodic potential sweep, reduced mercury was oxidized, and then a sensitive and well-defined stripping peak at about -0.20 V appeared. Under identical conditions, a MWNT film coated GCE greatly enhances the stripping peak current of mercury in contrast to a bare GCE. Low concentrations of I(-) remarkably improve the determining sensitivity, since this increases the accumulation efficiency of Hg(2+) at the MWNT film coated GCE. The stripping peak current is proportional to the concentration of Hg(2+) over the range 8 x 10(-10)-5 x 10(-7) mol L(-1). The lowest detectable concentration of Hg(2+) is 2 x 10(-10) mol L(-1) at 5 min accumulation. The relative standard deviation (RSD) at 1 x 10(-8) mol L(-1) Hg(2+) was about 6% ( n=10). By using this proposed method, Hg(2+) in some water samples was determined, and the results were compared with those obtained by atomic absorption spectrometry (AAS). The two results are similar, suggesting that the MWNT-film coated GCE has great potential in practical analysis.

  1. An amperometric hydrogen peroxide biosensor based on Co3O4 nanoparticles and multiwalled carbon nanotube modified glassy carbon electrode

    NASA Astrophysics Data System (ADS)

    Kaçar, Ceren; Dalkiran, Berna; Erden, Pınar Esra; Kiliç, Esma

    2014-08-01

    In this work a new type of hydrogen peroxide biosensor was fabricated based on the immobilization of horseradish peroxidase (HRP) by cross-linking on a glassy carbon electrode (GCE) modified with Co3O4 nanoparticles, multiwall carbon nanotubes (MWCNTs) and gelatin. The introduction of MWCNTs and Co3O4 nanoparticles not only enhanced the surface area of the modified electrode for enzyme immobilization but also facilitated the electron transfer rate, resulting in a high sensitivity of the biosensor. The fabrication process of the sensing surface was characterized by scanning electron microscopy (SEM), cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). Amperometric detection of hydrogen peroxide was investigated by holding the modified electrode at -0.30 V (vs. Ag/AgCl). The biosensor showed optimum response within 5 s at pH 7.0. The optimized biosensor showed linear response range of 7.4 × 10-7-1.9 × 10-5 M with a detection limit of 7.4 × 10-7. The applicability of the purposed biosensor was tested by detecting hydrogen peroxide in disinfector samples. The average recovery was calculated as 100.78 ± 0.89.

  2. Amperometric choline biosensor based on multiwalled carbon nanotubes/zirconium oxide nanoparticles electrodeposited on glassy carbon electrode.

    PubMed

    Pundir, S; Chauhan, N; Narang, J; Pundir, C S

    2012-08-01

    A bienzymatic choline biosensor was constructed by coimmobilizing acetylcholinesterase (AChE) and choline oxidase (ChO) onto nanocomposite of carboxylated multiwalled carbon nanotubes (c-MWCNTs) and zirconium oxide nanoparticles (ZrO(2)NPs) electrodeposited on the surface of a glassy carbon electrode (GCE) and using it (AChE-ChO/c-MWCNT/ZrO(2)NPs/GCE) as working electrode, Ag/AgCl as reference electrode, and Pt wire as auxiliary electrode connected through a potentiostat. The enzyme electrode was characterized by scanning electron microscopy (SEM), Fourier transform infrared (FTIR) spectroscopy, and cyclic voltammetry (CV) studies, optimized, and evaluated. The biosensor exhibited optimum response within 4 s at +0.2V, pH 7.4, and 25 °C. The detection limit and working range of the biosensor were 0.01 μM and 0.05 to 200 μM, respectively. The half-life of the enzyme electrode was 60 days at 4 °C. The serum choline level, as measured by the biosensor, was 9.0 to 12.8 μmol/L (with a mean of 10.81 μmol/L) in apparently healthy persons and 5.0 to 8.4 μmol/L (with a mean of 6.53 μmol/L) in persons suffering from Alzheimer's disease. The enzyme electrode was unaffected by a number of serum substances.

  3. Fluorescence quenching studies of potential-dependent DNA reorientation dynamics at glassy carbon electrode surfaces.

    PubMed

    Li, Qin; Cui, Chenchen; Higgins, Daniel A; Li, Jun

    2012-09-05

    The potential-dependent reorientation dynamics of double-stranded DNA (ds-DNA) attached to planar glassy carbon electrode (GCE) surfaces were investigated. The orientation state of surface-bound ds-DNA was followed by monitoring the fluorescence from a 6-carboxyfluorescein (FAM6) fluorophore covalently linked to the distal end of the DNA. Positive potentials (i.e., +0.2 V vs open circuit potential, OCP) caused the ds-DNA to align parallel to the electrode surface, resulting in strong dipole-electrode quenching of FAM6 fluorescence. Switching of the GCE potential to negative values (i.e., -0.2 V vs OCP) caused the ds-DNA to reorient perpendicular to the electrode surface, with a concomitant increase in FAM6 fluorescence. In addition to the very fast (submilliseconds) dynamics of the initial reorientation process, slow (0.1-0.9 s) relaxation of FAM6 fluorescence to intermediate levels was also observed after potential switching. These dynamics have not been previously described in the literature. They are too slow to be explained by double layer charging, and chronoamperometry data showed no evidence of such effects. Both the amplitude and rate of the dynamics were found to depend upon buffer concentration, and ds-DNA length, demonstrating a dependence on the double layer field. The dynamics are concluded to arise from previously undetected complexities in the mechanism of potential-dependent ds-DNA reorientation. The possible origins of these dynamics are discussed. A better understanding of these dynamics will lead to improved models for potential-dependent ds-DNA reorientation at electrode surfaces and will facilitate the development of advanced electrochemical devices for detection of target DNAs.

  4. Toluidine blue adsorbed on alcohol dehydrogenase modified glassy carbon electrode for voltammetric determination of ethanol.

    PubMed

    Periasamy, Arun Prakash; Umasankar, Yogeswaran; Chen, Shen-Ming

    2011-01-15

    A novel toluidine blue O (TBO) adsorbed alcohol dehydrogenase (ADH) biocomposite film have been prepared through simple adsorption technique with the help of electrostatic interaction between oppositely charged layers. Nafion (NF) coating was made on top of the biocomposite film modified glassy carbon electrode (GCE) to protect ADH from leaching. The fabricated ADH/TBO/NF biocomposite electrode remains highly stable in the pH range from 4 to 13. More facile electron transfer process occurs at ADH/TBO/NF biocomposite than at TBO/NF film, which is obvious from the six folds increase in k(s) value. Maximum surface coverage concentration (Γ) of TBO is noticed at ADH/TBO/NF film, which is 82% higher than at TBO/NF and 15% higher than at ADH/TBO film modified GCEs. Electrochemical impedance spectroscopy studies reveal that ADH has been well immobilized in the biocomposite film. Scanning electron microscopy studies confirm the discriminate surface morphology of various components present in the biocomposite film. Cyclic voltammetry studies validate that ADH/TBO/NF biocomposite film exhibits excellent electrocatalytic activity for ethanol oxidation at low over potential (I(pa)=-0.14 V). The same studies show biocomposite film possesses a good sensitivity of 7.91 μAM(-1)cm(-2) for ethanol determination. This above sensitivity value is 17.40% higher than the sensitivity obtained for TBO/NF film (6.74 μAM(-1)cm(-2)). Further, using differential pulse voltammetry, a sensitivity of 1.70 μAM(-1)cm(-2) has been achieved for ADH/TBO/NF biocomposite film. Copyright © 2010 Elsevier B.V. All rights reserved.

  5. Passivation of carbon steel through mercury implantation

    NASA Technical Reports Server (NTRS)

    Wilbur, P. J.; Robinson, R. S.

    1981-01-01

    An experiment, in which carbon steel samples were implanted with mercury ions from a broad beam ion source and their corrosion characteristics in air were evaluated, is described. Mercury doses of a few mA min/square cm at energies of a few hundred electron volts are shown to effect significant improvements in the corrosion resistance of the treated surfaces. In a warm moist environment the onset of rusting was extended from 15 min. for an untreated sample to approximately 30 hrs. for one implanted at a dose of 33 mA min/square cm with 1000 eV mercury ions.

  6. Analytical applications of glassy carbon electrodes modified with multi-wall carbon nanotubes dispersed in polyethylenimine as detectors in flow systems.

    PubMed

    Sánchez Arribas, Alberto; Bermejo, Esperanza; Chicharro, Manuel; Zapardiel, Antonio; Luque, Guillermina L; Ferreyra, Nancy F; Rivas, Gustavo A

    2007-07-23

    This work reports the advantages of using glassy carbon electrodes (GCEs) modified with multi-wall carbon nanotubes (CNT) dispersed in polyethylenimine (PEI) as detectors in flow injection and capillary electrophoresis. The presence of the dispersion of CNT in PEI at the electrode surface allows the highly sensitive and reproducible determination of hydrogen peroxide, different neurotransmitters (dopamine (D) and its metabolite dopac, epinephrine (E), norepinephrine (NE)), phenolic compounds (phenol (P), 3-chlorophenol (3-CP) and 2,3-dichlorophenol (2,3CP)) and herbicides (amitrol). Sensitivities enhancements of 150 and 140 folds compared to GCE were observed for hydrogen peroxide and amitrol, respectively. One of the most remarkable properties of the resulting electrode is the antifouling effect of the CNT/PEI layer. No passivation was observed either for successive additions (30) or continuous flow (for 30 min) of the compounds under investigation, even dopac or phenol. A critical comparison of the amperometric and voltammetric signal of these different analytes at bare- and PEI-modified glassy carbon electrodes and pyrolytic graphite electrodes is also included, demonstrating that the superior performance of CNT is mainly due to their unique electrochemical properties. Glassy carbon electrodes modified with CNT-PEI dispersion also show an excellent performance as amperometric detector in the electrophoretic separation of phenolic compounds and neurotransmitters making possible highly sensitive and reproducible determinations.

  7. Electrochemical evaluation and determination of antiretroviral drug fosamprenavir using boron-doped diamond and glassy carbon electrodes.

    PubMed

    Gumustas, Mehmet; Ozkan, Sibel A

    2010-05-01

    Fosamprenavir is a pro-drug of the antiretroviral protease inhibitor amprenavir and is oxidizable at solid electrodes. The anodic oxidation behavior of fosamprenavir was investigated using cyclic and linear sweep voltammetry at boron-doped diamond and glassy carbon electrodes. In cyclic voltammetry, depending on pH values, fosamprenavir showed one sharp irreversible oxidation peak or wave depending on the working electrode. The mechanism of the oxidation process was discussed. The voltammetric study of some model compounds allowed elucidation of the possible oxidation mechanism of fosamprenavir. The aim of this study was to determine fosamprenavir levels in pharmaceutical formulations and biological samples by means of electrochemical methods. Using the sharp oxidation response, two voltammetric methods were described for the determination of fosamprenavir by differential pulse and square-wave voltammetry at the boron-doped diamond and glassy carbon electrodes. These two voltammetric techniques are 0.1 M H(2)SO(4) and phosphate buffer at pH 2.0 which allow quantitation over a 4 x 10(-6) to 8 x 10(-5) M range using boron-doped diamond and a 1 x 10(-5) to 1 x 10(-4) M range using glassy carbon electrodes, respectively, in supporting electrolyte. All necessary validation parameters were investigated and calculated. These methods were successfully applied for the analysis of fosamprenavir pharmaceutical dosage forms, human serum and urine samples. The standard addition method was used in biological media using boron-doped diamond electrode. No electroactive interferences from the tablet excipients or endogenous substances from biological material were found. The results were statistically compared with those obtained through an established HPLC-UV technique; no significant differences were found between the voltammetric and HPLC methods.

  8. A poly(3-acetylthiophene) modified glassy carbon electrode for selective voltammetric measurement of uric acid in urine sample.

    PubMed

    Aslanoglu, Mehmet; Kutluay, Aysegul; Abbasoglu, Sultan; Karabulut, Serpil

    2008-03-01

    A reliable and reproducible method for the determination of uric acid in urine samples has been developed. The method is based on the modification of a glassy carbon electrode by 3-acetylthiophene using cyclic voltammetry. The poly(3-acetylthiophene) modified glassy carbon electrode showed an excellent electrocatalytic effect towards the oxidation of uric acid in 0.1 m phosphate buffer solution (PBS) at pH 7.2. Compared with a bare glassy carbon electrode (GCE), an obvious shift of the oxidation peak potential in the cathodic direction and a marked enhancement of the anodic current response for uric acid were observed. The poly(3-acetylthiophene)/GCE was used for the determination of uric acid using square wave voltammetry. The peak current increased linearly with the concentration of uric acid in the range of 1.25 x 10(-5)-1.75 x 10(-4) M. The detection limit was 5.27 x 10(-7) M by square wave voltammetry. The poly(3-acetylthiophene)/GCE was also effective to determine uric acid and ascorbic acid in a mixture and resolved the overlapping anodic peaks of these two species into two well-defined voltammetric peaks in cyclic voltammetry at 0.030 V and 0.320 V (vs. Ag/AgCl) for ascorbic acid and uric acid, respectively. The modified electrode exhibited stable and sensitive current responses toward uric acid and ascorbic acid. The method has successfully been applied for determination of uric acid in urine samples.

  9. A hydrogen peroxide sensor based on Ag nanoparticles electrodeposited on natural nano-structure attapulgite modified glassy carbon electrode.

    PubMed

    Chen, Huihui; Zhang, Zhe; Cai, Dongqing; Zhang, Shengyi; Zhang, Bailin; Tang, Jilin; Wu, Zhengyan

    2011-10-30

    A novel strategy to fabricate hydrogen peroxide (H(2)O(2)) sensor was developed by electrodepositing Ag nanoparticles (NPs) on a glassy carbon electrode modified with natural nano-structure attapulgite (ATP). The result of electrochemical experiments showed that such constructed sensor had a favorable catalytic ability to reduce H(2)O(2). The good catalytic activity of the sensor was ascribed to the ATP that facilitated the formation and homogenous distribution of small Ag NPs. The resulted sensor achieved 95% of the steady-state current within 2s and had a 2.4 μM detection limit of H(2)O(2).

  10. A sensitive determination of estrogens with a Pt nano-clusters/multi-walled carbon nanotubes modified glassy carbon electrode.

    PubMed

    Lin, Xiangqin; Li, Yongxin

    2006-08-15

    On the top of a multi-walled carbon nanotubes (MWNTs) modified glassy carbon electrode (MWNTs/GCE), Pt nanoclusters were electrochemically deposited, fabricating a Pt/MWNTs composite modified electrode, Pt/MWNTs/GCE. X-ray photoelectron spectroscopy, powder X-ray diffraction and field emission scanning electron microscope were used for the surface characterization of the electrode, and demonstrated the formation and distribution of Pt clusters of Pt nanoparticles of 8.4 nm in averaged size in the MWNTs matrix. The preliminary study found that this composite modified electrode has strong electrocatalytic activity toward the oxidation of estrogens involving estradiol, estrone and estriol. The voltammetric behavior of estrogens on this electrode was investigated by cyclic voltammetry, linear sweep voltammetry and square-wave voltammetry. In comparison with the MWNTs/GCE or a Pt nanoparticles modified GCE prepared in the similar way, this composite modified electrode exhibited much higher current sensitivity and catalytic activity. This electrode is also stable. The linear range of square-wave voltammetric determination was 5.0 x 10(-7)-1.5 x 10(-5)mol/L for estradiol, 2.0 x 10(-6)-5.0 x 10(-5)mol/L for estrone, and 1.0 x 10(-6)-7.5 x 10(-5)mol/L for estriol. Under an assumption that the concentration ratio of estradiol:estrone:estriol is 2:2:1, the real sample of blood serums was tested for the determination using this electrode. Satisfactory result was obtained with averaged recovery of 105%.

  11. A 3D microfluidic chip for electrochemical detection of hydrolysed nucleic bases by a modified glassy carbon electrode.

    PubMed

    Vlachova, Jana; Tmejova, Katerina; Kopel, Pavel; Korabik, Maria; Zitka, Jan; Hynek, David; Kynicky, Jindrich; Adam, Vojtech; Kizek, Rene

    2015-01-22

    Modification of carbon materials, especially graphene-based materials, has wide applications in electrochemical detection such as electrochemical lab-on-chip devices. A glassy carbon electrode (GCE) modified with chemically alternated graphene oxide was used as a working electrode (glassy carbon modified by graphene oxide with sulphur containing compounds and Nafion) for detection of nucleobases in hydrolysed samples (HCl pH = 2.9, 100 °C, 1 h, neutralization by NaOH). It was found out that modification, especially with trithiocyanuric acid, increased the sensitivity of detection in comparison with pure GCE. All processes were finally implemented in a microfluidic chip formed with a 3D printer by fused deposition modelling technology. As a material for chip fabrication, acrylonitrile butadiene styrene was chosen because of its mechanical and chemical stability. The chip contained the one chamber for the hydrolysis of the nucleic acid and another for the electrochemical detection by the modified GCE. This chamber was fabricated to allow for replacement of the GCE.

  12. A 3D Microfluidic Chip for Electrochemical Detection of Hydrolysed Nucleic Bases by a Modified Glassy Carbon Electrode

    PubMed Central

    Vlachova, Jana; Tmejova, Katerina; Kopel, Pavel; Korabik, Maria; Zitka, Jan; Hynek, David; Kynicky, Jindrich; Adam, Vojtech; Kizek, Rene

    2015-01-01

    Modification of carbon materials, especially graphene-based materials, has wide applications in electrochemical detection such as electrochemical lab-on-chip devices. A glassy carbon electrode (GCE) modified with chemically alternated graphene oxide was used as a working electrode (glassy carbon modified by graphene oxide with sulphur containing compounds and Nafion) for detection of nucleobases in hydrolysed samples (HCl pH = 2.9, 100 °C, 1 h, neutralization by NaOH). It was found out that modification, especially with trithiocyanuric acid, increased the sensitivity of detection in comparison with pure GCE. All processes were finally implemented in a microfluidic chip formed with a 3D printer by fused deposition modelling technology. As a material for chip fabrication, acrylonitrile butadiene styrene was chosen because of its mechanical and chemical stability. The chip contained the one chamber for the hydrolysis of the nucleic acid and another for the electrochemical detection by the modified GCE. This chamber was fabricated to allow for replacement of the GCE. PMID:25621613

  13. Glassy carbons from poly(furfuryl alcohol) copolymers: structural studies by high-resolution solid-state NMR techniques

    SciTech Connect

    Eckert, H.; Levendis, Y.A.; Flagan, R.C.

    1988-08-25

    The chemical structure of glass carbon particles produced from poly(furfuryl alcohol) copolymers is studied by /sup 13/C cross-polarization/magic-angle spinning (CP-MAS) NMR and high-speed /sup 1/H MAS NMR. In agreement with earlier proposals, /sup 13/C NMR spectra confirm the buildup of a highly unsaturated system at the expense of furan rings and aliphatic carbon atoms, and upon heating to 800 K this conversion is essentially complete. Successive carbonization by air oxidation or pyrolysis at temperatures up to 1600 K is reflected in a gradual decrease of the /sup 13/C chemical shift from ca. 130 to 115 ppm versus tetramethylsilane. /sup 1/H MAS NMR is used to detect and quantitate the amount of residual C-bonded hydrogen species at various stages of the carbonization process. In addition, these spectra show intense, narrow resonances due to sorbed H/sub 2/O molecules, which resonate over a wide range of chemical shifts (between 2.5 and /minus/8 ppm versus tetramethylsilane). In analogy with effects observed by Tabony and co-workers for molecules adsorbed above the basal plane of graphite, the upfield shifts observed for water sorbed in the glassy carbons of the present study are attributed to the large susceptibility anisotropy of submicroscopically ordered, turbostratic, or partially graphitized regions of the samples. The extent of this ordering is inversely correlated with the absolute content of residual C-bonded hydrogen species and depends mainly on the temperature of pyrolysis, whereas the oxygen content of the heating atmosphere and the composition of the initial polymeric material appear to be of secondary importance. The results suggest that sorbed H/sub 2/O molecules can function as sensitive NMR chemical shift probes for the initial stages of crystallization processes in glassy carbons.

  14. Highly Stable Glassy Carbon Interfaces for Long-Term Neural Stimulation and Low-Noise Recording of Brain Activity

    PubMed Central

    Vomero, Maria; Castagnola, Elisa; Ciarpella, Francesca; Maggiolini, Emma; Goshi, Noah; Zucchini, Elena; Carli, Stefano; Fadiga, Luciano; Kassegne, Sam; Ricci, Davide

    2017-01-01

    We report on the superior electrochemical properties, in-vivo performance and long term stability under electrical stimulation of a new electrode material fabricated from lithographically patterned glassy carbon. For a direct comparison with conventional metal electrodes, similar ultra-flexible, micro-electrocorticography (μ-ECoG) arrays with platinum (Pt) or glassy carbon (GC) electrodes were manufactured. The GC microelectrodes have more than 70% wider electrochemical window and 70% higher CTC (charge transfer capacity) than Pt microelectrodes of similar geometry. Moreover, we demonstrate that the GC microelectrodes can withstand at least 5 million pulses at 0.45 mC/cm2 charge density with less than 7.5% impedance change, while the Pt microelectrodes delaminated after 1 million pulses. Additionally, poly(3,4-ethylenedioxythiophene)-poly(styrenesulfonate) (PEDOT-PSS) was selectively electrodeposited on both sets of devices to specifically reduce their impedances for smaller diameters (<60 μm). We observed that PEDOT-PSS adhered significantly better to GC than Pt, and allowed drastic reduction of electrode size while maintaining same amount of delivered current. The electrode arrays biocompatibility was demonstrated through in-vitro cell viability experiments, while acute in vivo characterization was performed in rats and showed that GC microelectrode arrays recorded somatosensory evoked potentials (SEP) with an almost twice SNR (signal-to-noise ratio) when compared to the Pt ones. PMID:28084398

  15. Electroanalytical investigation and determination of pefloxacin in pharmaceuticals and serum at boron-doped diamond and glassy carbon electrodes.

    PubMed

    Uslu, Bengi; Topal, Burcu Dogan; Ozkan, Sibel A

    2008-02-15

    The anodic behavior and determination of pefloxacin on boron-doped diamond and glassy carbon electrodes were investigated using cyclic, linear sweep, differential pulse and square wave voltammetric techniques. In cyclic voltammetry, pefloxacin shows one main irreversible oxidation peak and additional one irreversible ill-defined wave depending on pH values for both electrodes. The results indicate that the process of pefloxacin is irreversible and diffusion controlled on boron-doped diamond electrode and irreversible but adsorption controlled on glassy carbon electrode. The peak current is found to be linear over the range of concentration 2x10(-6) to 2x10(-4)M in 0.5M H(2)SO(4) at about +1.20V (versus Ag/AgCl) for differential pulse and square wave voltammetric technique using boron-doped diamond electrode. The repeatability, reproducibility, precision and accuracy of the methods in all media were investigated. Selectivity, precision and accuracy of the developed methods were also checked by recovery studies. The procedures were successfully applied to the determination of the drug in pharmaceutical dosage forms and humans serum samples with good recovery results. No electroactive interferences from the excipients and endogenous substances were found in the pharmaceutical dosage forms and biological samples, respectively.

  16. Highly Stable Glassy Carbon Interfaces for Long-Term Neural Stimulation and Low-Noise Recording of Brain Activity

    NASA Astrophysics Data System (ADS)

    Vomero, Maria; Castagnola, Elisa; Ciarpella, Francesca; Maggiolini, Emma; Goshi, Noah; Zucchini, Elena; Carli, Stefano; Fadiga, Luciano; Kassegne, Sam; Ricci, Davide

    2017-01-01

    We report on the superior electrochemical properties, in-vivo performance and long term stability under electrical stimulation of a new electrode material fabricated from lithographically patterned glassy carbon. For a direct comparison with conventional metal electrodes, similar ultra-flexible, micro-electrocorticography (μ-ECoG) arrays with platinum (Pt) or glassy carbon (GC) electrodes were manufactured. The GC microelectrodes have more than 70% wider electrochemical window and 70% higher CTC (charge transfer capacity) than Pt microelectrodes of similar geometry. Moreover, we demonstrate that the GC microelectrodes can withstand at least 5 million pulses at 0.45 mC/cm2 charge density with less than 7.5% impedance change, while the Pt microelectrodes delaminated after 1 million pulses. Additionally, poly(3,4-ethylenedioxythiophene)-poly(styrenesulfonate) (PEDOT-PSS) was selectively electrodeposited on both sets of devices to specifically reduce their impedances for smaller diameters (<60 μm). We observed that PEDOT-PSS adhered significantly better to GC than Pt, and allowed drastic reduction of electrode size while maintaining same amount of delivered current. The electrode arrays biocompatibility was demonstrated through in-vitro cell viability experiments, while acute in vivo characterization was performed in rats and showed that GC microelectrode arrays recorded somatosensory evoked potentials (SEP) with an almost twice SNR (signal-to-noise ratio) when compared to the Pt ones.

  17. An Easily Fabricated Electrochemical Sensor Based on a Graphene-Modified Glassy Carbon Electrode for Determination of Octopamine and Tyramine.

    PubMed

    Zhang, Yang; Zhang, Meiqin; Wei, Qianhui; Gao, Yongjie; Guo, Lijuan; Al-Ghanim, Khalid A; Mahboob, Shahid; Zhang, Xueji

    2016-04-13

    A simple electrochemical sensor has been developed for highly sensitive detection of octopamine and tyramine by electrodepositing reduced graphene oxide (ERGO) nanosheets onto the surface of a glassy carbon electrode (GCE). The electrocatalytic oxidation of octopamine and tyramine is individually investigated at the surface of the ERGO modified glassy carbon electrode (ERGO/GCE) by using cyclic voltammetry (CV) and differential pulse voltammetry (DPV). Several essential factors including the deposition cycle of reduced graphene oxide nanosheets and the pH of the running buffer were investigated in order to determine the optimum conditions. Furthermore, the sensor was applied to the quantification of octopamine and tyramine by DPV in the concentration ranges from 0.5 to 40 μM and 0.1 to 25 μM, respectively. In addition, the limits of detection of octopamine and tyramine were calculated to be 0.1 μM and 0.03 μM (S/N = 3), respectively. The sensor showed good reproducibility, selectivity and stability. Finally, the sensor successfully detected octopamine and tyramine in commercially available beer with satisfactory recovery ranges which were 98.5%-104.7% and 102.2%-103.1%, respectively. These results indicate the ERGO/GCE based sensor is suitable for the detection of octopamine and tyramine.

  18. An Easily Fabricated Electrochemical Sensor Based on a Graphene-Modified Glassy Carbon Electrode for Determination of Octopamine and Tyramine

    PubMed Central

    Zhang, Yang; Zhang, Meiqin; Wei, Qianhui; Gao, Yongjie; Guo, Lijuan; Al-Ghanim, Khalid A.; Mahboob, Shahid; Zhang, Xueji

    2016-01-01

    A simple electrochemical sensor has been developed for highly sensitive detection of octopamine and tyramine by electrodepositing reduced graphene oxide (ERGO) nanosheets onto the surface of a glassy carbon electrode (GCE). The electrocatalytic oxidation of octopamine and tyramine is individually investigated at the surface of the ERGO modified glassy carbon electrode (ERGO/GCE) by using cyclic voltammetry (CV) and differential pulse voltammetry (DPV). Several essential factors including the deposition cycle of reduced graphene oxide nanosheets and the pH of the running buffer were investigated in order to determine the optimum conditions. Furthermore, the sensor was applied to the quantification of octopamine and tyramine by DPV in the concentration ranges from 0.5 to 40 μM and 0.1 to 25 μM, respectively. In addition, the limits of detection of octopamine and tyramine were calculated to be 0.1 μM and 0.03 μM (S/N = 3), respectively. The sensor showed good reproducibility, selectivity and stability. Finally, the sensor successfully detected octopamine and tyramine in commercially available beer with satisfactory recovery ranges which were 98.5%–104.7% and 102.2%–103.1%, respectively. These results indicate the ERGO/GCE based sensor is suitable for the detection of octopamine and tyramine. PMID:27089341

  19. Highly Stable Glassy Carbon Interfaces for Long-Term Neural Stimulation and Low-Noise Recording of Brain Activity.

    PubMed

    Vomero, Maria; Castagnola, Elisa; Ciarpella, Francesca; Maggiolini, Emma; Goshi, Noah; Zucchini, Elena; Carli, Stefano; Fadiga, Luciano; Kassegne, Sam; Ricci, Davide

    2017-01-13

    We report on the superior electrochemical properties, in-vivo performance and long term stability under electrical stimulation of a new electrode material fabricated from lithographically patterned glassy carbon. For a direct comparison with conventional metal electrodes, similar ultra-flexible, micro-electrocorticography (μ-ECoG) arrays with platinum (Pt) or glassy carbon (GC) electrodes were manufactured. The GC microelectrodes have more than 70% wider electrochemical window and 70% higher CTC (charge transfer capacity) than Pt microelectrodes of similar geometry. Moreover, we demonstrate that the GC microelectrodes can withstand at least 5 million pulses at 0.45 mC/cm(2) charge density with less than 7.5% impedance change, while the Pt microelectrodes delaminated after 1 million pulses. Additionally, poly(3,4-ethylenedioxythiophene)-poly(styrenesulfonate) (PEDOT-PSS) was selectively electrodeposited on both sets of devices to specifically reduce their impedances for smaller diameters (<60 μm). We observed that PEDOT-PSS adhered significantly better to GC than Pt, and allowed drastic reduction of electrode size while maintaining same amount of delivered current. The electrode arrays biocompatibility was demonstrated through in-vitro cell viability experiments, while acute in vivo characterization was performed in rats and showed that GC microelectrode arrays recorded somatosensory evoked potentials (SEP) with an almost twice SNR (signal-to-noise ratio) when compared to the Pt ones.

  20. Bactericidal properties of silver implanted pyrolytic carbon

    NASA Astrophysics Data System (ADS)

    Zhao, J.; Feng, H. J.; Tang, H. Q.; Zheng, J. H.

    2006-02-01

    The bactericidal properties of Ag +-implanted pyrolytic carbon was investigated using gram positive staphylococcus aureus. The pyrolytic carbon samples were implanted by silver ions with the dose ranging from 5 × 10 14 to 5 × 10 18 ions/cm 2 at the energy of 70 keV. The samples were characterized by X-ray diffraction (XRD), Rutherford backscatterring spectrum (RBS) and scanning electron microscopy (SEM). The results show that the bactericidal ratio increases with the ion dose when silver ion dose under the saturated dose of 5 × 10 17 ions/cm 2. The bactericidal ratio is over 97% when the ion dose exceeds that. RBS analysis shows that the silver atoms penetrate into the sample surface and forms a Gaussian-like distribution in pyrolytic carbon substrate. The sputtering effect is helpful to form a silver-rich surface region which plays an important role to kill bacteria. XRD analysis shows that silver mainly existed in (1 1 1), (2 0 0), (3 1 1) crystal plane in accordance with the fcc crystal structure. SEM characterization shows that the surface morphology also important for killing germs.

  1. Carbon nanotube detectors for microchip CE: comparative study of single-wall and multiwall carbon nanotube, and graphite powder films on glassy carbon, gold, and platinum electrode surfaces.

    PubMed

    Pumera, Martin; Merkoçi, Arben; Alegret, Salvador

    2007-04-01

    The performance of microchip electrophoresis/electrochemistry system with carbon nanotube (CNT) film electrodes was studied. Electrocatalytic activities of different carbon materials (single-wall CNT (SWCNT), multiwall CNT (MWCNT), carbon powder) cast on different electrode substrates (glassy carbon (GC), gold, and platinum) were compared in a microfluidic setup and their performance as microchip electrochemical detectors was assessed. An MWCNT film on a GC electrode shows electrocatalytic effect toward oxidation of dopamine (E(1/2) shift of 0.09 V) and catechol (E(1/2) shift of 0.19 V) when compared to a bare GC electrode, while other CNT/carbon powder films on the GC electrode display negligible effects. Modification of a gold electrode by graphite powder results in a strong electrocatalytic effect toward oxidation of dopamine and catechol (E(1/2) shift of 0.14 and 0.11 V, respectively). A significant shift of the half-wave potentials to lower values also provide the MWCNT film (E(1/2) shift of 0.08 and 0.08 V for dopamine and catechol, respectively) and the SWCNT film (E(1/2) shift of 0.10 V for catechol) when compared to a bare gold electrode. A microfluidic device with a CNT film-modified detection electrode displays greatly improved separation resolution (R(s)) by a factor of two compared to a bare electrode, reflecting the electrocatalytic activity of CNT.

  2. Fabrication of Graphene Using Carbon Ion Implantation

    NASA Astrophysics Data System (ADS)

    Colon, Tomeka; Smith, Cydale; Muntele, Claudiu

    2012-02-01

    Graphene is a flat monolayer of carbon atoms tightly packed into a two-dimensional (2D) honeycomb lattice and is a basic building block for graphitic materials of all other dimensionalities. It can be wrapped up into 0D fullerenes, rolled into 1D nanotubes, or stacked into 3D graphite. Graphene's high electrical conductivity and high optical transparency make it a candidate for transparent conducting electrodes, required for such applications as touchscreens, liquid crystal displays, organic photovoltaic cells, and organic light-emitting diodes. In particular, graphene's mechanical strength and flexibility are advantageous compared to indium tin oxide, which is brittle, and graphene films may be deposited from solution over large areas. One method to grow epitaxial graphene is by starting with single crystal silicon carbide (SiC). When SiC is heated under certain conditions, silicon evaporates leaving behind carbon that reorganizes into layers of graphene. Here we report on an alternate method of producing graphene by using low energy carbon implantation in a nickel layer deposited on silicon dioxide mechanical support, followed by heat treatment in a reducing atmosphere to induce carbon migration and self-assembly. We used high resolution RBS and Raman spectroscopy for process and sample characterization. Details will be discussed during the meeting.

  3. Covalent attachment of diphosphine ligands to glassy carbon electrodes via Cu-catalyzed alkyne-azide cycloaddition. Metallation with Ni( ii )

    SciTech Connect

    Das, Atanu K.; Engelhard, Mark H.; Lense, Sheri; Roberts, John A. S.; Bullock, R. Morris

    2015-01-01

    Covalent tethering of a P2N2ligand to a planar, azide-terminated glassy carbon electrode surface was accomplished using a CuI-catalyzed “click” reaction, followed by metallation with NiII.

  4. Photogeneration of singlet oxygen by the phenothiazine derivatives covalently bound to the surface-modified glassy carbon

    NASA Astrophysics Data System (ADS)

    Blacha-Grzechnik, Agata; Piwowar, Katarzyna; Krukiewicz, Katarzyna; Koscielniak, Piotr; Szuber, Jacek; Zak, Jerzy K.

    2016-05-01

    The selected group of four amine-derivatives of phenothiazine was covalently grafted to the glassy carbon surface in the four-step procedure consisting of the electrochemical reduction of the diazonium salt followed by the electrochemical and chemical post-modification steps. The proposed strategy involves the bonding of linker molecule to which the photosensitizer is attached. The synthesized organic layers were characterized by means of cyclic voltammetry, XPS and Raman Spectroscopy. It was shown that the phenothiazines immobilized via proposed strategy retain their photochemical properties and are able to generate 1O2 when activated by the laser radiation. The effectiveness of in situ singlet oxygen generation by those new solid photoactive materials was determined by means of UVVis spectroscopy. The reported, covalently modified solid surfaces may find their application as the singlet oxygen photogenerators in the fine chemicals' synthesis or in the wastewater treatment.

  5. Novel Signal-Amplified Fenitrothion Electrochemical Assay, Based on Glassy Carbon Electrode Modified with Dispersed Graphene Oxide

    PubMed Central

    Wang, Limin; Dong, Jinbo; Wang, Yulong; Cheng, Qi; Yang, Mingming; Cai, Jia; Liu, Fengquan

    2016-01-01

    A novel signal-amplified electrochemical assay for the determination of fenitrothion was developed, based on the redox behaviour of organophosphorus pesticides on a glassy carbon working electrode. The electrode was modified using graphene oxide dispersion. The electrochemical response of fenitrothion at the modified electrode was investigated using cyclic voltammetry, current-time curves, and square-wave voltammetry. Experimental parameters, namely the accumulation conditions, pH value, and volume of dispersed material, were optimised. Under the optimum conditions, a good linear relationship was obtained between the oxidation peak current and the fenitrothion concentration. The linear range was 1–400 ng·mL−1, with a detection limit of 0.1 ng·mL−1 (signal-to-nose ratio = 3). The high sensitivity of the sensor was demonstrated by determining fenitrothion in pakchoi samples. PMID:27003798

  6. Glucose oxidase/colloidal gold nanoparticles immobilized in Nafion film on glassy carbon electrode: Direct electron transfer and electrocatalysis.

    PubMed

    Zhao, Shuang; Zhang, Kai; Bai, Yu; Yang, Weiwei; Sun, Changqing

    2006-10-01

    The direct electron transfer of glucose oxidase (GOD) was achieved based on the immobilization of GOD/colloidal gold nanoparticles on a glassy carbon electrode by a Nafion film. The immobilized GOD displayed a pair of well-defined and nearly reversible redox peaks with a formal potential (Eo ') of -0.434 V in 0.1 M pH 7.0 phosphate buffer solution and the response showed a surface-controlled electrode process. The dependence of Eo ' on solution pH indicated that the direct electron transfer reaction of GOD was a two-electron-transfer coupled with a two-proton-transfer reaction process. The experimental results also demonstrated that the immobilized GOD retained its electrocatalytic activity for the oxidation of glucose. So the resulting modified electrode can be used as a biosensor for detecting glucose.

  7. Differential pulse voltammetric determination of nanomolar concentrations of antiviral drug acyclovir at polymer film modified glassy carbon electrode.

    PubMed

    Dorraji, Parisa S; Jalali, Fahimeh

    2016-04-01

    An electrochemical sensor for the sensitive detection of acyclovir was developed by the electropolymerization of Eriochrome black T at a pretreated glassy carbon electrode. The surface morphology of the modified electrode was characterized by field emission scanning electron microscopy. Under the optimized conditions, a significant electrochemical improvement was observed toward the electrooxidation of acyclovir on the modified electrode surface relative to the unmodified electrode. The detection limit of 12 nM and two linear calibration ranges of 0.03-0.3 μM and 0.3-1.5 μM were obtained for acyclovir determination using a differential pulse voltammetric method in acetate buffer (0.1 M, pH 4.0). Real sample studies were carried out in human blood serum and pharmaceutical formulations, which offered good recovery (98-102%). The electrode showed excellent reproducibility, selectivity and antifouling effects.

  8. Examination of performance of glassy carbon paste electrode modified with gold nanoparticle and xanthine oxidase for xanthine and hypoxanthine detection.

    PubMed

    Cubukçu, Meliha; Timur, Suna; Anik, Ulkü

    2007-12-15

    A composite electrode was prepared by modifying glassy carbon microparticles with gold nanoparticles (Au-nps) and xanthine oxidase enzyme (XOD) for xanthine (X) and hypoxanthine (Hx) detection. After the optimization of the system for X, the biosensor was characterized for X and Hx. A linearity was obtained in the concentration range between 5.00 x 10(-7) and 1.00 x 10(-5) M for X with equation of y=0.24 x + 0.712 and 5.00 x 10(-6) to 1.50 x 10(-4) M for Hx, with equation of y = 0.014 x + 0.575, respectively. Obtained results were compared to X and/or Hx biosensors including/not including Au-np in the structure. The developed system was also applied for detection of Hx in canned tuna fish sample and very promising results were obtained.

  9. A highly sensitive hydrogen peroxide sensor based on (Ag-Au NPs)/poly[o-phenylenediamine] modified glassy carbon electrode.

    PubMed

    Shamsipur, Mojtaba; Karimi, Ziba; Amouzadeh Tabrizi, Mahmoud

    2015-11-01

    Herein, the poly(o-phenylenediamine) decorated with gold-silver nanoparticle (Ag-Au NPs) nanocomposite modified glassy carbon was used for the determination of hydrogen peroxide. Electrochemical experiments indicated that the proposed sensor possesses an excellent sensitivity toward the reduction of hydrogen peroxide. The resulting sensor exhibited a good response to hydrogen peroxide over linear range from 0.2 to 60.0μM with a limit of detection of 0.08μM, good reproducibility, long-term stability and negligible interference from ascorbic acid, uric acid and dopamine. The proposed sensor was successfully applied to the determination of hydrogen peroxide in human serum sample. Copyright © 2015 Elsevier B.V. All rights reserved.

  10. Electrocatalytic oxidation of hydrazine and hydroxylamine by graphene oxide-Pd nanoparticle-modified glassy carbon electrode.

    PubMed

    Lee, Eunhee; Kim, Daekun; You, Jung-Min; Kim, Seul Ki; Yun, Mira; Jeon, Seungwon

    2012-12-01

    Pd nanoparticle catalysts supported by thiolated graphene oxide (tGO) on a glassy carbon electrode (GCE), and denoted as tGO-Pd/GCE, are used in this study for the electrochemical determination of hydroxylamine and hydrazine. The physicochemical properties of tGO-Pd were characterized by transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS) and electrochemical impedance spectroscopy (EIS). They showed strong catalytic activity toward the oxidation of hydroxylamine and hydrazine. Cyclic voltammetry (CV) and amperometry were used to characterize the sensors' performances. The detection limits of hydroxylamine and hydrazine by tGO-Pd/GCE were 0.31 and 0.25 microM (s/n = 3), respectively. The sensors' sensitivity, selectivity, and stability were also investigated.

  11. Interfacial electron transfer of glucose oxidase on poly(glutamic acid)-modified glassy carbon electrode and glucose sensing.

    PubMed

    Zhou, Xuechou; Tan, Bingcan; Zheng, Xinyu; Kong, Dexian; Li, Qinglu

    2015-11-15

    The interfacial electron transfer of glucose oxidase (GOx) on a poly(glutamic acid)-modified glassy carbon electrode (PGA/GCE) was investigated. The redox peaks measured for GOx and flavin adenine dinucleotide (FAD) are similar, and the anodic peak of GOx does not increase in the presence of glucose in a mediator-free solution. These indicate that the electroactivity of GOx is not the direct electron transfer (DET) between GOx and PGA/GCE and that the observed electroactivity of GOx is ascribed to free FAD that is released from GOx. However, efficient electron transfer occurred if an appropriate mediator was placed in solution, suggesting that GOx is active. The PGA/GCE-based biosensor showed wide linear response in the range of 0.5-5.5 mM with a low detection limit of 0.12 mM and high sensitivity and selectivity for measuring glucose.

  12. Enhancement of electrogenerated chemiluminescence of luminol by ascorbic acid at gold nanoparticle/graphene modified glassy carbon electrode.

    PubMed

    Dong, Yongping; Gao, Tingting; Zhou, Ying; Chu, Xiangfeng; Wang, Chengming

    2015-01-05

    Gold nanoparticle/graphene (GNP/GR) nanocomposite was one-pot synthesized from water soluble graphene and HAuCl₄ by hydrothermal method and characterized by TEM, Raman spectroscopy, XRD, XPS, UV-vis spectroscopy, and electrochemical impedance spectroscopy (EIS). Electrogenerated chemiluminescence (ECL) of luminol was investigated at the GNP/GR modified glassy carbon electrode (GNP/GR/GCE) and the GNP modified glassy carbon electrode (GNP/GCE) in aqueous solution respectively. The results revealed that one strong anodic ECL peak could be observed at ∼0.8 V at two modified electrodes compared with that at the bare electrode. The intensity of the anodic ECL at the GNP/GR/GCE is weaker than that at the GNP/GCE, which should be due to the synergic effect of the enhancing effect of gold nanoparticles and the inhibiting effect of graphene on anodic luminol ECL. One strong cathodic ECL peak located at ∼-0.8 V could be observed at the GNP/GR/GCE but not at the GNP/GCE, which should be result from the adsorbed oxygen at the graphene film. In the presence of ascorbic acid, the anodic ECL at the GNP/GR/GCE was enhanced more than 8-times, which is more apparent than that at the GNP/GCE. Whereas, the cathodic ECL peak was seriously inhibited at the GNP/GR/GCE. The enhanced ECL intensity at the GNP/GR/GCE varied linearly with the logarithm of ascorbic acid concentration in the range of 1.0 × 10(-8) to 1.0 × 10(-6)mol L(-1) with a detection limit of 1.0 × 10(-9) mol L(-1). The possible ECL mechanism was also discussed. Copyright © 2014 Elsevier B.V. All rights reserved.

  13. Enhancement of electrogenerated chemiluminescence of luminol by ascorbic acid at gold nanoparticle/graphene modified glassy carbon electrode

    NASA Astrophysics Data System (ADS)

    Dong, Yongping; Gao, Tingting; Zhou, Ying; Chu, Xiangfeng; Wang, Chengming

    2015-01-01

    Gold nanoparticle/graphene (GNP/GR) nanocomposite was one-pot synthesized from water soluble graphene and HAuCl4 by hydrothermal method and characterized by TEM, Raman spectroscopy, XRD, XPS, UV-vis spectroscopy, and electrochemical impedance spectroscopy (EIS). Electrogenerated chemiluminescence (ECL) of luminol was investigated at the GNP/GR modified glassy carbon electrode (GNP/GR/GCE) and the GNP modified glassy carbon electrode (GNP/GCE) in aqueous solution respectively. The results revealed that one strong anodic ECL peak could be observed at ∼0.8 V at two modified electrodes compared with that at the bare electrode. The intensity of the anodic ECL at the GNP/GR/GCE is weaker than that at the GNP/GCE, which should be due to the synergic effect of the enhancing effect of gold nanoparticles and the inhibiting effect of graphene on anodic luminol ECL. One strong cathodic ECL peak located at ∼-0.8 V could be observed at the GNP/GR/GCE but not at the GNP/GCE, which should be result from the adsorbed oxygen at the graphene film. In the presence of ascorbic acid, the anodic ECL at the GNP/GR/GCE was enhanced more than 8-times, which is more apparent than that at the GNP/GCE. Whereas, the cathodic ECL peak was seriously inhibited at the GNP/GR/GCE. The enhanced ECL intensity at the GNP/GR/GCE varied linearly with the logarithm of ascorbic acid concentration in the range of 1.0 × 10-8 to 1.0 × 10-6 mol L-1 with a detection limit of 1.0 × 10-9 mol L-1. The possible ECL mechanism was also discussed.

  14. Highly selective determination of dopamine in the presence of ascorbic acid and serotonin at glassy carbon electrodes modified with carbon nanotubes dispersed in polyethylenimine.

    PubMed

    Rodríguez, Marcela C; Rubianes, María D; Rivas, Gustavo A

    2008-11-01

    We report the highly selective and sensitive voltammetric dopamine quantification in the presence of ascorbic acid and serotonin by using glassy carbon electrodes modified with a dispersion of multi-wall carbon nanotubes (MWCNT) in polyethylenimine, PEI (GCE/MWCNT-PEI). The electrocatalytic activity of the MWCNT deposited on the glassy carbon electrode has allowed an important decrease in the overvoltages for the oxidation of ascorbic acid and dopamine, making possible a clear definition of dopamine, serotonin and ascorbic acid oxidation processes. The sensitivities for dopamine in the presence and absence of 1.0 mM ascorbic acid and serotonin were (2.18 +/- 0.03) x 10(5) microAM(-1) (r = 0.9998); and (2.10 +/- 0.07) x 10(5) miroAM(-1) (r=0.9985), respectively, demonstrating the excellent performance of the GCE/MWCNT-PEI. The detection limit for dopamine in the mixture was 9.2 x 10(-7) M. The R. S. D. for the determination of 50 microM dopamine using four different electrodes was 3.9% when modified with the same MWCNT/PEI dispersion, and 4.6% when using four different dispersions. The modified electrode has been successfully applied for recovery assays of dopamine in human blood serum. Therefore, the new sensor represents an interesting and promising alternative for the electrochemical quantification of neurotransmitters and other analytes of clinical interest.

  15. Simultaneous voltammetric determination of enrofloxacin and ciprofloxacin in urine and plasma using multiwall carbon nanotubes modified glassy carbon electrode by least-squares support vector machines.

    PubMed

    Ensafi, Ali A; Taei, M; Khayamian, T; Hasanpour, F

    2010-01-01

    A simple and sensitive method is proposed for the electrochemical determination of enrofloxacin (ENRO) and its primary metabolite ciprofloxacin (CIPRO) at a multiwall carbon nanotubes/glassy carbon electrode (MWCNT/GCE) using a least-squares support vector machine (LS-SVM) and linear sweep voltammetry. Simultaneous determination of ENRO and CIPRO at bare glassy carbon is associated with certain difficulties due to voltammogram overlapping and their low sensitivity. The resolution of the mixture was carried out using LS-SVM as a multivariate calibration method. Under the optimum conditions at pH 7.0, the linear sweep currents increased linearly with ENRO and CIPRO concentrations in ranges of 2.0-780.0 micromol L(-1) (0.7-280.3 microg mL(-1)) and 3.0-1200 micromol L(-1) (1.0-397.7 microg mL(-1)), respectively. The detection limits for ENRO and CIPRO were 0.5 and 0.9 micromol L(-1), respectively. The proposed method was applied to simultaneously determine both compounds in human urine, plasma and in pharmaceutical samples.

  16. Electrochemical behavior of o-sec-butylphenol at glassy carbon electrode modified with multiwalled carbon nanotubes and 1-butyl-3-methylimidazolium hexafluorophosphate.

    PubMed

    Zheng, Shaohua; Huang, Ying; Chen, Guonan

    2012-09-21

    A sensitive electrochemical sensor based on immobilized multiwalled carbon nanotubes (MWCNTs) and 1-butyl-3-methylimidazolium hexafluorophosphate (BMIM·PF(6)) on a glassy carbon electrode (GCE) for o-sec-butylphenol (osBP) was proposed. The electro-oxidation behavior was studied, the experimental conditions were optimized and kinetic parameters were calculated. The results indicated that this electrochemical sensor has the advantages of fast electron-transfer rate, minimal fouling of electrodes, high sensitivity and stability for o-sec-butylphenol. Upon comparison with a glassy carbon electrode, this senor would effectively minimize the over-potential and increase the electrochemical response to o-sec-butylphenol. Under the optimum conditions, the peak current was linear to the osBP concentration range from 1 × 10(-7) to 2.5 × 10(-5) M with the detection limit of 8.65 × 10(-9) M (S/N = 3). The proposed method was applied to the determination of spiked water samples with satisfactory results.

  17. Determination of mutagenic amines in water and food samples by high pressure liquid chromatography with amperometric detection using a multiwall carbon nanotubes-glassy carbon electrode.

    PubMed

    Bueno, Ana María; Marín, Miguel Ángel; Contento, Ana María; Ríos, Ángel

    2016-02-01

    A chromatographic method, using amperometric detection, for the sensitive determination of six representative mutagenic amines was developed. A glassy carbon electrode (GCE), modified with multiwall carbon nanotubes (GCE-CNTs), was prepared and its response compared to a conventional glassy carbon electrode. The chromatographic method (HPLC-GCE-CNTs) allowed the separation and the determination of heterocyclic aromatic amines (HAAs) classified as mutagenic amines by the International Agency for Research of Cancer. The new electrode was systematically studied in terms of stability, sensitivity, and reproducibility. Statistical analysis of the obtained data demonstrated that the modified electrode provided better sensitivity than the conventional unmodified ones. Detection limits were in the 3.0 and 7.5 ng/mL range, whereas quantification limits ranged between 9.5 and 25.0 ng/mL were obtained. The applicability of the method was demonstrated by the determination of the amines in several types of samples (water and food samples). Recoveries indicate very good agreement between amounts added and those found for all HAAs (recoveries in the 92% and 105% range).

  18. Electroanalysis using macro-, micro-, and nanochemical architectures on electrode surfaces. Bulk surface modification of glassy carbon microspheres with gold nanoparticles and their electrical wiring using carbon nanotubes.

    PubMed

    Dai, Xuan; Wildgoose, Gregory G; Salter, Chris; Crossley, Alison; Compton, Richard G

    2006-09-01

    Gold nanoparticles (approximately 30-60 nm in diameter) were deposited onto the surface of glassy carbon microspheres (10-20 microm) through electroless plating to produce bulk (i.e., gram) quantities of nanoparticle surface-modified microspheres. The gold nanoparticle-modified powder was then characterized by means of scanning electron microscopy and cyclic voltammetry. The voltammetric response of a macroelectrode consisting of a film of gold nanoparticle-modified glassy carbon microspheres, bound together and "wired-up" using multiwalled carbon nanotubes (MWCNTs), was investigated. We demonstrate that by intelligently exploiting both nano- and microchemical architectures and wiring up the electroactive centers using MWCNTs in this way, we can obtain macroelectrode voltammetric behavior while only using approximately 1% by mass of the expensive gold material that would be required to construct the equivalent gold film macrodisk electrode. The potential utility of electrodes constructed using chemical architectures such as this was demonstrated by applying them to the analytical determination of arsenic(III) concentration. An optimized limit of detection of 2.5 ppb was obtained.

  19. New biosensing platforms based on the layer-by-layer self-assembling of polyelectrolytes on Nafion/carbon nanotubes-coated glassy carbon electrodes.

    PubMed

    Rivas, Gustavo A; Miscoria, Silvia A; Desbrieres, Jacques; Barrera, Gustavo D

    2007-01-15

    We are proposing for the first time the use of a Nafion/multi-walled carbon nanotubes dispersion deposited on glassy carbon electrodes (GCE) as a new platform for developing enzymatic biosensors based on the self-assembling of a chitosan derivative and different oxidases. The electrodes are obtained by deposition of a layer of Nafion/multi-wall carbon nanotubes dispersion on glassy carbon electrodes, followed by the adsorption of a chitosan derivative as polycation and glucose oxidase, l-aminoacid oxidase or polyphenol oxidase, as polyanions and biorecognition elements. The optimum configuration for glucose biosensors has allowed a highly sensitive (sensitivity=(0.28+/-0.02)muAmM(-1), r=0.997), fast (4s in reaching the maximum response), and highly selective (0% interference of ascorbic acid and uric acid at maximum physiological levels) glucose quantification at 0.700V with detection and quantification limits of 0.035 and 0.107mM, respectively. The repetitivity for 10 measurements was 5.5%, while the reproducibility was 8.4% for eight electrodes. The potentiality of the new platform was clearly demonstrated by using the carbon nanotubes/Nafion layer as a platform for the self-assembling of l-aminoacid oxidase and polyphenol oxidase. Therefore, the platform we are proposing here, that combines the advantages of nanostructured materials with those of the layer-by-layer self-assembling of polyelectrolytes, opens the doors to new and exciting possibilities for the development of enzymatic and affinity biosensors using different transdution modes.

  20. A kanamycin sensor based on an electrosynthesized molecularly imprinted poly-o-phenylenediamine film on a single-walled carbon nanohorn modified glassy carbon electrode.

    PubMed

    Han, Shuang; Li, Bingqian; Song, Ze; Pan, Sihao; Zhang, Zhichao; Yao, Hui; Zhu, Shuyun; Xu, Guobao

    2016-12-19

    A single-walled carbon nanohorn (SWCNH) has been used to construct a molecularly imprinted electrochemical sensor for the first time. Kanamycin, a widely used aminoglycoside antibiotic, is used as a representative analyte to test the detection strategy. The kanamycin sensor was constructed by the electropolymerization of a molecularly imprinted poly-o-phenylenediamine film on a SWCNH modified glassy carbon electrode. The sensor was investigated in the presence or absence of kanamycin by cyclic voltammetry to verify the changes in the redox peak currents of K3Fe(CN)6. The sensor exhibits a linear range of 0.1-50 μM with a detection limit of 0.1 μM. It also shows high recognition ability, indicating that the SWCNH-based molecularly imprinted sensor is promising.

  1. An electrochemical sensor for detection of laccase activities from Penicillium simplicissimum in compost based on carbon nanotubes modified glassy carbon electrode.

    PubMed

    Liu, Jian-Xiao; Zhou, Wen-Jing; Gong, Ji-Lai; Tang, Lin; Zhang, Yi; Yu, Hong-Yan; Wang, Bin; Xu, Xiang-Min; Zeng, Guang-Ming

    2008-12-01

    An electrochemical sensor for detection of the activity of laccase from Penicillium simplicissimum isolated from the composting has been developed. The sensor is based on glassy carbon electrode modified with multi-wall carbon nanotubes (CNTs). The introduction of CNTs into this system can greatly enhance the electrochemical signal in this assay more sensitively, selectively and rapidly than that in conventional spectrophotometric assays. It was found that the optimal pH value of the electrolyte was 5.6. The results showed a good linear correlation between the current and the concentration of laccase activities measured by spectrophotometry, where the current slope was measured by chronoamperometry with a coefficient of 0.9835. Therefore, this electrochemical sensor can be used for rapid detection of laccase activity from P. simplicissimum. Furthermore, it may be potentially used for rapid quantification of P. simplicissimum according to the relationship between the laccase activities and the biomass.

  2. Determination of tryptophan and kynurenine in human plasma by liquid chromatography-electrochemical detection with multi-wall carbon nanotube-modified glassy carbon electrode.

    PubMed

    Liu, Lihong; Chen, Ying; Zhang, Yulin; Wang, Fang; Chen, Zilin

    2011-08-01

    A novel method was developed for the simultaneous determination of kynurenine and tryptophan by high-performance liquid chromatography with electrochemical detection at multi-wall carbon nanotube (MWCNT)-modified glassy carbon electrode. The separation and detection conditions were optimized. The typical HPLC experiments were conducted by using a reversed-phase ODS column with a mobile phase consisting of stock acetate buffer (pH 5)-methanol (4:1, v/v) using an isocratic elution at the flow rate of 1.0 mL/min. The obtained LODs for kynurenine and tryptophane were 0.5 and 0.4 µmol/L, respectively. The analytical method for human plasma samples was validated and confirmed by LC-UV and LC-MS. The recoveries were in the range of 84.8-110%, and the precision was lower than 5.9%. Copyright © 2010 John Wiley & Sons, Ltd.

  3. Electrochemical behavior of dye-linked L-proline dehydrogenase on glassy carbon electrodes modified by multi-walled carbon nanotubes

    PubMed Central

    Zheng, Haitao; Lin, Leyi; Okezaki, Yosuke; Kawakami, Ryushi; Sakuraba, Haruhiko; Ohshima, Toshihisa; Takagi, Keiichi

    2010-01-01

    Summary A glassy carbon electrode (GC) was modified by multi-walled carbon nanotubes (MWCNTs). The modified electrode showed a pair of redox peaks that resulted from the oxygen-containing functional groups on the nanotube surface. A recombinant thermostable dye-linked L-proline dehydrogenase (L-proDH) from hyperthermophilic archaeon (Thermococcus profundus) was further immobilized by physical adsorption. The modified electrode (GC/MWCNTs/L-proDH) exhibited an electrocatalytic signal for L-proline compared to bare GC, GC/L-proDH and GC/MWCNTs electrodes, which suggested that the presence of MWCNTs efficiently enhances electron transfer between the active site of enzyme and electrode surface. The immobilized L-proDH showed a typical Michaelis–Menten catalytic response with lower apparent constant. PMID:21977403

  4. Electro-oxidation and determination of antihistamine drug, cetirizine dihydrochloride at glassy carbon electrode modified with multi-walled carbon nanotubes.

    PubMed

    Patil, Roopa H; Hegde, Rajesh N; Nandibewoor, Sharanappa T

    2011-03-01

    A multi-walled carbon nanotube (MWCNT) film-modified glassy carbon electrode (GCE) was constructed for the determination of an antihistamine drug, cetirizine dihydrochloride (CTZH) using cyclic voltammetry (CV). Owing to the unique structure and extraordinary properties of MWCNT, the MWCNT film has shown an obvious electrocatalytic activity towards oxidation of CTZH, since it facilitates the electron transfer and significantly enhances the oxidation peak current of CTZH. All experimental parameters have been optimized. Under the optimum conditions, the oxidation peak current was linearly proportional to the concentration of CTZH in the range from 5.0×10(-7) to 1.0×10(-5)M. The detection limit was 7.07×10(-8)M with 180s accumulation. Finally, the proposed sensitive and simple electrochemical method was successfully applied to CTZH determination in pharmaceutical and urine samples.

  5. A Voltammetric Biosensor Based on Glassy Carbon Electrodes Modified with Single-Walled Carbon Nanotubes/Hemoglobin for Detection of Acrylamide in Water Extracts from Potato Crisps.

    PubMed

    Krajewska, Agnieszka; Radecki, Jerzy; Radecka, Hanna

    2008-09-23

    The presence of toxic acrylamide in a wide range of food products such as potato crisps, French fries or bread has been confirmed by Swedish scientists from Stockholm University. The neurotoxicity, possible carcinogenicity of this compound and its metabolites compels us to control them by quantitative and qualitative assays. Acrylamide forms adduct with hemoglobin (Hb) as a result of the reaction the -NH2 group of the Nterminal valine with acrylamide. In this work we present the use of glassy carbon electrodes coated with single-walled carbon nanotubes (SWCNTs) and Hb for voltammetric detection of acrylamide in water solutions. The electrodes presented a very low detection limit (1.0×10(-9) M). The validation made in the matrix obtained by water extraction of potato crisps showed that the electrodes presented are suitable for the direct determination of acrylamide in food samples.

  6. A Novel Electrochemical Sensor for Probing Doxepin Created on a Glassy Carbon Electrode Modified with Poly(4-Amino- benzoic Acid)/Multi-Walled Carbon Nanotubes Composite Film

    PubMed Central

    Xu, Xiao-Li; Huang, Fei; Zhou, Guo-Liang; Zhang, Song; Kong, Ji-Lie

    2010-01-01

    A novel electrochemical sensor for sensitive detection of doxepin was prepared, which was based on a glassy carbon electrode modified with poly(4-aminobenzoic acid)/multi-walled carbon nanotubes composite film [poly(4-ABA)/MWNTs/GCE]. The sensor was characterized by scanning electron microscopy and electrochemical methods. It was observed that poly(4-ABA)/MWNTs/GCE showed excellent preconcentration function and electrocatalytic activities towards doxepin. Under the selected conditions, the anodic peak current was linear to the logarithm of doxepin concentration in the range from 1.0 × 10−9 to 1.0 × 10−6 M, and the detection limit obtained was 1.0 × 10−10 M. The poly(4-ABA)/MWNTs/GCE was successfully applied in the measurement of doxepin in commercial pharmaceutical formulations, and the analytical accuracy was confirmed by comparison with a conventional ultraviolet spectrophotometry assay. PMID:22163661

  7. Biosensor based on tyrosinase immobilized on a single-walled carbon nanotube-modified glassy carbon electrode for detection of epinephrine

    PubMed Central

    Apetrei, Irina Mirela; Apetrei, Constantin

    2013-01-01

    A biosensor comprising tyrosinase immobilized on a single-walled carbon nanotube-modified glassy carbon electrode has been developed. The sensitive element, ie, tyrosinase, was immobilized using a drop-and-dry method followed by cross-linking. Tyrosinase maintained high bioactivity on this nanomaterial, catalyzing the oxidation of epinephrine to epinephrine-quinone, which was electrochemically reduced (−0.07 V versus Ag/AgCl) on the biosensor surface. Under optimum conditions, the biosensor showed a linear response in the range of 10–110 μM. The limit of detection was calculated to be 2.54 μM with a correlation coefficient of 0.977. The repeatability, expressed as the relative standard deviation for five consecutive determinations of 10−5 M epinephrine solution was 3.4%. A good correlation was obtained between results obtained by the biosensor and those obtained by ultraviolet spectrophotometric methods. PMID:24348034

  8. Electrochemical behavior and analytical application of ciprofloxacin using a multi-walled nanotube composite film-glassy carbon electrode.

    PubMed

    Fotouhi, Lida; Alahyari, Mahnaz

    2010-11-01

    A simple, rapid and applicable electrochemical method was developed for the determination of ciprofloxacin (Cf) based on a multi-wall carbon nanotubes film-modified glassy carbon electrode (MWCNT/GCE). The constructed electrode (MWCNT/GCE) exhibited excellent electrocatalytic behavior in the oxidation of Cf as evidenced by the enhancement of the oxidation peak current and the shift in the oxidation potential to lower values (by 130 mV) in comparison with the bare GCE. A detailed analysis of cyclic voltammograms and chronoamperograms gave fundamental electrochemical parameters including the electroactive surface coverage (Gamma), the transfer coefficient (alpha), the standard rate constant (k(s)) and diffusion coefficient (D). Under optimized conditions in voltammetric method, the dynamic linear calibration curve for Cf was obtained in the concentration range of 40-1000 micromol/L with the detection limit of 6 micromol/L. The analytical performance of this sensor has been evaluated for detection of the analyte in urine and serum samples. Copyright (c) 2010 Elsevier B.V. All rights reserved.

  9. MIPs-graphene nanoplatelets-MWCNTs modified glassy carbon electrode for the determination of cardiac troponin I.

    PubMed

    Ma, Ya; Shen, Xiao-Lei; Wang, Hai-Shui; Tao, Jia; Huang, Jian-Zhi; Zeng, Qiang; Wang, Li-Shi

    2017-03-01

    An electrochemical sensor with high selectivity in addition to sensitivity was developed for the determination of cardiac troponin I (cTnI), based on the modification of cTnI imprinted polymer film on a glassy carbon electrode (GCE). The sensor was fabricated by layer-by-layer assembled graphene nanoplatelets (GS), multiwalled carbon nanotubes (MWCNTs), chitosan (CS), glutaraldehyde (GA) composites, which can increase the electronic transfer rate and the active surface area to capture a larger number of antigenic proteins. MWCNTs/GS based imprinted polymers (MIPs/MWCNTs/GS) were synthesized by means of methacrylic acid (MAA) as the monomer, ethylene glycol dimethacrylate (EGDMA) as the cross linker α,α'-azobisisobutyronitrile (AIBN) as the initiator and cTnI as the template. In comparison with conventional methods, the proposed electrochemical sensor is highly sensitive for cTnI, providing a better linear response range from 0.005 to 60 ng cm(-3) and a lower limit of detection (LOD) of 0.0008 ng cm(-3) under optimal experimental conditions. In addition, the electrochemical sensor exhibited good specificity, acceptable reproducibility and stability. Moreover, satisfactory results were obtained in real human serum samples, indicating that the developed method has the potential to find application in clinical detection of cTnI as an alternative approach.

  10. Electrochemically oxidized multiwalled carbon nanotube/glassy carbon electrode as a probe for simultaneous determination of dopamine and doxorubicin in biological samples.

    PubMed

    Haghshenas, Esmaeel; Madrakian, Tayyebeh; Afkhami, Abbas

    2016-04-01

    A facile and effective approach of fabricating oxidized multiwalled carbon nanotube/glassy carbon electrode (OMWCNT/GCE) is herein reported. The OMWCNT/GCE was prepared by electrochemical oxidation method in basic media (0.5 mol L(-1) NaOH solution) and used as a sensor for simultaneous determination of dopamine (DA) and doxorubicin (DOX). Scanning electron microscopy, energy dispersive X-ray spectroscopy and cyclic voltammetry were used for characterization and performance study of the OMWCNT/GCE. The modified electrode exhibited good electrocatalytic properties toward the oxidation of DA and DOX. Peaks potential difference of 240 mV between DA and DOX was large enough to determine DA and DOX individually and simultaneously. Square wave voltammetry (SWV) was used for the simultaneous determination of DA and DOX in their binary mixture. Under the optimum conditions, the linear concentration dependences of SW peak current responses were observed for DA and DOX in the concentration ranges of 0.03-55 μmol L(-1) and 0.04-90 μmol L(-1), respectively. The detection limits (S/N = 3) were 8.5 × 10(-3) μmol L(-1), and 9.4 × 10(-3) μmol L(-1) for DA and DOX, respectively. The analytical utility of OMWCNT/GCE was also successfully demonstrated for the simultaneous determination of DA and DOX in human blood serum and urine samples. Graphical Abstract Fabrication of new oxidized multiwalled carbon nanotube/glassy carbon electrode for simultaneous determination of dopamine and doxorubicin.

  11. Direct Electrochemistry of Hemoglobin Immobilized on a Functionalized Multi-Walled Carbon Nanotubes and Gold Nanoparticles Nanocomplex-Modified Glassy Carbon Electrode

    PubMed Central

    Hong, Jun; Zhao, Ying-Xue; Xiao, Bao-Lin; Moosavi-Movahedi, Ali Akbar; Ghourchian, Hedayatollah; Sheibani, Nader

    2013-01-01

    Direct electron transfer of hemoglobin (Hb) was realized by immobilizing Hb on a carboxyl functionalized multi-walled carbon nanotubes (FMWCNTs) and gold nanoparticles (AuNPs) nanocomplex-modified glassy carbon electrode. The ultraviolet-visible absorption spectrometry (UV-Vis), transmission electron microscopy (TEM) and Fourier transform infrared (FTIR) methods were utilized for additional characterization of the AuNPs and FMWCNTs. The cyclic voltammogram of the modified electrode has a pair of well-defined quasi-reversible redox peaks with a formal potential of −0.270 ± 0.002 V (vs. Ag/AgCl) at a scan rate of 0.05 V/s. The heterogeneous electron transfer constant (ks) was evaluated to be 4.0 ± 0.2 s−1. The average surface concentration of electro-active Hb on the surface of the modified glassy carbon electrode was calculated to be 6.8 ± 0.3 × 10−10 mol cm−2. The cathodic peak current of the modified electrode increased linearly with increasing concentration of hydrogen peroxide (from 0.05 nM to 1 nM) with a detection limit of 0.05 ± 0.01 nM. The apparent Michaelis-Menten constant (Kmapp) was calculated to be 0.85 ± 0.1 nM. Thus, the modified electrode could be applied as a third generation biosensor with high sensitivity, long-term stability and low detection limit. PMID:23881129

  12. [Electrocatalytic oxidation of SMZ at multi-wall carbon nanotubes-Nafion modified glassy carbon electrode and its electrochemical determination application].

    PubMed

    Sun, Yu-Qin; You, Wei; Gao, Zuo-Ning

    2008-04-01

    Electrochemical behaviors, electrochemical kinetics and electrochemical determination of sulfamethoxazole (SMZ) at both glassy carbon electrode (GCE) and multi-wall carbon nanotubes-Nafion modified glassy carbon electrode (MWCNTs-Nafion/GCE) were investigated by cyclic voltammetry (CV), chronocoulometry (CC), chronoamperometry (CA), linear scan voltammetry (LSV) and amperometric i-t curve. The experimental results showed that the electrochemical oxidation of SMZ was sluggish on GCE, but the oxidation peak current of SMZ increased significantly at MWCNTs-Nafion/GCE in comparison with that at the bare GCE, which indicated that MWCNTs-Nafion/GCE could catalyze the electrochemical oxidation of SMZ very well. The plot of oxidation peak currents versus the square roots of the scanning rates for the redox in the potential range of 10-1,000 mV x s(-1) showed a straight line, as expected for a diffusion-limited electrochemical process for SMZ electrochemical oxidation. At the bare GCE and MWCNTs-Nafion/GCE the oxidation peak current was linearly proportional to the concentration of SMZ over the concentration range 5.0 x 10(-5)-2.5 x 10(-3) mol x L(-1) and 1.0 x 10(-5)-6.0 x 10(-3) mol x L(-1). The detection limits were 1.0 x 10(-5) and 5.0 x 10(-7) mol x L(-1). The relative standard deviation was between 0.85% -1.98% and the recovery was in the range of 98%-101.2%. This MWCNTs-Nafion/GCE could be applied in SMZ electrochemical determination with satisfied results. The proposed method can be applied to the determination of SMZ in tablet samples with satisfied results.

  13. Electrochemical and spectroelectrochemical behavior of the TCNQ(0/)(-) couple on a glassy carbon electrode. Layer-by-layer nucleation and growth.

    PubMed

    Gómez, L; Rodríguez-Amaro, R

    2006-08-15

    On the basis of the electrochemical results obtained for thin films of 7,7,8,8- tetracyanoquinodimethane (TCNQ) on a glassy carbon electrode, the reduction and oxidation of the [TCNQ](0/)(-) couple in KCl aqueous media occurs via a mechanism involving layer-by-layer nucleation and growth. In situ recorded UV-visible spectroelectrochemical data allow two different crystal structures for the oxidized form of TCNQ to be discriminated.

  14. Langmuir-Blodgett film of p-tert-butylthiacalix[4]arene modified glassy carbon electrode as voltammetric sensor for the determination of Hg(II).

    PubMed

    Wang, Fei; Wei, Xiaohan; Wang, Chenbin; Zhang, Shusheng; Ye, Baoxian

    2010-01-15

    The pi-A isotherms and UV-vis spectra of the transferred films suggested that the monolayer of p-tert-butylthiacalix[4]arene can coordinate with Hg(2+) at the air-water surface. From these observations, a glassy carbon electrode coated with Langmuir-Blodgett film of p-tert-butylthiacalix[4] arene as a new voltammetric sensor is designed for the determination of trace amounts of Hg(2+). Compared with bare glassy carbon electrode and modified glassy carbon electrode using direct coating method, the Langmuir-Blodgett film-modified electrode can greatly improve the measuring sensitivity of Hg(2+). Under the selected conditions, the Langmuir-Blodgett film-modified electrode in 0.1molL(-1) H(2)SO(4)+0.01molL(-1) KCl solution shows a linear voltammetric response for Hg(2+) in the range of 5.0x10(-10) to 1.5x10(-7)molL(-1), with a detection limit of 2.0x10(-10)molL(-1). The proposed method was also applied to determine Hg(2+) in water samples (tap, lake and river water). In addition, the fabricated electrode exhibited a distinct advantage of simple preparation, non-toxicity, good reproducibility and good stability.

  15. [Carbon fiber-reinforced plastics as implant materials].

    PubMed

    Bader, R; Steinhauser, E; Rechl, H; Siebels, W; Mittelmeier, W; Gradinger, R

    2003-01-01

    Carbon fiber-reinforced plastics have been used clinically as an implant material for different applications for over 20 years.A review of technical basics of the composite materials (carbon fibers and matrix systems), fields of application,advantages (e.g., postoperative visualization without distortion in computed and magnetic resonance tomography), and disadvantages with use as an implant material is given. The question of the biocompatibility of carbon fiber-reinforced plastics is discussed on the basis of experimental and clinical studies. Selected implant systems made of carbon composite materials for treatments in orthopedic surgery such as joint replacement, tumor surgery, and spinal operations are presented and assessed. Present applications for carbon fiber reinforced plastics are seen in the field of spinal surgery, both as cages for interbody fusion and vertebral body replacement.

  16. Mechanistic characterization and inhibition of sphingomyelinase C over substituted Iron Schiff bases of chitosan adsorbed on glassy carbon electrode.

    PubMed

    Caro, Claudia A; Lillo, Luis; Valenzuela, Francisco J; Cabello, Gerardo

    2017-02-01

    The medical treatment of laxoscelisms is based solely on supportive measures. Although equine antiserum for Sphingomyelinase C (SMASE) and D isomers are available, it is not used due to the risk of an anaphylactic reaction and its unproven efficacy. As potential enzyme inhibitors, derivatives of Iron chitosan complexes were studied (Shiff base having -R = -H, -Cl, -Br, -F, -OCH3, -CH3, -NO2). These chitosan complexes were chosen because they have revealed good results in medicine and catalysis due to their biodegradable characteristics and bioavailability. Besides considering that these complexes have not been studied in relation to this toxin. The mechanisms underlying the catalytic and catcher effects of Iron chitosan complexes were studied using electrochemistry, UV-Vis spectroscopy and microscopic assay at physiological pH. The electrochemical studies showed that one of seven Schiff bases of chitosan adsorbed on glassy carbon electrode was electrocatalytically active for the oxidation of sphingomyelinase at 1.27 V, and that allowed proposing a reaction scheme for SMASE oxidation by adsorbed Iron complexes. On the other hand, even though the spectroscopic studies indicated that there was no chemical bond formation between the complex and SMASE in solution, the microscopic studies showed that this complex proved to be a remarkable cellular protector in presence of the enzyme. In conclusion, Shiff base of chitosan with R = -CH3 was the only active complex in front of sphingomyelinase C, protecting red blood cells, according to our electrochemical and microscopic studies.

  17. Fabrication of alpha-Fe2O3 nanopowder modified glassy carbon electrode for applications in electrochemical sensing.

    PubMed

    Goyal, Rajendra N; Pandey, Ashish K; Kaur, Davinder; Kumar, Ashvani

    2009-08-01

    In the present study, Fe2O3 nanopowder has been grown by Ultrasonic mist chemical vapor deposition (UM-CVD), which is a promising method for large area deposition at low temperatures taking in to account of its simplicity, inexpensiveness and safety. Room temperature XRD results revealed prominent hematite phase with intense (104) reflection and was also in agreement with the HR-TEM results. In situ high temperature X-ray diffraction (XRD) studies clearly indicated the change of phase from hematite to magnetite as the temperature increases above 300 degrees C. The surface morphology and particle size distribution of Fe2O3 nanopowder were characterized using field emission scanning electron microscope (FE-SEM) and high resolution transmission electron microscope (HR-TEM), which revealed that the particles were spherical in nature and distributed in range of 50-100 nm. SQUID magnetometry results indicate the ferromagnetic nature of the nanopowder with crystallite size of 6 nm as calculated from M-H curve. Transmittance of approximately 55% and estimated direct band gap of 2.5 eV was observed. Further, the nanopowder was used to modify glassy carbon electrode (GCE) and the modified electrode was found to exhibit electrocatalytic activity for the oxidation of dopamine. It is expected that the nanopowder will exhibit promising applications in the development of sensors.

  18. A reagentless non-enzymatic hydrogen peroxide sensor presented using electrochemically reduced graphene oxide modified glassy carbon electrode.

    PubMed

    Mutyala, Sankararao; Mathiyarasu, Jayaraman

    2016-12-01

    Herein, we report a simple, facile and reproducible non-enzymatic hydrogen peroxide (H2O2) sensor using electrochemically reduced graphene oxide (ERGO) modified glassy carbon electrode (GCE). The modified electrode was characterized by Fourier transform infrared (FT-IR), UV-Visible, scanning electron microscopy (SEM) and atomic force microscopy (AFM) techniques. Cyclic voltammetric (CV) analysis revealed that ERGO/GCE exhibited virtuous charge transfer properties for a standard redox systems and showed excellent performance towards electroreduction of H2O2. Amperometric study using ERGO/GCE showed high sensitivity (0.3μA/μM) and faster response upon the addition of H2O2 at an applied potential of -0.25V vs. Ag/AgCl. The detection limit is assessed to be 0.7μM (S/N=3) and the time to reach a stable study state current is <3s for a linear range of H2O2 concentration (1-16μM). In addition, the modified electrode exhibited good reproducibility and long-term stability. Copyright © 2016 Elsevier B.V. All rights reserved.

  19. A sensitive bisphenol A voltammetric sensor relying on AuPd nanoparticles/graphene composites modified glassy carbon electrode.

    PubMed

    Su, Bingyuan; Shao, Huilin; Li, Na; Chen, Xiaomei; Cai, Zhixiong; Chen, Xi

    2017-05-01

    In this work, a sensitive bisphenol A (BPA) electrochemical sensor was assembled using a surfactant-free AuPd nanoparticles-loaded graphene nanosheets (AuPdNPs/GNs) modified electrode. The AuPdNPs monodispersed on GNs were successfully prepared by the spontaneous redox reaction between bimetallic precursors and GNs. Because no surfactant or halide ions were involved in the proposed synthesis, the prepared composite was enabled to directly modify a glassy carbon electrode without any pre-treatments. Moreover, due to the synergetic effect of Au and Pd, AuPdNPs/GNs displayed high electrochemical activity with well-defined voltammetric peaks of BPA oxidation and lower overpotential compared with monometallic PdNPs and AuNPs supported GNs. According to the results of differential pulse voltammetry (DPV), under optimized conditions, a good linear response was observed for the concentration of BPA in the range of 0.05-10μM with a detection limit of 8nM. The developed electrochemical sensor was successfully applied to determine BPA in food package. This study indicated that AuPdNPs/GNs based electrochemical sensor can be a promising and reliable tool for rapid analysis of emergency pollution affairs of BPA.

  20. Electrochemical detection of malathion pesticide using acetylcholinesterase biosensor based on glassy carbon electrode modified with conducting polymer film.

    PubMed

    Guler, Muhammet; Turkoglu, Vedat; Kivrak, Arif

    2016-06-01

    Acetylcholinesterase (AChE) biosensor based on conducting poly([2,2̍';5̍' 2″]-terthiophene-3̍-carbaldehyde) (PTT) modified glassy carbon electrode (GCE) was constructed. AChE was immobilized on PTT film surface through the covalent bond between aldehyde and amino groups. The properties of PTT modified GCE were studied using cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS), and scanning electron microscopy (SEM). The biosensor showed an oxidation peak at +0.83 V related to the oxidation of thiocholine, hydrolysis product of acetylthiocholine iodide (ATCI), catalyzed by AChE. The optimum current response of the biosensor was observed at pH 7.5-8.0, 40 °C and 120 U/cm(2) of AChE concentration. The biosensor showed a high sensitivity (183.19 μA/mM), a linear range from 0.015 to 1.644 mM, and a good reproducibility with 1.7 % of relative standard deviation (RSD). The biosensor showed a good stability. The interference of glycin, ascorbic acid, histidine, uric acid, dopamine, and arginine on the biosensor response was studied. An important analytical response from these inteferents that overlaps the biosensor response was not observed. The inhibition rate of malathion as a model pesticide was proportional to its concentrations from 9.99 to 99.01 nM. The detection limit was 4.08 nM.

  1. Highly sensitive ethanol chemical sensor based on nanostructured SnO2 doped ZnO modified glassy carbon electrode

    NASA Astrophysics Data System (ADS)

    Harraz, Farid A.; Ismail, Adel A.; Ibrahim, Ahmed A.; Al-Sayari, S. A.; Al-Assiri, M. S.

    2015-10-01

    Chemical sensors represent an essential strategy for the monitoring of environmental constituents at low level exposures, but are often limited by relatively low sensitivity and slow response time. Here we report highly crystalline SnO2 doped ZnO framework with a cave-shaped porous nanostructure synthesized by a facile chemical approach as a high performance ethanol chemical sensor. A simple sensing system in solution is established using the modified glassy carbon electrode and applying the current-potential (I-V) and cyclic voltammetry techniques. With unique pore channels and small crystallite size, efficient electron and ion transport occur, leading to a remarkable sensitivity of 62.56 μA cm-2 mM-1 which is, to our knowledge, 9 orders of magnitude higher than those previously reported. The calibration plot is linear (r2 = 0.9887) over ethanol concentration range 0.195-25 mM, with a limit of detection 0.137 mM. The interaction of ethanol is a diffusion dominated with fast electron-transfer kinetics. The findings can open up exciting opportunities to fabricate highly efficient chemical sensors.

  2. Morphology-dependent NiO modified glassy carbon electrode surface for lead(II) and cadmium(II) detection

    NASA Astrophysics Data System (ADS)

    Li, Xuewu; Wen, Hao; Fu, Qiang; Peng, Dai; Yu, Jingui; Zhang, Qiaoxin; Huang, Xingjiu

    2016-02-01

    Glassy carbon electrode (GCE) surfaces have been modified with different NiO morphologies consisting of rods NiO, flakes NiO and balls NiO prepared via the hydrothermal synthesis method for Pb(II) and Cd(II) detection by using the square wave anodic stripping voltammetry (SWASV). Meanwhile, the typical cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS), BET surface area and adsorption property of the modified electrode surfaces have been investigated to evaluate their electrochemical detection effect. Results show that balls NiO modified GCE can get the optimal detection ability for its highest detection sensitivity to Pb(II) (13.46 A M-1) and Cd(II) (5.10 A M-1), the lowest detection limit (DL) to Pb(II) (0.08 μM) and Cd(II) (0.07 μM) as well as the superior linear relativity. In addition, an enhanced current at redox peaks, lower electron transfer resistance, larger BET surface area and stronger adsorption capacity have been confirmed for the balls NiO modified GCE surface. Finally, excellent stability and reproducibility of balls NiO modified electrodes for Pb(II) and Cd(II) detection have also been proved via the SWASV responses.

  3. Electrochemical determination of maltol in beverages with glassy carbon electrode and its silica sol-gel modified electrode.

    PubMed

    Di, Junwei; Bi, Shuping; Zhang, Feng

    2004-05-28

    The electrochemical behavior of maltol on a glassy carbon (GC) electrode was investigated. The results were applied to differential pulse voltammetric determination of maltol in beverages pretreated by ultrafiltration. Under the optimum experimental conditions, the linear range is 1x10(-5) to 6x10(-4)moll(-1) maltol and the relative standard deviation for 0.4mmoll(-1) maltol is 0.6% (n=9). The detection limit was 5mumoll(-1). Furthermore, silica sol-gel film on GC electrode could be used as suitable selective membrane, which integrated selective membrane on the electrode and substituted for the pretreatment of ultrafiltration. Under the above conditions, maltol was determined by semi-differential linear sweep voltammetry at a silica sol-gel modified GC electrode in the concentration range of 5x10(-6) to 5x10(-4)moll(-1). The detection limit was 2mumoll(-1) and the relative standard deviation for 0.1mmoll(-1) maltol was 0.7% (n=7). The proposed method is of sensitivity, simplicity, rapidness and no contamination. It had been applied to the direct determination of maltol in beverages such as grape wines, drinks and beers without any pretreatment. The results obtained with the present method were satisfactory with those obtained by spectrophotometry. It could be used as a simple and practical method for the determination of the flavor enhancer maltol in beverages.

  4. Electrocatalytic Oxidation of Ascorbic Acid Using a Poly(aniline-co-m-ferrocenylaniline) Modified Glassy Carbon Electrode

    PubMed Central

    Chairam, Sanoe; Sriraksa, Worawit; Amatatongchai, Maliwan; Somsook, Ekasith

    2011-01-01

    A poly(aniline-co-m-ferrocenylaniline) was successfully synthesized on a glassy carbon electrode (GCE) by electrochemical copolymerization using a scan potential range from −0.3 to +0.9 V (vs. Ag/AgCl) in 0.5 M H2SO4 containing 30% acetonitrile (ACN), 0.1 M aniline (Ani) and 0.005 M m-ferrocenyaniline (m-FcAni). The field emission scanning electron microscope (FESEM) and electrochemical methods were used to characterize the poly(Ani-co-m-FcAni) modified electrode. The poly(Ani-co-m-FcAni)/GCE exhibited excellent electrocatalytic oxidation of ascorbic acid (AA) in citrate buffer solution (CBS, pH 5.0). The anodic peak potential of AA was shifted from +0.55 V at the bare GCE to +0.25 V at the poly(Ani-co-m-FcAni)/GCE with higher current responses than those seen on the bare GCE. The scan number at the 10th cycle was selected as the maximum scan cycle in electrochemical polymerization. The limit of detection (LOD) was estimated to be 2.0 μM based on the signal-to-noise ratio (S/N = 3). The amperometric responses demonstrated an excellent selectivity for AA determination over glucose (Glu) and dopamine (DA). PMID:22346636

  5. Simultaneous voltammetric determination of acetaminophen and tramadol using Dowex50wx2 and gold nanoparticles modified glassy carbon paste electrode.

    PubMed

    Sanghavi, Bankim J; Srivastava, Ashwini K

    2011-11-14

    A glassy carbon paste electrode (GCPE) modified with a cation exchanger resin, Dowex50wx2 and gold nanoparticles (D50wx2-GNP-GCPE) has been developed for individual and simultaneous determination of acetaminophen (ACOP) and tramadol (TRA). The electrochemical behavior of both the molecules has been investigated employing cyclic voltammetry (CV), chronocoulometry (CC), electrochemical impedance spectroscopy (EIS) and adsorptive stripping square wave voltammetry (AdSSWV). The studies revealed that the oxidation of ACOP and TRA is facilitated at D50wx2-GNP-GCPE. Using AdSSWV, the method allowed simultaneous determination of ACOP and TRA in the linear working range of 3.34×10(-8) to 4.22×10(-5) M with detection limits of 4.71×10(-9) and 1.12×10(-8) M (S/N=3) for ACOP and TRA respectively. The prepared modified electrode shows several advantages such as simple preparation method, long-time stability, ease of preparation and regeneration of the electrode surface by simple polishing and excellent reproducibility. The high sensitivity and selectivity of D50wx2-GNP-GCPE were demonstrated by its practical application in the determination of both ACOP and TRA in pharmaceutical formulations, urine and blood serum samples.

  6. A novel poly(cyanocobalamin) modified glassy carbon electrode as electrochemical sensor for voltammetric determination of peroxynitrite.

    PubMed

    Wang, Yan; Chen, Zhen-zhen

    2010-07-15

    This report described the direct voltammetric detection of peroxynitrite (ONOO(-)) at a novel cyanocobalamin modified glassy carbon electrode prepared by electropolymeriation method. The electrochemical behaviors of peroxynitrite at the modified electrode were studied by cyclic voltammetry. The results showed that this new electrochemical sensor exhibited an excellent electrocatalytic activity to oxidation of peroxynitrite. The mechanism of catalysis was discussed. Based on electrocatalytic oxidation of peroxynitrite at the poly(cyanocobalamin) modified electrode, peroxynitrite was sensitively detected by differential pulse voltammetry. Under optimum conditions, the anodic peak current was linear to concentration of peroxynitrite in the range of 2.0x10(-6) to 3.0x10(-4) mol L(-1) with a detection limit of 1.0x10(-7) mol L(-1) (S/N of 3). The proposed method has been applied to determination of peroxynitrite in human serum with satisfactory results. This poly(cyanocobalamin) modified electrode showed high selectivity and sensitivity to peroxynitrite determination, which could be used in quantitative detection of peroxynitrite in vivo and in vitro. Copyright 2010 Elsevier B.V. All rights reserved.

  7. Amperometric detection of Sudan I in red chili powder samples using Ag nanoparticles decorated graphene oxide modified glassy carbon electrode.

    PubMed

    Prabakaran, E; Pandian, K

    2015-01-01

    A simple and sensitive electrochemical method was developed to determine the concentration of Sudan I in chili powder based on silver nanoparticles decorated graphene oxide modified glassy carbon electrode (AgNPs@GO/GCE). The voltammetry behaviour of Sudan I on modified GCE was investigated in phosphate buffer medium (PBS) with various pH ranges and the electron transfer properties were studied. It is found that the AgNPs@GO/GCE can catalyse the reduction of azo group, -N=N- followed by electrochemical oxidation of (-)OH group present in Sudan I dye molecule. Quantitative detection of Sudan I present in food products was carried out by amperometry method in which reduction potential was fixed at -0.77 V vs. Ag/AgCl. The amperometry method showed an excellent performance with a sensitivity of 6.83 μA mM(-1) and a detection limit of 11.4 × 10(-7)ML(-1). A linear calibration graph was constructed in the ranging 3.90 × 10(-6) to 3.19 × 10(-5)ML(-1). The method was successfully applied for the determination of Sudan I in red chili powder samples.

  8. Electrocatalytic oxidation of ascorbic acid using a poly(aniline-co-m-ferrocenylaniline) modified glassy carbon electrode.

    PubMed

    Chairam, Sanoe; Sriraksa, Worawit; Amatatongchai, Maliwan; Somsook, Ekasith

    2011-01-01

    A poly(aniline-co-m-ferrocenylaniline) was successfully synthesized on a glassy carbon electrode (GCE) by electrochemical copolymerization using a scan potential range from -0.3 to +0.9 V (vs. Ag/AgCl) in 0.5 M H2SO4 containing 30% acetonitrile (ACN), 0.1 M aniline (Ani) and 0.005 M m-ferrocenyaniline (m-FcAni). The field emission scanning electron microscope (FESEM) and electrochemical methods were used to characterize the poly(Ani-co-m-FcAni) modified electrode. The poly(Ani-co-m-FcAni)/GCE exhibited excellent electrocatalytic oxidation of ascorbic acid (AA) in citrate buffer solution (CBS, pH 5.0). The anodic peak potential of AA was shifted from +0.55 V at the bare GCE to +0.25 V at the poly(Ani-co-m-FcAni)/GCE with higher current responses than those seen on the bare GCE. The scan number at the 10th cycle was selected as the maximum scan cycle in electrochemical polymerization. The limit of detection (LOD) was estimated to be 2.0 μM based on the signal-to-noise ratio (S/N = 3). The amperometric responses demonstrated an excellent selectivity for AA determination over glucose (Glu) and dopamine (DA).

  9. Amino-functionalized mesoporous silica modified glassy carbon electrode for ultra-trace copper(II) determination.

    PubMed

    Dai, Xingxin; Qiu, Fagui; Zhou, Xuan; Long, Yumei; Li, Weifeng; Tu, Yifeng

    2014-10-27

    This paper described a facile and direct electrochemical method for the determination of ultra-trace Cu(2+) by employing amino-functionalized mesoporous silica (NH2-MCM-41) as enhanced sensing platform. NH2-MCM-41 was prepared by using a post-grafting process and characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and fourier transform infrared (FTIR) spectroscopy. NH2-MCM-41 modified glassy carbon (GC) electrode showed higher sensitivity for anodic stripping voltammetric (ASV) detection of Cu(2+) than that of MCM-41 modified one. The high sensitivity was attributed to synergistic effect between MCM-41 and amino-group, in which the high surface area and special mesoporous morphology of MCM-41 can cause strong physical absorption, and amino-groups are able to chelate copper ions. Some important parameters influencing the sensor response were optimized. Under optimum experimental conditions the sensor linearly responded to Cu(2+) concentration in the range from 5 to 1000 ng L(-1) with a detection limit of 0.9 ng L(-1) (S/N=3). Moreover, the sensor possessed good stability and electrode renewability. In the end, the proposed sensor was applied for determining Cu(2+) in real samples and the accuracy of the results were comparable to those obtained by inductively coupled plasma optical emission spectrometry (ICP-OES) method. Copyright © 2014 Elsevier B.V. All rights reserved.

  10. Electrochemical sensor for Isoniazid based on the glassy carbon electrode modified with reduced graphene oxide-Au nanomaterials.

    PubMed

    Guo, Zhuo; Wang, Ze-Yu; Wang, Hui-Hua; Huang, Guo-Qing; Li, Meng-Meng

    2015-12-01

    A sensitive electrochemical sensor has been fabricated to detect Isoniazid (INZ) using reduced graphene oxide (RGO) and Au nanocomposites (RGO-Au). RGO-Au nanocomposites were synthesized by a solution-based approach of chemical co-reduction of Au(III) and graphene oxide (GO), and were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Raman spectroscopy, and Fourier transform infrared (FT-IR). The Au nanoparticles separate the RGO sheets in the precipitate and prevent RGO sheets from aggregation upon π-π stacking interactions. RGO-Au nanocomposites were used to modify the glassy carbon electrode (GCE). The electrochemical properties of RGO-Au/GCE were investigated by cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS), and the RGO-Au/GCE exhibited remarkably strong electrocatalytic activities towards INZ. Under the optimized conditions, there was linear relationships between the peak currents and the concentrations in the range of 1.0×10(-7)M to 1.0×10(-3)M for INZ, with the limit of detection (LOD) (based on S/N=3) of 1.0×10(-8)M for INZ.

  11. The effect of glassy carbon surface oxides in non-aqueous voltammetry: the case of quinones in acetonitrile.

    PubMed

    Staley, Patrick A; Newell, Christina M; Pullman, David P; Smith, Diane K

    2014-11-04

    Glassy carbon (GC) electrodes are well-known to contain oxygenated functional groups such as phenols, carbonyls, and carboxylic acids on their surface. The effects of these groups on voltammetry in aqueous solution are well-studied, but there has been little discussion of their possible effects in nonaqueous solution. In this study, we show that the acidic functional groups, particularly phenols, are likely causes of anomalous features often seen in the voltammetry of quinones in nonaqueous solution. These features, a too small second cyclic voltammetric wave and extra current between the two waves that sometimes appears to be a small, broad third voltammetric wave, have previously been attributed to different types of dimerization. In this work, concentration-dependent voltammetry in acetonitrile rules out dimerization with a series of alkyl-benzoquinones because the anomalous features get larger as the concentration decreases. At low concentrations, solution bimolecular reactions will be relatively less important than reactions with surface groups. Addition of substoichiometric amounts of naphthol at higher quinone concentrations produces almost identical behavior as seen at low quinone concentrations with no added naphthol. This implicates hydrogen bonding and proton transfer from the surface phenolic groups as the cause of the anomalous features in quinone voltammetry at GC electrodes. This conclusion is supported by the perturbation of surface oxide coverage on GC electrodes through different electrode pretreatments.

  12. Electrocatalytical oxidation and sensitive determination of acetaminophen on glassy carbon electrode modified with graphene-chitosan composite.

    PubMed

    Zheng, Meixia; Gao, Feng; Wang, Qingxiang; Cai, Xili; Jiang, Shulian; Huang, Lizhang; Gao, Fei

    2013-04-01

    The electrochemical behaviors of acetaminophen (ACOP) on a graphene-chitosan (GR-CS) nanocomposite modified glassy carbon electrode (GCE) were investigated by cyclic voltammetry (CV), chronocoulometry (CC) and differential pulse voltammetry (DPV). Electrochemical characterization showed that the GR-CS nanocomposite had excellent electrocatalytic activity and surface area effect. As compared with bare GCE, the redox signal of ACOP on GR-CS/GCE was greatly enhanced. The values of electron transfer rate constant (ks), diffusion coefficient (D) and the surface adsorption amount (Γ(*)) of ACOP on GR-CS/GCE were determined to be 0.25s(-1), 3.61×10(-5) cm(2) s(-1) and 1.09×10(-9) mol cm(-2), respectively. Additionally, a 2e(-)/2H(+) electrochemical reaction mechanism of ACOP was deduced based on the acidity experiment. Under the optimized conditions, the ACOP could be quantified in the range from 1.0×10(-6) to 1.0×10(-4) M with a low detection limit of 3.0×10(-7) M based on 3S/N. The interference and recovery experiments further showed that the proposed method is acceptable for the determination of ACOP in real pharmaceutical preparations.

  13. Fabrication of folic acid sensor based on the Cu doped SnO2 nanoparticles modified glassy carbon electrode

    NASA Astrophysics Data System (ADS)

    Lavanya, N.; Radhakrishnan, S.; Sudhan, N.; Sekar, C.; Leonardi, S. G.; Cannilla, C.; Neri, G.

    2014-07-01

    A novel folic acid biosensor has been fabricated using Cu doped SnO2 nanoparticles (NPs) synthesized by a simple microwave irradiation method. Powder XRD and TEM studies confirmed that both the pure and Cu doped SnO2 (Cu: 0, 10, 20wt%) crystallized in tetragonal rutile-type structure with spherical morphology. The average crystallite size of pure SnO2 was estimated to be around 16 nm. Upon doping, the crystallite sizes decreased to 9 nm and 5 nm for 10 and 20wt% Cu doped SnO2 respectively. XPS studies confirmed the electronic state of Sn and Cu to be 4+ and 2+ respectively. Cu (20wt%) doped SnO2 NPs are proved to be a good sensing element for the determination of folic acid (FA). Cu-SnO2 NPs (20wt%) modified glassy carbon electrode (GCE) exhibited the lowest detection limit of 0.024 nM over a wide folic acid concentration range of 1.0 × 10-10 to 6.7 × 10-5 M at physiological pH of 7.0. The fabricated sensor is highly selective towards the determination of FA even in the presence of a 100 fold excess of common interferent ascorbic acid. The sensor proved to be useful for the estimation of FA content in pharmaceutical sample with satisfactory recovery.

  14. Adsorption stripping voltammetry of phenol at Nafion-modified glassy carbon electrode in the presence of surfactants.

    PubMed

    Yi, H; Wu, K; Hu, S; Cui, D

    2001-12-24

    In this paper, a new voltammetric method for the determination of phenol is described. In pH 8.00 phosphate buffer and in the presence of long-chain cationic surfactant-cetyltrimethylammonium bromide-phenol has a very sensitive oxidation peak at 0.47 V (vs. SCE) on the Nafion-modified glassy carbon electrode (GCE). The experimental parameters, such as supporting electrolyte and pH values, amounts of Nafion, varieties and concentration of surfactants, accumulation potential and time, as well as scan rate were optimized. The peak current is linear with the concentration of phenol in the range from 8x10(-9) to 1x10(-5) M, and the detection limit is 1x10(-9) M after being accumulated at -0.50 V (vs. SCE) for 3 min. Trace levels of phenol in water samples were determined by using this voltammetric method, the average recovery was calculated to be 99.56%.

  15. Determination of fenitrothion in water using a voltammetric sensor based on a polymer-modified glassy carbon electrode.

    PubMed

    Amare, Meareg; Abicho, Samuel; Admassie, Shimelis

    2014-01-01

    A glassy carbon electrode (GCE) modified with poly(4-amino-3-hydroxynaphthalene sulfonic acid) (poly-AHNSA) was used for the selective and sensitive determination of fenitrothion (FT) organophosphorus pesticide in water. The electrochemical behavior of FT at the bare GCE and the poly-AHNSA/GCE were compared using cyclic voltammetry. Enhanced peak current response and shift to a lower potential at the polymer-modified electrode indicated the electrocatalytic activity of the polymer film towards FT. Under optimized solution and method parameters, the adsorptive stripping square wave voltammetric reductive peak current of FT was linear to FT concentration in the range of 0.001 to 6.6 x 10(-6) M, and the LOD obtained (3delta/m) was 7.95 x 10(-10) M. Recoveries in the range 96-98% of spiked FT in tap water and reproducible results with RSD of 2.6% (n = 5) were obtained, indicating the potential applicability of the method for the determination of trace levels of FT in environmental samples.

  16. Determination of trace levels of diosmin in a pharmaceutical preparation by adsorptive stripping voltammetry at a glassy carbon electrode.

    PubMed

    El-Shahawi, M S; Bashammakh, A S; El-Mogy, T

    2006-10-01

    A systematic study on the electrochemical behavior of diosmin in Britton-Robinson buffer (pH 2.0-10.0) at a glassy carbon electrode (GCE) was made. The oxidation process of the drug was found to be quasi-reversible with an adsorption-controlled step. The adsorption stripping response was evaluated with respect to various experimental conditions, such as the pH of the supporting electrolyte, the accumulation potential and the accumulation time. The observed anodic peak current at +0.73 V vs. Ag/AgCl reference electrode increased linearly over two orders of magnitude from 5.0x10(-8) M to 9.0x10(-6) M. A limit of detection down to 3.5x10(-8) M of diosmin at the GCE was achieved with a mean recovery of 97+/-2.1%. Based on the electrochemical data, an open-circuit accumulation step in a stirred sample solution of BR at pH 3.0 was developed. The proposed method was successfully applied to the determination of the drug in pharmaceutical formulations. The results compared favorably with the data obtained via spectrophotometric and HPLC methods.

  17. Simultaneous determination of dopamine, ascorbic acid and uric acid at poly (Evans Blue) modified glassy carbon electrode.

    PubMed

    Lin, Liqing; Chen, Jinghua; Yao, Hong; Chen, Yuanzhong; Zheng, Yanjie; Lin, Xinhua

    2008-06-01

    A sensitive and selective electrochemical method for the determination of dopamine using an Evans Blue polymer film modified on glassy carbon electrode was developed. The Evans blue polymer film modified electrode shows excellent electrocatalytic activity toward the oxidation of dopamine in phosphate buffer solution (pH 4.5). The linear range of 1.0 x 10(-6)-3.0 x 10(-5) M and detection limit of 2.5 x 10(-7) M were observed in pH 4.5 phosphate buffer solutions. The interference studies showed that the modified electrode exhibits excellent selectivity in the presence of large excess of ascorbic acid and uric acid. The separation of the oxidation peak potentials for dopamine-ascorbic acid and dopamine-uric acid were about 182 mV and 180 mV, respectively. The differences are large enough to determine AA, DA and UA individually and simultaneously. This work provides a simple and easy approach to selectively detect dopamine in the presence of ascorbic acid and uric acid in physiological samples.

  18. Application of neural networks with novel independent component analysis methodologies to a Prussian blue modified glassy carbon electrode array.

    PubMed

    Wang, Liang; Yang, Die; Fang, Cheng; Chen, Zuliang; Lesniewski, Peter J; Mallavarapu, Megharaj; Naidu, Ravendra

    2015-01-01

    Sodium potassium absorption ratio (SPAR) is an important measure of agricultural water quality, wherein four exchangeable cations (K(+), Na(+), Ca(2+) and Mg(2+)) should be simultaneously determined. An ISE-array is suitable for this application because its simplicity, rapid response characteristics and lower cost. However, cross-interferences caused by the poor selectivity of ISEs need to be overcome using multivariate chemometric methods. In this paper, a solid contact ISE array, based on a Prussian blue modified glassy carbon electrode (PB-GCE), was applied with a novel chemometric strategy. One of the most popular independent component analysis (ICA) methods, the fast fixed-point algorithm for ICA (fastICA), was implemented by the genetic algorithm (geneticICA) to avoid the local maxima problem commonly observed with fastICA. This geneticICA can be implemented as a data preprocessing method to improve the prediction accuracy of the Back-propagation neural network (BPNN). The ISE array system was validated using 20 real irrigation water samples from South Australia, and acceptable prediction accuracies were obtained. Copyright © 2014 Elsevier B.V. All rights reserved.

  19. Simultaneous voltammetric determination of ascorbic acid, dopamine and uric acid using polybromothymol blue film-modified glassy carbon electrode.

    PubMed

    Xu, Xiongwei; Lin, Qihuang; Liu, Ailin; Chen, Wei; Weng, Xiuhua; Wang, Changlian; Lin, Xinhua

    2010-06-01

    A sensitive and selective electrochemical method for simultaneous determination of ascorbic acid (AA), dopamine (DA), and uric acid (UA) using an electropolymerized bromothymol blue (BTB)-modified glassy carbon electrode (GCE) was developed. The electrochemically synthesized film was investigated using electrochemical impedance spectroscopy and voltammetric methods. The electrochemical behavior of the polymer-modified electrode depends on film thickness, i.e., the electropolymyerization time. The poly-BTB-modified GCE shows excellent electrocatalytic activity toward the oxidation of AA, DA, and UA in phosphate buffer solution (pH 5.0). The voltametric peak separations of AA/DA, DA/UA, and AA/UA on this modified electrode are 118 mV, 298 mV, and 455 mV, respectively. Therefore the voltammetric responses of these three compounds can be resolved well on the polymer-modified electrode, and simultaneous determination of these three compounds can be achieved. In addition, this modified electrode can be successfully applied to determine AA and DA in injection and UA in urine samples without interference.

  20. Stripping voltammetric determination of pyridine-2-aldoxime methochloride at the iron(III) doped zeolite modified glassy carbon electrode.

    PubMed

    Mehretie, Solomon; Losada, José; Tessema, Merid; Admassie, Shimelis; Solomon, Theodros; Perez-Pariente, Joaquin; Díaz, Isabel

    2012-12-07

    An iron(III) doped zeolite modified glassy carbon electrode was constructed for the determination of pyridine-2-aldoxime methochloride. X-ray diffraction and chemical analysis were utilized to determine the optimum pH and chemical content for doping zeolite. Cyclic voltammetry was used to characterize the modified electrode and study the kinetics of the acid treated and untreated modified electrode. Acid treatment of the modified electrode showed a better electrochemical behavior compared to the untreated iron(III) doped zeolite modified electrode. Square wave anodic stripping voltammetry was employed to investigate the working pH and preconcentration time. The analytical performance of the modified electrode was evaluated, and a linear anodic stripping response for pyridine-2-aldoxime methochloride in the concentration range of 0.5-100.0 μM with a detection limit of 1.61 × 10(-7) M was obtained. Finally, the developed method was successfully applied for the determination of pyridine-2-aldoxime methochloride in a biological sample.

  1. A novel poly(taurine) modified glassy carbon electrode for the simultaneous determination of epinephrine and dopamine.

    PubMed

    Wang, Yan; Chen, Zhen-zhen

    2009-11-01

    A novel taurine modified glassy carbon electrode was prepared by electropolymerization method. The electrochemical behaviors of epinephrine (EP) and dopamine (DA) at the modified electrode were studied by cyclic voltammetry. The modified electrode exhibited enhanced sensitivity and excellent electrochemical discrimination to DA and EP. The cathodic peaks of the two species were well-separated with a potential difference of about 390 mV, so the poly(taurine) modified electrode was used for simultaneous voltammetric measurement of EP and DA by differential pulse voltammetry. Under the optimum conditions, the cathodic peak currents were linear to concentrations of EP and DA in the range of 2.0 x 10(-6) to 6.0 x 10(-4)mol L(-1) and 1.0 x 10(-6) to 8.0 x 10(-4)mol L(-1), respectively. The detection limits for EP and DA were 3.0 x 10(-7) and 1.0 x 10(-7)mol L(-1), respectively. Because the oxidation of ascorbic acid (AA) is an irreversible reaction at modified electrode, the interference of AA for determining EP and DA was eliminated. The modified electrode has been satisfactorily used for the simultaneous determination of EP and DA in pharmaceutical injections.

  2. Potential of glassy carbon and silicon carbide photonic structures as electromagnetic radiation shields for atmospheric re-entry.

    PubMed

    Komarevskiy, Nikolay; Shklover, Valery; Braginsky, Leonid; Hafner, Christian; Lawson, John

    2012-06-18

    During high-velocity atmospheric entries, space vehicles can be exposed to strong electromagnetic radiation from ionized gas in the shock layer. Glassy carbon (GC) and silicon carbide (SiC) are candidate thermal protection materials due to their high melting point and also their good thermal and mechanical properties. Based on data from shock tube experiments, a significant fraction of radiation at hypersonic entry conditions is in the frequency range from 215 to 415 THz. We propose and analyze SiC and GC photonic structures to increase the reflection of radiation in that range. For this purpose, we performed numerical optimizations of various structures using an evolutionary strategy. Among the considered structures are layered, porous, woodpile, inverse opal and guided-mode resonance structures. In order to estimate the impact of fabrication inaccuracies, the sensitivity of the reflectivity to structural imperfections is analyzed. We estimate that the reflectivity of GC photonic structures is limited to 38% in the aforementioned range, due to material absorption. However, GC material can be effective for photonic reflection of individual, strong spectral line. SiC on the other hand can be used to design a good reflector for the entire frequency range.

  3. Electrochemical deposition and behavior of mixed-valent molybdenum oxide film at glassy carbon and ITO electrodes

    NASA Astrophysics Data System (ADS)

    Koçak, Süleyman; Ertaş, Fatma Nil; Dursun, Zekerya

    2013-01-01

    The effect of solution composition and the type of the anionic species on the electrochemical formation of mixed-valent molybdenum oxide on a glassy carbon and ITO electrode surfaces was elucidated. Susccessive recording of the voltammograms has shown that anionic species display different stabilizing effect on the reductive formation of hydrogen molybdenum bronzes [MoO3-x (OH)x] and chloroacetic acid buffer has given the best results. The deposit was built upon cycling the potential between 0 and -0.9 V (vs. Ag/AgCl) via reduction of Mo(VI) to Mo(V) on the electrode surface in pH 3.0 chloroacetic acid solution. Electrochemical impedance measurements carried out in this medium revealed a shift in potential zero charge values from -0.2 V to -0.55 V after the potential of the GCE had been cycled for 30 min. An establishment of mixed-valent molybdenum oxide deposit by time on the gold electrode surface was proved by quartz crystal microbalance measurements. Atomic force and scanning electron microscopy techniques were made use of so as to characterize the surface structures of the electrodes. X-ray photoelectron spectroscopy studies confirmed that the deposit contains both Mo(V) and Mo(VI). The deposited films exhibited unique catalytic activity towards nitrite oxidation consistent with the change in peak characteristics.

  4. Electrochemical Determination of Chlorpyrifos on a Nano-TiO₂Cellulose Acetate Composite Modified Glassy Carbon Electrode.

    PubMed

    Kumaravel, Ammasai; Chandrasekaran, Maruthai

    2015-07-15

    A rapid and simple method of determination of chlorpyrifos is important in environmental monitoring and quality control. Electrochemical methods for the determination of pesticides are fast, sensitive, reproducible, and cost-effective. The key factor in electrochemical methods is the choice of suitable electrode materials. The electrode materials should have good stability, reproducibility, more sensitivity, and easy method of preparation. Mercury-based electrodes have been widely used for the determination of chlorpyrifos. From an environmental point of view mercury cannot be used. In this study a biocompatible nano-TiO2/cellulose acetate modified glassy carbon electrode was prepared by a simple method and used for the electrochemical sensing of chlorpyrifos in aqueous methanolic solution. Electroanalytical techniques such as cyclic voltammetry, differential pulse voltammetry, and amperometry were used in this work. This electrode showed very good stability, reproducibility, and sensitivity. A well-defined peak was obtained for the reduction of chlorpyrifos in cyclic voltammetry and differential pulse voltammetry. A smooth noise-free current response was obtained in amperometric analysis. The peak current obtained was proportional to the concentration of chlorpyrifos and was used to determine the unknown concentration of chlorpyrifos in the samples. Analytical parameters such as LOD, LOQ, and linear range were estimated. Analysis of real samples was also carried out. The results were validated through HPLC. This composite electrode can be used as an alternative to mercury electrodes reported in the literature.

  5. Potential of Glassy Carbon and Silicon Carbide Photonic Structures as Electromagnetic Radiation Shields for Atmospheric Re-entry

    NASA Technical Reports Server (NTRS)

    Komarevskiy,Nikolay; Shklover, Valery; Braginsky, Leonid; Hafner, Christian; Lawson, John W.

    2012-01-01

    During high-velocity atmospheric entries, space vehicles can be exposed to strong electromagnetic radiation from ionized gas in the shock layer. Glassy carbon (GC) and silicon carbide (SiC) are candidate thermal protection materials due to their high melting point and also their good thermal and mechanical properties. Based on data from shock tube experiments, a significant fraction of radiation at hypersonic entry conditions is in the frequency range from 215 to 415 THz. We propose and analyze SiC and GC photonic structures to increase the reflection of radiation in that range. For this purpose, we performed numerical optimizations of various structures using an evolutionary strategy. Among the considered structures are layered, porous, woodpile, inverse opal and guided-mode resonance structures. In order to estimate the impact of fabrication inaccuracies, the sensitivity of the reflectivity to structural imperfections is analyzed. We estimate that the reflectivity of GC photonic structures is limited to 38% in the aforementioned range, due to material absorption. However, GC material can be effective for photonic reflection of individual, strong spectral line. SiC on the other hand can be used to design a good reflector for the entire frequency range.

  6. Amperometric sensor based on tricobalt tetroxide nanoparticles-graphene nanocomposite film modified glassy carbon electrode for determination of tyrosine.

    PubMed

    Jiang, Lin; Gu, Shuqing; Ding, Yaping; Ye, Daixin; Zhang, Zhen; Zhang, Fenfen

    2013-07-01

    An electrochemical sensor based on tricobalt tetroxide nanoparticles-graphene nanocomposite film modified glassy carbon electrodes (GCEs) for sensitive determination of L-tyrosine (L-Tyr) was presented here. The nanoparticles were fabricated by electro-polymerization technology. Scanning electron microscopy was implemented to characterize morphology of the nanocomposite film. The electron transfer behavior of modified electrodes was investigated in 5 mM K3[Fe(CN)6]/K4[Fe(CN)6] solution using cyclic voltammetry and electrochemical impedance spectroscopy (EIS). The electrochemical response of modified electrodes toward L-Tyr was investigated by cyclic voltammetry (CV), square wave voltammetry (SWV), amperometry in detail. The results indicated that synergistic effect of Co3O4 NPs and graphene film dramatically improved the conductivity and sensitivity of the sensor. Under optimal conditions, a wide linear relationship between the responses and L-Tyr concentrations ranging from 1.0×10(-8) to 4.0×10(-5) mol L(-1) was obtained with a comparatively low detection limit of 1.0×10(-9) mol L(-1). Furthermore, the sensor also displays excellent sensitivity and high stability. To further study the practical applicability of the fabricated sensor, it was applied to detect real samples and the received results were satisfactory.

  7. NH2 + implantations induced superior hemocompatibility of carbon nanotubes

    NASA Astrophysics Data System (ADS)

    Guo, Meixian; Li, Dejun; Zhao, Mengli; Zhang, Yiteng; Deng, Xiangyun; Geng, Dongsheng; Li, Ruying; Sun, Xueliang; Gu, Hanqing; Wan, Rongxin

    2013-05-01

    NH2 + implantation was performed on multiwalled carbon nanotubes (MWCNTs) prepared by chemical vapor deposition. The hemocompatibility of MWCNTs and NH2 +-implanted MWCNTs was evaluated based on in vitro hemolysis, platelet adhesion, and kinetic-clotting tests. Compared with MWCNTs, NH2 +-implanted MWCNTs displayed more perfect platelets and red blood cells in morphology, lower platelet adhesion rate, lower hemolytic rate, and longer kinetic blood-clotting time. NH2 +-implanted MWCNTs with higher fluency of 1 × 1016 ions/cm2 led to the best thromboresistance, hence desired hemocompatibility. Fourier transfer infrared and X-ray photoelectron spectroscopy analyses showed that NH2 + implantation caused the cleavage of some pendants and the formation of some new N-containing functional groups. These results were responsible for the enhanced hemocompatibility of NH2 +-implanted MWCNTs.

  8. A highly efficient nano-cluster artificial peroxidase and its direct electrochemistry on a nano complex modified glassy carbon electrode.

    PubMed

    Hong, Jun; Wang, Wei; Huang, Kun; Yang, Wei-Yun; Zhao, Ying-Xue; Xiao, Bao-Lin; Gao, Yun-Fei; Moosavi-Movahedi, Zainab; Ghourchian, Hedayatollah; Moosavi-Movahedi, Ali Akbar

    2012-01-01

    A nano-cluster with highly efficient peroxide activity was constructed based on nafion (NF) and cytochrome c (Cyt c). UV-Vis spectrometry and transmission electron microscopy (TEM) methods were utilized for characterization of the nano-structured enzyme or artificial peroxidase (AP). The nano-cluster was composed of a Chain-Ball structure, with an average ball size of about 40 nm. The Michaelis-Menten (K(m)) and catalytic rate (k(cat)) constants of the AP were determined to be 2.5 ± 0.4 µM and 0.069 ± 0.001 s(-1), respectively, in 50 mM PBS at pH 7.0. The catalytic efficiency of the AP was evaluated to be 0.028 ± 0.005 µM(-1) s(-1), which was 39 ± 5% as efficient as the native horseradish peroxidase (HRP). The AP was also immobilized on a functional multi-wall carbon nanotube (MWNCTs)-gold colloid nanoparticles (AuNPs) nano-complex modified glassy carbon (GC) electrode. The cyclic voltammetry of AP on the nano complex modified GC electrode showed a pair of well-defined redox peaks with a formal potential (E°') of -45 ± 2 mV (vs. Ag/AgCl) at a scan rate of 0.05 V/s. The heterogeneous electron transfer rate constant (k(s)) was evaluated to be 0.65 s(-1). The surface concentration of electroactive AP on GC electrode (Γ) was 7 × 10(-10) mol cm(-2). The apparent Michaelis-Menten constant (K(m)(app)) was 0.23 nM.

  9. Nanomolar determination of 4-nitrophenol based on a poly(methylene blue)-modified glassy carbon electrode.

    PubMed

    Giribabu, Krishnamoorthy; Suresh, Ranganathan; Manigandan, Ramadoss; Munusamy, Settu; Kumar, Sivakumar Praveen; Muthamizh, Selvamani; Narayanan, Vengidusamy

    2013-10-07

    A poly(methylene blue)-modified glassy carbon electrode (PMB/GCE) was fabricated by electropolymerisation of methylene blue on a GCE and further utilized to investigate the electrochemical determination of 4-nitrophenol (4-NP) by cyclic voltammetry (CV), differential pulse voltammetry and chronocoulometry. The morphology of the PMB on GCE was examined using a scanning electron microscope (SEM). An oxidation peak of 4-NP at the PMB modified electrode was observed at 0.28 V, and in the case of bare GCE, no oxidation peak was observed, which indicates that PMB/GCE exhibits a remarkable effect on the electrochemical determination of 4-NP. Due to this remarkable effect of PMB/GCE, a sensitive and simple electrochemical method was proposed for the determination of 4-NP. The effect of the scan rate and pH was investigated to determine the optimum conditions at which the PMB/GCE exhibits a higher sensitivity with a lower detection limit. Moreover, kinetic parameters such as the electron transfer number, proton transfer number and standard heterogeneous rate constant were calculated. Under optimum conditions, the oxidation current of 4-NP is proportional to its concentration in the range of 15-250 nM with a correlation coefficient of 0.9963. The detection limit was found to be 90 nM (S/N = 3). The proposed method based on PMB/GCE is simple, easy and cost effective. To further confirm its possible application, the proposed method was successfully used for the determination of 4-NP in real water samples with recoveries ranging from 97% to 101.6%. The interference due to sodium, potassium, calcium, magnesium, copper, zinc, iron, sulphate, carbonate, chloride, nitrate and phosphate was found to be almost negligible.

  10. Pulsed amperometric detection at glassy carbon electrodes: A new waveform for sensitive and reproducible determination of electroactive compounds.

    PubMed

    Nardiello, Donatella; Palermo, Carmen; Natale, Anna; Quinto, Maurizio; Centonze, Diego

    2015-09-24

    In this work, the application of a new pulsed amperometric detection (PAD) waveform at a glassy carbon electrode, operating in typical chromatographic mobile phases, is proposed for the sensitive and reproducible determination of arylethanolaminic and phenolic moiety based compounds (e.g. beta-agonists and polyphenols). Preliminary experiments by cyclic voltammetry were carried out to investigate the electrochemical behaviour and to select the detection and cleaning electrode potentials. The proposed potential-time profile was designed to prevent the carbon electrode fouling under repeated analyses, thus ensuring a reproducible and sensitive quantitative determination, without the need of any mechanical or chemical electrode cleaning procedure. The waveform electrochemical parameters, including detection and delay times, were optimized in terms of sensitivity, limit of detection and response stability. The optimized waveform allowed the sensitive and stable detection of model compounds, such as clenbuterol and caffeic acid, that showed detection limits of 0.1 μg L(-1) and 14 μg L(-1), quantification limits of 0.4 μg L(-1) and 46 μg L(-1), and linearity up to 100 μg L(-1) (r = 0.9993) and 10 mg L(-1) (r = 0.9998), respectively. Similar results were obtained for other compounds of the same classes, with precision values under repeatability conditions ranging from 3.0 to 5.9%. The proposed method can be then considered as an excellent alternative to the post-column detection of beta-agonists, phenols and polyphenols. Copyright © 2015 Elsevier B.V. All rights reserved.

  11. Metal-Catalyzed Alkynylation of Brominated Polyphenylenes. Thermoset Precursors of High Density Monolithic Glassy Carbon

    DTIC Science & Technology

    1993-11-22

    melting events at 152 and 1750C on the first heating scan to 2300C. While the char yield for 4a was only 50% by TGA analysis , the charred material was...after TGA analysis was also a black powder, again indicating that no flow had occurred. The char had a density of 1.59 g/cc. 1 I Polymers 16b and 16c had...material appeared as shiny black droplets after TGA analysis . The charred carbon material from 19a had a density of 1.56 g/cc. Polymers 19b and 19c

  12. Glassy carbon electrode modified with horse radish peroxidase/organic nucleophilic-functionalized carbon nanotube composite for enhanced electrocatalytic oxidation and efficient voltammetric sensing of levodopa.

    PubMed

    Shoja, Yalda; Rafati, Amir Abbas; Ghodsi, Javad

    2016-01-01

    A novel and selective enzymatic biosensor was designed and constructed for voltammetric determination of levodopa (L-Dopa) in aqueous media (phosphate buffer solution, pH=7). Biosensor development was on the basis of to physically immobilizing of horse radish peroxidase (HRP) as electrochemical catalyst by sol-gel on glassy carbon electrode modified with organic nucleophilic carbon nanotube composite which in this composite p-phenylenediamine (pPDA) as organic nucleophile chemically bonded with functionalized MWCNT (MWCNT-COOH). The results of this study suggest that prepared bioorganic nucleophilic carbon nanotube composite (HRP/MWCNT-pPDA) shows fast electron transfer rate for electro oxidation of L-Dopa because of its high electrochemical catalytic activity toward the oxidation of L-Dopa, more--NH2 reactive sites and large effective surface area. Also in this work we measured L-Dopa in the presence of folic acid and uric acid as interferences. The proposed biosensor was characterized by scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDX), FT-IR spectroscopy and cyclic voltammetry (CV). The differential pulse voltammetry (DPV) was used for determination of L-Dopa from 0.1 μM to 1.9 μM with a low detection limit of 40 nM (for S/N=3) and sensitivity was about 35.5 μA/μM. Also this biosensor has several advantages such as rapid response, high stability and reproducibility.

  13. Electron Cyclotron Resonance-Sputtered Nanocarbon Film Electrode Compared with Diamond-Like Carbon and Glassy Carbon Electrodes as Regards Electrochemical Properties and Biomolecule Adsorption

    NASA Astrophysics Data System (ADS)

    Xue, Qiang; Kato, Dai; Kamata, Tomoyuki; Umemura, Shigeru; Hirono, Shigeru; Niwa, Osamu

    2012-09-01

    The electrochemical properties and biocompatible characteristics at an electron cyclotron resonance (ECR)-sputtered nanocarbon film electrode, a diamond-like carbon (DLC) electrode and a glassy carbon (GC) electrode have been studied. The three carbon electrodes show significant current reductions with increased peak separations as a result of protein fouling before oxygen plasma treatment, but the current reductions of the ECR-sputtered nanocarbon and DLC film electrodes are smaller than that of the GC electrode due to their superior surface flatness. The oxygen plasma pretreated ECR-sputtered nanocarbon film electrode exhibits a significant improvement in anti-fouling performance with an improved electron transfer. This is because the pretreated ECR-sputtered nanocarbon film enabled the surface to introduce surface oxygen functionalities that not only improve the interaction between the analytes and the electrode surface but also make the film surface more hydrophilic, which is important for the suppression of biomolecule adsorption. At the same time, the pretreated ECR-sputtered nanocarbon film also retained an ultraflat surface even after pretreatment as a result of the low background current. This excellent performance can only be achieved with our ECR-sputtered nanocarbon film, indicating that our film is promising for application to electrochemical detectors for various biomolecular analytes.

  14. Implantation of nitrogen, carbon, and phosphorus ions into metals

    SciTech Connect

    Guseva, M.I.; Gordeeva, G.V.

    1987-01-01

    The application of ion implantation for alloying offers a unique opportunity to modify the chemical composition, phase constitution, and microstructure of the surface layers of metals. The authors studied ion implantation of nitrogen and carbon into the surface layers of metallic targets. The phase composition of the implanted layers obtained on the Kh18N10T stainless steel, the refractory molybdenum alloy TsM-6, niobium, and nickel was determined according to the conventional method of recording the x-ray diffraction pattern of the specimens using monochromatic FeK/sub alpha/-radiation on a DRON-2,0 diffractometer. The targets were bombarded at room temperature in an ILU-3 ion accelerator. The implantation of metalloid ions was also conducted with the targets being bombarded with 100-keV phosphorus ions and 40-keV carbon ions.

  15. Platinum nanoparticles decorated dendrite-like gold nanostructure on glassy carbon electrodes for enhancing electrocatalysis performance to glucose oxidation

    NASA Astrophysics Data System (ADS)

    Jia, Hongmei; Chang, Gang; Lei, Ming; He, Hanping; Liu, Xiong; Shu, Honghui; Xia, Tiantian; Su, Jie; He, Yunbin

    2016-10-01

    Platinum nanoparticles decorated dendrite-like gold nanostructure, bimetal composite materials on glassy carbon electrode (Pt/DGNs/GC) for enhancing electrocatalysis to glucose oxidation was designed and successfully fabricated by a facile two-step deposition method without any templates, surfactants, or stabilizers. Dendrite-like gold nanostructure was firstly deposited on the GC electrode via the potentiostatic method, and then platinum nanoparticles were decorated on the surface of gold substrate through chemical reduction deposition. X-ray diffraction (XRD), field-emission scanning electron microscope (FE-SEM), energy-dispersive X-ray spectroscopy (EDS) were applied to characterize the evolution of morphology and structure of the as-prepared Pt/DGNs/GC. Based on electrochemical measurements such as cyclic voltammetry, linear voltammetry and chronoamperometry, Pt/DGNs/GC exhibited significantly enhanced electrocatalytic performance to glucose oxidation compared those of pure dendrite-like Au nanoparticles in our previous report. Controlling chemical reduction deposition time, the amount of platinum nanoparticles on Au surface could be regulated, which further tuned electrocatalytic properties toward glucose oxidation. The dendrite-like gold surface partially covered by platinum nanoparticles dramatically enhanced the electrocatalytic performance for the oxidation of glucose because of excellent synergetic effects between gold and platinum species and the increased electrochemical active area from Pt nanoparticles loading. The non-enzymatic glucose biosensor based on Pt/DGNs/GC showed a rapid respond time (within 2 s), wide linear range (from 0.1 mM to 14 mM), low detection limit (0.01 mM), supernal sensitivity (275.44 μA cm-2 mM-1, R = 0.993), satisfactory reproducibility and good stability for glucose sensing. It was demonstrated that Pt/DGNs/GC could work as promising candidate for factual non-enzymatic glucose detection.

  16. Determination of Anthracene on Ag-Au Alloy Nanoparticles/Overoxidized-Polypyrrole Composite Modified Glassy Carbon Electrodes

    PubMed Central

    Mailu, Stephen N.; Waryo, Tesfaye T.; Ndangili, Peter M.; Ngece, Fanelwa R.; Baleg, Abd A.; Baker, Priscilla G.; Iwuoha, Emmanuel I.

    2010-01-01

    A novel electrochemical sensor for the detection of anthracene was prepared by modifying a glassy carbon electrode (GCE) with over-oxidized polypyrrole (PPyox) and Ag-Au (1:3) bimetallic nanoparticles (Ag-AuNPs). The composite electrode (PPyox/Ag-AuNPs/GCE) was prepared by potentiodynamic polymerization of pyrrole on GCE followed by its overoxidation in 0.1 M NaOH. Ag-Au bimetallic nanoparticles were chemically prepared by the reduction of AgNO3 and HAuCl4 using C6H5O7Na3 as the reducing agent as well as the capping agent and then immobilized on the surface of the PPyox/GCE. The nanoparticles were characterized by UV-visible spectroscopy technique which confirmed the homogeneous formation of the bimetallic alloy nanoparticles. Transmission electron microscopy showed that the synthesized bimetallic nanoparticles were in the range of 20–50 nm. The electrochemical behaviour of anthracene at the PPyox/Ag-AuNPs/GCE with Ag: Au atomic ratio 25:75 (1:3) exhibited a higher electrocatalytic effect compared to that observed when GCE was modified with each constituent of the composite (i.e., PPyox, Ag-AuNPs) and bare GCE. A linear relationship between anodic current and anthracene concentration was attained over the range of 3.0 × 10−6 to 3.56 × 10−4 M with a detection limit of 1.69 × 10−7 M. The proposed method was simple, less time consuming and showed a high sensitivity. PMID:22163419

  17. Fibre laser machining for glassy carbon master mould and soft lithography based two-step printing for Ag nanoparticle structures

    NASA Astrophysics Data System (ADS)

    Hu, Qin; Chopra, Pranav

    2011-04-01

    Traditional manufacturing techniques widely used in semiconductor industries involve many processing steps that consume both time and material and lead to high cost. Soft Lithography (SL) offers a new way to print micro/nano structures, which is a fast and low cost alternative to the conventional route, although the high processing temperature of metals, semiconductors and ceramics limits the application SL techniques. In this paper we report the use of Ag nanoparticles as building blocks to make structures by combing the merits of SL, nanotechnology and laser engineering, which provide a simple additive route with low capital investment. Glassy carbon (GC) was chosen as the material for the rigid master mould, as no release coating is needed for replicating the polydimethylsiloxane (PDMS) mould. GC moulds were machined by a nanosecond-pulsed Yb fibre laser. The machined GC moulds were further cleaned by PDMS and the same fibre laser system to remove the process debris. The master mould was further replicated by PDMS. PDMS replicas with either positive or negative features from the master mould were attainable. A two-step strategy was used to print patterns using PDMS mould and Ag nanoparticle paste. Metal patterns were formed on various substrates, and the PDMS mould was left clean and ready for reuse. The resultant printed patterns were found to be uniform over millimetre range, with negligible residual layer, and the thickness of up to several micrometres. The thermal responses of Ag nanoparticles at various sintering temperatures were investigated. The factors affecting the resolution of printed structures were discussed.

  18. Simultaneous Electrochemical Detection of Dopamine and Ascorbic Acid Using an Iron Oxide/Reduced Graphene Oxide Modified Glassy Carbon Electrode

    PubMed Central

    Peik-See, Teo; Pandikumar, Alagarsamy; Nay-Ming, Huang; Hong-Ngee, Lim; Sulaiman, Yusran

    2014-01-01

    The fabrication of an electrochemical sensor based on an iron oxide/graphene modified glassy carbon electrode (Fe3O4/rGO/GCE) and its simultaneous detection of dopamine (DA) and ascorbic acid (AA) is described here. The Fe3O4/rGO nanocomposite was synthesized via a simple, one step in-situ wet chemical method and characterized by different techniques. The presence of Fe3O4 nanoparticles on the surface of rGO sheets was confirmed by FESEM and TEM images. The electrochemical behavior of Fe3O4/rGO/GCE towards electrocatalytic oxidation of DA was investigated by cyclic voltammetry (CV) and differential pulse voltammetry (DPV) analysis. The electrochemical studies revealed that the Fe3O4/rGO/GCE dramatically increased the current response against the DA, due to the synergistic effect emerged between Fe3O4 and rGO. This implies that Fe3O4/rGO/GCE could exhibit excellent electrocatalytic activity and remarkable electron transfer kinetics towards the oxidation of DA. Moreover, the modified sensor electrode portrayed sensitivity and selectivity for simultaneous determination of AA and DA. The observed DPVs response linearly depends on AA and DA concentration in the range of 1–9 mM and 0.5–100 μM, with correlation coefficients of 0.995 and 0.996, respectively. The detection limit of (S/N = 3) was found to be 0.42 and 0.12 μM for AA and DA, respectively. PMID:25195850

  19. Determination of anthracene on Ag-Au alloy nanoparticles/overoxidized-polypyrrole composite modified glassy carbon electrodes.

    PubMed

    Mailu, Stephen N; Waryo, Tesfaye T; Ndangili, Peter M; Ngece, Fanelwa R; Baleg, Abd A; Baker, Priscilla G; Iwuoha, Emmanuel I

    2010-01-01

    A novel electrochemical sensor for the detection of anthracene was prepared by modifying a glassy carbon electrode (GCE) with over-oxidized polypyrrole (PPyox) and Ag-Au (1:3) bimetallic nanoparticles (Ag-AuNPs). The composite electrode (PPyox/Ag-AuNPs/GCE) was prepared by potentiodynamic polymerization of pyrrole on GCE followed by its overoxidation in 0.1 M NaOH. Ag-Au bimetallic nanoparticles were chemically prepared by the reduction of AgNO(3) and HAuCl(4) using C(6)H(5)O(7)Na(3) as the reducing agent as well as the capping agent and then immobilized on the surface of the PPyox/GCE. The nanoparticles were characterized by UV-visible spectroscopy technique which confirmed the homogeneous formation of the bimetallic alloy nanoparticles. Transmission electron microscopy showed that the synthesized bimetallic nanoparticles were in the range of 20-50 nm. The electrochemical behaviour of anthracene at the PPyox/Ag-AuNPs/GCE with Ag: Au atomic ratio 25:75 (1:3) exhibited a higher electrocatalytic effect compared to that observed when GCE was modified with each constituent of the composite (i.e., PPyox, Ag-AuNPs) and bare GCE. A linear relationship between anodic current and anthracene concentration was attained over the range of 3.0 × 10(-6) to 3.56 × 10(-4) M with a detection limit of 1.69 × 10(-7) M. The proposed method was simple, less time consuming and showed a high sensitivity.

  20. Gold nanoparticles decorated on cobalt porphyrin-modified glassy carbon electrode for the sensitive determination of nitrite ion.

    PubMed

    Muthukumar, Palanisamy; Abraham John, S

    2014-05-01

    The present study reports the electrochemical determination of nitrite ion using citrate-gold nanoparticles (cit-AuNPs) decorated on meso-tetra(para-aminophenyl)porphyrinatocobalt(II) (Co(II)MTpAP) self-assembled glassy carbon electrode (GCE). The decoration of cit-AuNPs on Co(II)MTpAP was achieved with the aid of amine groups present on the surface of the self-assembled monolayer (SAM) of Co(II)MTpAP. The SEM image shows that the cit-AuNPs were densely packed on Co(II)MTpAP. The AuNPs decorated electrode was successfully used for the determination of nitrite ion. The cit-AuNPs decorated electrode not only shifted nitrite ion oxidation potential towards less positive potential but also greatly enhanced its current when compared to bare and Co(II)MTpAP SAM modified electrodes. The amperometric current increases linearly while increasing the concentration of nitrite ion ranging from 0.5×10(-6) to 4.7×10(-3) M and the detection limit was found to be 60 nM (S/N=3). Further, the modified electrode was successfully used to determine nitrite ion in the presence of 200-fold excess of common interferents such as Na+, NO3-, I-, K+, CO3(2-), Ca2+, SO4(2-), NH4+, Cl- and glucose. The practical application of the cit-AuNPs decorated electrode was demonstrated by determining nitrite ion in water samples.

  1. Electrochemical generation of volatile lead species using a cadmium cathode: Comparison with graphite, glassy carbon and platinum cathodes

    NASA Astrophysics Data System (ADS)

    Sáenz, María; Fernández, Lenys; Domínguez, José; Alvarado, José

    2012-05-01

    Working electrodes made out of pyrolytic graphite, glassy carbon, platinum and cadmium were compared for the electrochemical generation of volatile lead species. The same electrolytic cell, using each of the different working electrodes was coupled to an atomic absorption spectrometer and the experimental conditions were optimized in each case, using a univariate approach, to produce the maximum possible amount of volatile lead species. The experiments were focused on the variation of cathode hydrogen overvoltage by the application of a constant current during analysis. Under optimum conditions the performance of the electrochemical hydride generator cell should depend on the cathode material selected due to the different hydrogen overpotential of each material. The lead absorbance signal was taken as a measure of the efficiency of volatile lead species production. Best results were obtained using the Cd cathode, due to its relatively highest hydrogen overpotential, a carrier gas (Ar) flow rate of 55 mL min- 1 an electrolytic current of 0.8 A and a catholyte (HCl) concentration 0.05 mol L- 1. The analytical figures of merit of the method using the Cd electrode were evaluated and the susceptibility of the method to interferences was assessed by its application to the determination of trace amounts of lead in the presence of the most significant interferents. The calibration curve was linear between 0.5 and 15 μg L- 1 Pb. Detection limits and characteristic mass values were 0.21 μg L- 1 and 0.26 μg L- 1 respectively. A bovine liver standard reference material and a spiked urine sample were analyzed to check accuracy.

  2. [Osseontegration of trial implants of carbon fiber reinforced plastics].

    PubMed

    Schreiner, U; Schwarz, M; Scheller, G; Schroeder-Boersch, H; Jani, L

    2000-01-01

    To what extent are carbon fibre-reinforced plastics (CFRP) suitable as an osseous integration surface for implants? CFRP test implants having a plexus-structured, rhombus-structured, and plexus-structured, hydroxyapatite surface were implanted in the femura of mini-plgs. Exposure time lasted 12 weeks. The implants were subjected to a macroradiological, a histological-histomorphometrical, and a fluorescence-microscopical evaluation. One half of the uncoated, plexus-structured implants were not osteointegrated, the other half displayed an osteointegration rate of 11.8% in the spongy area and 29.8% in the cortex layer. The HA-coated test implants showed an osteointegration of 29.5% in the spongiosa and 56.8% in the cortex layer. The rhombus-structured test implants had an osteointegration of 29.2% (spongiosa) and 46.2% (cortex layer). Compared to the osteointegration of metallic, especially titanium surfaces the CFRP surfaces tested by us fared worse, especially the uncoated, plexus-structured surfaces. For this reason we view very critically the use of carbon-fibre reinforced plastics together with the surfaces tested by us as osteointegrating surfaces.

  3. Voltammetric behavior of dopamine at a glassy carbon electrode modified with NiFe(2)O(4) magnetic nanoparticles decorated with multiwall carbon nanotubes.

    PubMed

    Ensafi, Ali A; Arashpour, B; Rezaei, B; Allafchian, Ali R

    2014-06-01

    Voltammetric behavior of dopamine was studied on a glassy carbon electrode (GCE) modified-NiFe(2)O(4) magnetic nanoparticles decorated with multiwall carbon nanotubes. Impedance spectroscopy and cyclic voltammetry were used to characterize the behavior of dopamine at the surface of modified-GCE. The modified electrode showed a synergic effect toward the oxidation of dopamine. The oxidation peak current is increased linearly with the dopamine concentration (at pH7.0) in wide dynamic ranges of 0.05-6.0 and 6.0-100μmolL(-1) with a detection limit of 0.02μmolL(-1), using differential pulse voltammetry. The selectivity of the method was studied and the results showed that the modified electrode is free from interference of organic compounds especially ascorbic acid, uric acid, cysteine and urea. Its applicability in the determination of dopamine in pharmaceutical, urine samples and human blood serum was also evaluated. The proposed electrochemical sensor has appropriate properties such as high selectivity, low detection limit and wide linear dynamic range when compared with that of the previous reported papers for dopamine detection. Copyright © 2014 Elsevier B.V. All rights reserved.

  4. A very low potential electrochemical detection of L-cysteine based on a glassy carbon electrode modified with multi-walled carbon nanotubes/gold nanorods.

    PubMed

    Silva, Francisco de Assis dos Santos; da Silva, Monique Gabriella Angelo; Lima, Phabyanno Rodrigues; Meneghetti, Mario Roberto; Kubota, Lauro Tatsuo; Goulart, Marilia Oliveira Fonseca

    2013-12-15

    A nanohybrid platform built with multi-walled carbon nanotubes and gold nanorods, prepared via a cationic surfactant-containing seed-mediated sequential growth process, in aqueous solution, on a glassy carbon substrate has been successfully developed to be used in the electrocatalytic oxidation of L-cysteine (Cys). The nanohybrid was characterized by transmission electron microscopy, Raman spectroscopy and electrochemical measurements. Cyclic voltammetry results had shown that the modified electrode allows the oxidation of Cys at a very low anodic potential (0.00 V vs. Ag/AgCl). The kinetic constant kcat for the catalytic oxidation of Cys was evaluated by chronoamperometry and provided a value of 5.6×10(4) L mol(-1) s(-1). The sensor presents a linear response range from 5.0 up to 200.0 µmol L(-1), detection limit of 8.25 nmol L(-1) and a sensitivity of 120 nA L µmol(-1). Copyright © 2013 Elsevier B.V. All rights reserved.

  5. Electrochemical determination of estrogenic compound bisphenol F in food packaging using carboxyl functionalized multi-walled carbon nanotubes modified glassy carbon electrode.

    PubMed

    Wang, Xin; Yang, Lijun; Jin, Xudong; Zhang, Lei

    2014-08-15

    A simple and highly sensitive electroanalytical method for the determination of bisphenol F (BPF) was developed, which was carried out on multi-walled carbon nanotubes-COOH (MWCNT-COOH) modified glassy carbon electrode (GCE) using cyclic voltammetry (CV) and differential pulse voltammetry (DPV). The results showed that MWCNT-COOH remarkably enhanced the oxidation of BPF, which improved the anodic peak current of BPF significantly. The mechanism was oxidation of BPF lose electrons on the electrode surface via adsorption-controlled process, electrode reaction is the two electrons/two protons process. Under the optimised conditions, the oxidation peak current was proportional to BPF concentration the range from 0.12 to 6.01 μg mL(-1). The detection limit was 0.11 μg mL(-1) (S/N=3), and the relative standard deviation (R.S.D.) was 3.5% (n=9). Moreover, the MWCNT-COOH/GCE electrode showed good reproducibility, stability and anti-interference. Therefore, the proposed method was successfully applied to determine BPF in food packing and the results were satisfactory. Copyright © 2014 Elsevier Ltd. All rights reserved.

  6. Facile synthesis of β-lactoglobulin-functionalized multi-wall carbon nanotubes and gold nanoparticles on glassy carbon electrode for electrochemical sensing.

    PubMed

    Du, Xin; Miao, Zhiying; Zhang, Di; Fang, Yuxin; Ma, Min; Chen, Qiang

    2014-12-15

    A facile approach was developed for the preparation of nanocomposite based on β-lactoglobulin (BLG)-functionalized multi-wall carbon nanotubes (MWCNTs) and gold nanoparticles (GNPs) for the first time. Owing to the amphipathic nature, BLG can be adopted onto the surface of MWCNTs to form BLG-MWCNTs with uniform dispersion in water. Taking advantage of sulfhydryl groups on BLG-MWCNTs, GNPs were decorated on the BLG-MWCNTs-modified glassy carbon electrode (GCE) by electrodeposition. The nanocomposite was characterized by transmission electron microscopy, scanning electron microscopy and X-ray spectroscopy analysis. Cyclic voltammetry and chronoamperometric method were used to evaluate the electrocatalytic ability of the nanocomposite. Furthermore, a glucose biosensor was developed based on the immobilization of glucose oxidase with cross-linking in the matrix of bovine serum albumin (BSA) on the nanocomposite modified GCE. The resulting biosensor exhibited high sensitivity (3.98 μA mM(-1)), wider linear range (0.025-5.5 mM), low detection limit (1.1 μM at the signal-to-noise ratio of 3) and fast response time (within 7s) for glucose detection. Copyright © 2014 Elsevier B.V. All rights reserved.

  7. Adsorptive anodic stripping differential pulse voltammetric determination of CellCept at Fe3O4 nanoparticles decorated multi-walled carbon nanotubes modified glassy carbon electrode.

    PubMed

    Gholivand, Mohammad Bagher; Solgi, Mohammad

    2017-03-01

    A simple and sensitive method based on adsorptive anodic stripping differential pulse voltammetry (AASDPV) for the determination of cellcept, using a magnetic Fe3O4 nanoparticles and functionalized (carboxylated) multi-walled carbon nanotubes modified glassy carbon electrode (f-MWCNs/Fe3O4/GCE) was developed. In phosphate buffer solution (pH = 5), the voltammogram of cellcept exhibited tow anodic peaks and the well-defined peak at about 0.611 V vs SCE was used for its monitoring. The modified electrode was characterized by different methods such as electrochemical impedance spectroscopy (EIS), scanning electron microscopy (SEM) and cyclic voltammetry (CV). The experimental parameters, such as pH, deposition potential and time, as well as scan rate were optimized. Under the optimized conditions, Ip (μA) was proportional to the cellcept concentration in the range of 0.05-200 μM (R(2) = 0.9989) with a detection limit of 9.0 nM and limit of quantification of 30.2 nM. The recovery was >98%. The practical analytical utilities of the modified electrode were demonstrated by the determination of cellcept in human urine and blood serum samples. Modified electrode showed an adequate sensitivity and stability for evaluated samples. Copyright © 2016 Elsevier Inc. All rights reserved.

  8. Simple flow injection for determination of sulfite by amperometric detection using glassy carbon electrode modified with carbon nanotubes-PDDA-gold nanoparticles.

    PubMed

    Amatatongchai, Maliwan; Sroysee, Wongduan; Chairam, Sanoe; Nacapricha, Duangjai

    2015-02-01

    A new approach is presented for sensitive and selective measurement of sulfite (SO3(2-)) in beverages based on a simple flow injection system with amperometric detection. In this work, the sulfite sensor was a glassy carbon electrode modified with multiwall carbon nanotubes-poly(diallyldimethylammonium chloride)-gold nanoparticles composites (CNTs-PDDA-AuNPs/GC). Electrochemical oxidation of sulfite with this electrode was first studied in 0.1M phosphate buffer (pH 7.0) using cyclic voltammetry. The results indicated that the CNTs-PDDA-AuNPs/GC electrode possesses electrocatalytic activity for the oxidation of sulfite with high sensitivity and selectivity. Sulfite was quantified using amperometric measurement with the new sensor at +0.4V vs Ag/AgCl in conjunction with flow injection. The linear working range for the quantitation of sulfite was 2-200 mg L(-1) (r(2)=0.998) with a detection limit of 0.03 mg L(-1) (3σ of blank) and an estimated precision of 1.5%.The proposed method was successfully applied to the determination of sulfite in fruit juices and wines with a sample throughput of 23 samples per hour.

  9. Modification of glassy carbon electrode with a bilayer of multiwalled carbon nanotube/tiron-doped polypyrrole: Application to sensitive voltammetric determination of acyclovir.

    PubMed

    Shahrokhian, Saeed; Azimzadeh, Mahnaz; Amini, Mohammad K

    2015-08-01

    A novel voltammetric sensor based on glassy carbon electrode (GCE) modified with a thin film of multi-walled carbon nanotubes (MWCNTs) coated with an electropolymerized layer of tiron-doped polypyrrole was developed and the resulting electrode was applied for the determination of acyclovir (ACV). The surface morphology and property of the modified electrode were characterized by field emission scanning electron microscopy and electrochemical impedance spectroscopy techniques. The electrochemical performance of the modified electrode was investigated by means of linear sweep voltammetry (LSV). The effect of several experimental variables, such as pH of the supporting electrolyte, drop size of the cast MWCNTssuspension, number of electropolymerization cycles and accumulation time was optimized by monitoring the LSV response of the modified electrode toward ACV. The best response was observed at pH7.0 after accumulation at open circuit for 160 s. Under the optimized conditions, a significant electrochemical improvement was observed toward the electrooxidation of ACV on the modified electrode surface relative to the bare GCE, resulting in a wide linear dynamic range (0.03-10.0μ M) and a low detection limit (10.0 nM) for ACV. Besides high sensitivity, the sensor represented high stability and good reproducibility for ACV analysis, and provided satisfactory results for the determination of this compound in pharmaceutical and clinical preparations. Copyright © 2015 Elsevier B.V. All rights reserved.

  10. Highly sensitive amperometric sensor for micromolar detection of trichloroacetic acid based on multiwalled carbon nanotubes and Fe(II)-phtalocyanine modified glassy carbon electrode.

    PubMed

    Kurd, Masoumeh; Salimi, Abdollah; Hallaj, Rahman

    2013-04-01

    A highly sensitive electrochemical sensor for the detection of trichloroacetic acid (TCA) is developed by subsequent immobilization of phthalocyanine (Pc) and Fe(II) onto multiwalled carbon nanotubes (MWCNTs) modified glassy carbon (GC) electrode. The GC/MWCNTs/Pc/Fe(II) electrode showed a pair of well-defined and nearly reversible redox couple correspondent to (Fe(III)Pc/Fe(II)Pc) with surface-confined characteristics. The surface coverage (Γ) and heterogeneous electron transfer rate constant (ks) of immobilized Fe(II)-Pc were calculated as 1.26×10(-10) mol cm(-2) and 28.13 s(-1), respectively. Excellent electrocatalytic activity of the proposed GC/MWCNTs/Pc/Fe(II) system toward TCA reduction has been indicated and the three consequent irreversible peaks for electroreduction of CCl3COOH to CH3COOH have been clearly seen. The observed chronoamperometric currents are linearly increased with the concentration of TCA at concentration range up to 20mM. Detection limit and sensitivity of the modified electrode were 2.0 μM and 0.10 μA μM(-1) cm(-2), respectively. The applicability of the sensor for TCA detection in real samples was tested. The obtained results suggest that the proposed system can serve as a promising electrochemical platform for TCA detection.

  11. Determination of serotonin on a glassy carbon electrode modified by electropolymerization of meso-tetrakis(2-aminophenyl)porphyrin and single walled carbon nanotubes.

    PubMed

    Kim, Seul Ki; Ahmed, Mohammad Shamsuddin; Jeong, Haesang; You, Jung-Min; Jeon, Seungwon

    2011-03-01

    A chemically modified electrode [poly(TAPP)-SWNT/GCE] was prepared by electropolymerization of meso-tetrakis(2-aminophenyl)porphyrin (TAPP)-single walled carbon nanotubes (SWNT) on the surface of a glassy carbon electrode (GCE). This modified electrode was employed as an electrochemical biosensor for the determination of serotonin concentration and exhibited a typical enhance effect on the current response of serotonin and lower oxidation overpotential. The biosensor was very effective to determined 5-HT in a mixture. The linear response was in the range 2.0 x 10(-7) to 1.0 x 10(-5) M, with a correlation coefficient of 0.999 [i(p)(microA) = 3.406 C (microM)+0.132] on the anodic current, with a detection limit of 1 x 10(-9) M. Due to the relatively low currents and different potentials in the electrochemical responses to ascorbic acid and dopamine, the modified electrode is a useful and effective sensing device for the selective and sensitive serotonin determination in the presence of ascorbic acid and dopamine.

  12. Pd-Au nanoparticle decorated carbon nanotube as a sensing layer on the surface of glassy carbon electrode for electrochemical determination of ceftazidime.

    PubMed

    Shahrokhian, Saeed; Salimian, Razieh; Rastgar, Shokoufeh

    2014-01-01

    A simple electrodeposition method is employed to construct a thin film modifier of palladium-gold nanoparticles (Pd-AuNPs) decorated multi-walled carbon nanotube (MWCNT) on the surface of glassy carbon electrode (GCE). Morphology and property of Pd-AuNPs-MWCNT have been examined by scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS). Electrochemical performance of Pd-AuNPs-MWCNT/GCE for detection of ceftazidime (CFZ) has been investigated by cyclic voltammetry (CV). This nanostructured film modified electrode effectively exhibited enhanced properties for detection of ceftazidime (CFZ). The effects of various experimental variables such as, the amount of casted MWCNT, time and potential of deposition of metal nanoparticles and the pH of the buffered solution on the electrode response are optimized. The proposed electrode showed a linear dynamic range of 0.05-50μM and the detection limit of 1nM for the CFZ. The modified electrode successfully supports the sensitive detection of trace amounts of the CFZ in pharmaceutical and clinical preparations.

  13. An electrochemical sensor for rizatriptan benzoate determination using Fe3O4 nanoparticle/multiwall carbon nanotube-modified glassy carbon electrode in real samples.

    PubMed

    Madrakian, Tayyebeh; Maleki, Somayeh; Heidari, Mozhgan; Afkhami, Abbas

    2016-06-01

    In this paper a sensitive and selective electrochemical sensor for determination of rizatriptan benzoate (RZB) was proposed. A glassy carbon electrode was modified with nanocomposite of multiwalled carbon nanotubes (MWCNTs) and Fe3O4 nanoparticles (Fe3O4/MWCNTs/GCE). The results obtained clearly show that the combination of MWCNTs and Fe3O4 nanoparticles definitely improves the sensitivity of modified electrode to RZB determination. The morphology and electroanalytical performance of the fabricated sensor were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), energy dispersive X-ray spectroscopy (EDS), square wave voltammetry (SWV) and cyclic voltammetry (CV). Also, the effect of experimental and instrumental parameters on the sensor response was evaluated. The square wave voltammetric response of the electrode to RZB was linear in the range 0.5-100.0 μmol L(-1) with a detection limit of 0.09 μmol L(-1) under the optimum conditions. The investigated method showed good stability, reproducibility and repeatability. The proposed sensor was successfully applied for real life samples of blood serum and RZB determination in pharmaceutical.

  14. Electrocatalytic oxidation and selective determination of an opioid analgesic methadone in the presence of acetaminophen at a glassy carbon electrode modified with functionalized multi-walled carbon nanotubes: application for human urine, saliva and pharmaceutical samples analysis.

    PubMed

    Amiri-Aref, Mohaddeseh; Raoof, Jahan Bakhsh; Ojani, Reza

    2013-09-01

    For the first time, electrocatalytic oxidation and selective determination of methadone (Mtd), as a long-acting opioid, in the presence of acetaminophen (Ac) has been investigated at a glassy carbon electrode modified with functionalized multi-walled carbon nanotubes. This simple and sensitive electrochemical sensor was fabricated through the drop-casting of functionalized multi-walled carbon nanotubes (fMWCNT) on the surface of a glassy carbon electrode (GCE). The electrocatalytic oxidations of Ac and Mtd are both individually and simultaneously investigated at the surface of the fMWCNT modified glassy carbon electrode (fMWCNT/MGCE) through using cyclic and differential pulse voltammetric studies. The fMWCNT/MGCE offered a considerable enhancement in the anodic peak current of Ac and Mtd associated with separating their overlapping voltammetric responses with potential difference of 290 mV. The catalytic peak currents obtained from differential pulse voltammetry of Ac and Mtd increased linearly with their concentration at the ranges of 0.45-90.0 μM and 0.5-100.0 μM, respectively, and the detection limits for Ac and Mtd were sequentially 0.35 μM and 0.28 μM. Furthermore, this electrochemical sensor was successfully implemented for the quantitative determination of Ac and Mtd in human urine, saliva and pharmaceutical samples using standard addition method and the obtained results were found to be satisfactory. Copyright © 2013 Elsevier B.V. All rights reserved.

  15. Surface functionalization of glassy carbon electrodes via adsorption, electrografting and click chemistry using quantum dots and alkynyl substituted phthalocyanines: a brief review

    NASA Astrophysics Data System (ADS)

    Nxele, Siphesihle Robin; Mashazi, Philani; Nyokong, Tebello

    2016-02-01

    In this work, glassy carbon electrodes are functionalised with alkynyl substituted phthalocyanines via electrografting and click chemistry as well as with quantum dots (QDs)-phthalocyanine conjugates via adsorption. The use of click chemistry and the addition of QDs is to try observe improvements in the electrocatalytic behaviour of electrocatalyst compared to similar electrocatalysts in literature. The electrografting and click chemistry methods provide greater molecule stability on the substrate surface due to the covalent bonds formed. Results show that these methods of electrode fabrication do improve the functionality of the electrocatalysts.

  16. Highly Sensitive Detection of Arsenite Based on Its Affinity toward Ruthenium Nanoparticles Decorated on Glassy Carbon Electrode.

    PubMed

    Gupta, Ruma; Gamare, Jayashree S; Pandey, Ashok K; Tyagi, Deepak; Kamat, Jayshree V

    2016-02-16

    Metallic ruthenium nanoparticles (Ru NPs) are formed on the glassy carbon electrode (GC) at electrodeposition potential of -0.75 V, as observed from X-ray photoelectron spectroscopy. Thus formed Ru NPs have the arsenite selective surface and conducting core that is ideally suited for designing a highly sensitive and reproducible response generating matrix for the arsenite detection at an ultratrace concentration in aqueous matrices. Contrary to this, arsenate ions sorb via chemical interactions on the ruthenium oxide (RuO2 and RuO3) NPs formed at -0.25 V, but not on the Ru NPs. For exploring a possibility of the quantification of arsenite in the ultratrace concentration range, the Ru NPs have been deposited on the GC by a potentiostatic pulse method of electrodeposition at optimized -0.75 V for 1000 s. Arsenite preconcentrates onto the Ru surface just by dipping the RuNPs/GC into the arsenite solution as it interacts chemically with Ru NPs. Electrochemical impedance spectroscopy of As(III) loaded RuNPs/GC shows a linear increase in the charge transfer resistance with an increase in As(III) conc. Using a differential pulse voltammetric technique, arsenite is oxidized to arsenate leading to its quantitative determination without any interference of Cu(2+) ions that are normally encountered in the water systems. Thus, the use of RuNPs/GC eliminates the need for a preconcentration step in stripping voltammetry, which requires optimization of the parameters like preconcentration potential, time, stirring, inferences, and so on. The RuNPs/GC based differential pulse voltammetric (DPV) technique can determine the concentration of arsenite in a few min with a detection limit of 0.1 ppb and 5.4% reproducibility. The sensitivity of 2.38 nA ppb(-1) obtained in the present work for As(III) quantification is considerably better than that reported in the literature, with a similar detection limit and mild conditions (pH = 2). The RuNPs/GC based DPV has been evaluated for its

  17. Phosphorous transient enhanced diffusion suppression and activation enhancement with cluster carbon co-implantation

    SciTech Connect

    Nakashima, Yoshiki; Hamamoto, Nariaki; Nagayama, Tsutomu; Koga, Yuji; Umisedo, Sei; Kawamura, Yasunori; Hashimoto, Masahiro; Onoda, Hiroshi

    2012-11-06

    Carbon co-implantation is well known as an effective method for suppressing boron/phosphorous transient enhanced diffusion (TED). Germanium pre-amorphization implantation (PAI) is usually applied prior to carbon co-implantation for suppressing channeling tail of dopants. In this study, cluster carbon was applied instead of the combination of germanium PAI and monomer carbon co-implantation prior to phosphorous implantation. Dependence of phosphorous activation and TED on amorphous layer thickness, carbon dose, carbon distribution and substrate temperature have been investigated. Cluster carbon implantation enables thick amorphous layer formation and TED suppression at the same time and low temperature implantation enhances the ability of amorphous layer formation so that shallow junction and low Rs can be achieved without Ge implantation.

  18. Multi-walled Carbon Nanotubes/Graphite Nanosheets Modified Glassy Carbon Electrode for the Simultaneous Determination of Acetaminophen and Dopamine.

    PubMed

    Zhang, Susu; He, Ping; Zhang, Guangli; Lei, Wen; He, Huichao

    2015-01-01

    Graphite nanosheets prepared by thermal expansion and successive sonication were utilized for the construction of a multi-walled carbon nanotubes/graphite nanosheets based amperometric sensing platform to simultaneously determine acetaminophen and dopamine in the presence of ascorbic acid in physiological conditions. The synergistic effect of multi-walled carbon nanotubes and graphite nanosheets catalyzed the electrooxidation of acetaminophen and dopamine, leading to a remarkable potential difference up to 200 mV. The as-prepared modified electrode exhibited linear responses to acetaminophen and dopamine in the concentration ranges of 2.0 × 10(-6) - 2.4 × 10(-4) M (R = 0.999) and 2.0 × 10(-6) - 2.0 × 10(-4) M (R = 0.998), respectively. The detection limits were down to 2.3 × 10(-7) M for acetaminophen and 3.5 × 10(-7) M for dopamine (S/N = 3). Based on the simple preparation and prominent electrochemical properties, the obtained multi-walled carbon nanotubes/graphite nanosheets modified electrode would be a good candidate for the determination of acetaminophen and dopamine without the interference of ascorbic acid.

  19. [Biodegradation of tracheal carbon implant in animal experiment].

    PubMed

    Scierski, Wojciech; Namysłowski, Grzegorz; Nozyński, Jerzy; Turecka, Lucyna; Misiołek, Maciej; Czecior, Eugeniusz; Lisowska, Grazyna; Mrówka-Kata, Katarzyna

    2008-01-01

    The radical treatment of tracheal stenosis comprises segmental resection and its reconstruction. The most successful type of reconstruction is the "end to end" technique. In cases with large tracheal defects (over 6 cm) this kind of reconstruction is impossible. From many years the adequate biomaterial is searched for the tracheal reconstruction. Most of the implanted biomaterials undergo biodegradation process. The aim of the study was to analyze the biodegradation process in carbon fibers of prosthesis implanted in tracheal defects in animal experiment. We studied the prosthesis implanted in tracheal defects in sheep. The prosthesis were built with composite biomaterial composed of carbon fibers and polisulfone. The observation period was 1, 2, 3, 4, 6, 8, 24 and 38 weeks. In the morphometric evaluations the breadth, curve width, fullness factor and mean grey level of carbon fibers were assessed. The results showed that carbon fibers undergo progressively degradation in animal environment. The width gradually decreased. The mean grey level in the first three weeks decreased, but in the next period it increased. Conclusion. The carbon fibers of segmental tracheal prosthesis undergo gradually degradation process in biological environment expressed by decreasing of their dimensions connected with the lost of irregularities and changes of structure density.

  20. A disposable electrochemical immunosensor for carcinoembryonic antigen based on nano-Au/multi-walled carbon nanotubes-chitosans nanocomposite film modified glassy carbon electrode.

    PubMed

    Huang, Ke-Jing; Niu, De-Jun; Xie, Wan-Zhen; Wang, Wei

    2010-02-05

    In this paper, a disposable electrochemical immunosensor for the detection of carcinoembryonic antigen (CEA) based on Au nanoparticles (AuNPs)/multi-walled carbon nanotubes (MWCNTs)-chitosans (Chits) composite film was developed. MWCNTs-Chits homogeneous composite was first dispersed in acetic acid solution and then the AuNPs was in situ synthesized at the composite. The mixture was dripped on the glassy carbon electrode (GCE) and then CEA antibody (anti-CEA) was immobilized on the resulted modified electrode to construct the immunosensor. The stepwise assembly process of the immunosensor was characterized by means of cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). CV and differential pulse voltammetry (DPV) studies demonstrated that the formation of antibody-antigen complexes decreased peak current of [Fe(CN)(6)](3-/4-) redox pair at the AuNPs/MWCNTs-Chits/GCE. The optimization of the pH of supporting electrolyte, the incubation temperature and time were studied in detail. Under optimal conditions, the peak current of DPV of the immunosensor decreased linearly with increasing CEA concentration in two ranges of 0.3-2.5 and 2.5-20 ng mL(-1), with a detection limit of 0.01 ng mL(-1) (S/N=3). This electrochemical immunoassay combines the specificity of the immunological reaction with the sensitivity of the AuNPs and MWCNTs amplified electrochemical detection. It would be valuable for diagnosis and monitoring of carcinoma. Copyright 2009 Elsevier B.V. All rights reserved.

  1. Simple flow injection for screening of total antioxidant capacity by amperometric detection of DPPH radical on carbon nanotube modified-glassy carbon electrode.

    PubMed

    Amatatongchai, M; Laosing, S; Chailapakul, O; Nacapricha, D

    2012-08-15

    An amperometric flow injection (FI) method suitable for evaluation of 'total antioxidant capacity' (TAC) is presented. In this method, a carrier stream of a solution of 2,2-diphenyl-1-picrylhydrazyl radical (DPPH(•)) continuously flows through an electrochemical cell, furnished with a carbon nanotube modified-glassy carbon electrode (CNT/GC) as the working electrode. At the applied voltage of 0.05V (vs. Ag/AgCl), DPPH(•) is reduced resulting in a constant electric current. For measurement of the TAC, a sample zone containing antioxidant(s) is injected into the carrier stream therein reduction reaction of DPPH(•) occurring within the sample zone. The decreased amount of the radical in the sample zone leads to a drop of the amperometric signal at the CNT/GC electrode. We have also compared the performance of the CNT/GC electrode to the unmodified GC electrode using cyclic voltammetry. The sensitivity of the CNT/GC electrode was more than twenty five times greater than the bare GC electrode. The study of the sweep rate dependence showed that the cathodic and anodic current of 0.1mM DPPH solution varied linearly (r(2)=0.998) with the square root of the scan rate, from 0.02 to 0.12 Vs(-1). These results demonstrated that the CNT/GC electrode is appropriate for the quantitation of antioxidants via amperometric detection of the residual concentration of non-reacted DPPH(•). We obtained linear calibrations for all the antioxidants tested including gallic acid, catechin, quercetin, caffeic acid and Trolox. The system offers rapid sample throughput (45 samples h(-1)) and good precision of 3.2% R.S.D., for 20 μL-injection of 2.5 μM Trolox (n=30). This method was applied to evaluate the TAC of extracts of some Thai indigenous vegetables.

  2. Trace level voltammetric determination of lead and cadmium in sediment pore water by a bismuth-oxychloride particle-multiwalled carbon nanotube composite modified glassy carbon electrode.

    PubMed

    Cerovac, Sandra; Guzsvány, Valéria; Kónya, Zoltán; Ashrafi, Amir M; Švancara, Ivan; Rončević, Srđan; Kukovecz, Ákos; Dalmacija, Božo; Vytřas, Karel

    2015-03-01

    Two multiwalled carbon nanotubes-based composites modified with bismuth and bismuth-oxychloride particles were synthesized and attached to the glassy carbon electrode substrate. The resultant configurations, Bi/MWCNT-GCE and BiOCl/MWNT-GCE, were then characterized with respect to their physicochemical properties and electroanalytical performance in combination with square-wave anodic stripping voltammetry (SWASV). Further, some key experimental conditions and instrumental parameters were optimized; namely: the supporting electrolyte composition, accumulation potential and time, together with the parameters of the SWV-ramp. The respective method with both electrode configurations has then been examined for the trace level determination of Pb(2+) and Cd(2+) ions and the results compared to those obtained with classical bismuth-film modified GCE. The different intensities of analytical signals obtained at the three electrodes for Pb(2+) and Cd(2+) vs. the saturated calomel reference electrode had indicated that the nature of the modifiers and the choice of the supporting electrolyte influenced significantly the corresponding stripping signals. The most promising procedure involved the BiOCl/MWCNT-GCE and the acetate buffer (pH 4.0) offering limits of determination of 4.0 μg L(-1) Cd(2+) and 1.9 μg L(-1) Pb(2+) when accumulating for 120 s at a potential of -1.20 V vs. ref. The BiOCl/MWCNT electrode was tested for the determination of target ions in the pore water of a selected sediment sample and the results agreed well with those obtained by graphite furnace atomic absorption spectrometry.

  3. Simultaneous determination of mycophenolate mofetil and its active metabolite, mycophenolic acid, by differential pulse voltammetry using multi-walled carbon nanotubes modified glassy carbon electrode.

    PubMed

    Madrakian, Tayyebeh; Soleimani, Mohammad; Afkhami, Abbas

    2014-09-01

    A highly sensitive electrochemical sensor for the simultaneous determination of mycophenolate mofetil (MPM) and mycophenolic acid (MPA) was fabricated by multi-walled carbon nanotubes modified glassy carbon electrode (MWCNTs/GCE). The electrochemical behavior of these two drugs was studied at the modified electrode using cyclic voltammetry and adsorptive differential pulse voltammetry. MPM and MPA were oxidized at the GCE during an irreversible process. DPV analysis showed two oxidation peaks at 0.87V and 1.1V vs. Ag/AgCl for MPM and an oxidation peak at 0.87V vs. Ag/AgCl for MPA in phosphate buffer solution of pH5.0. The MWCNTs/GCE displayed excellent electrochemical activities toward oxidation of MPM and MPA relative to the bare GCE. The experimental design algorithm was used for optimization of DPV parameters. The electrode represents linear responses in the range 5.0×10(-6) to 1.6×10(-4)molL(-1) and 2.5×10(-6)molL(-1) to 6.0×10(-5)molL(-1) for MPM and MPA, respectively. The detection limit was found to be 9.0×10(-7)molL(-1) and 4.0×10(-7)molL(-1) for MPM and MPA, respectively. The modified electrode showed a good sensitivity and stability. It was successfully applied to the simultaneous determination of MPM and MPA in plasma and urine samples.

  4. Determination of beta-carboline alkaloids in foods and beverages by high-performance liquid chromatography with electrochemical detection at a glassy carbon electrode modified with carbon nanotubes.

    PubMed

    Agüí, Lourdes; Peña-Farfal, Carlos; Yáñez-Sedeño, Paloma; Pingarrón, José M

    2007-03-07

    Simple and sensitive methods for the separation and quantification of beta-carboline alkaloids in foods and beverages by HPLC with electrochemical detection at carbon nanotubes-modified glassy carbon electrodes (CNTs-GCE) are reported. Electrode modification with multi-wall CNTs produced an improved amperometric response to beta-carbolines, in spite of the working medium consisting of methanol:acetonitrile: 0.05 mol L(-1) Na(2)HPO(4) solution of pH 9.0 (20:20:60). On the contrary to that observed at a bare GCE, a good repeatability of the amperometric measurements carried out at +900 mV versus Ag/AgCl (R.S.D. of 3.2% for i(p), n=20) was achieved at the CNTs-GCE. Using an Ultrabase C(18) column and isocratic elution with the above mentioned mobile phase, a complete resolution of the chromatographic peaks for harmalol, harmaline, norharmane, harmane and harmine, was achieved. Calibration graphs over the 0.25-100 microM range with detection limits ranging between 4 and 19 ng mL(-1), were obtained. The HPLC-ED at CNTs-GCE method was applied to the analysis of beer, coffee and cheese samples, spiked with beta-carbolines at concentration levels corresponding to those may be found in the respective samples. The steps involved in sample treatment, such as extraction and clean-up, were optimized for each type of sample. Recoveries ranging between 92 and 102% for beer, 92 and 101% for coffee, and 88 and 100% for cheese, at sub-microg mL(-1) or g(-1) analytes concentration levels were achieved.

  5. A joint experimental and computational search for authentic nano-electrocatalytic effects: electrooxidation of nitrite and L-ascorbate on gold nanoparticle-modified glassy carbon electrodes.

    PubMed

    Wang, Ying; Ward, Kristopher R; Laborda, Eduardo; Salter, Chris; Crossley, Alison; Jacobs, Robert M J; Compton, Richard G

    2013-02-11

    The investigation of electrocatalytic nanoeffects is tackled via joint electrochemical measurements and computational simulations. The cyclic voltammetry of electrodes modified with metal nanoparticles is modeled considering the kinetics of the electrochemical process on the bulk materials of the different regions of the electrode, that is, the substrate (glassy carbon) and the nanoparticles (gold). Comparison of experimental and theoretical results enables the detection of changes in the electrode kinetics at the nanoscale due to structural and/or electronic effects. This approach is applied to the experimental assessment of electrocatalytic effects by gold nanoparticles (Au NPs) in the electrooxidation of nitrite and L-ascorbate. Glassy carbon electrode is modified with Au NPs via seed-mediated growth method. Divergence between the kinetics of these processes on gold macroelectrodes and gold nanoparticles is examined. Whereas claimed catalytic effects are not observed in the electrooxidation of nitrite, electrocatalytic nanoeffects are verified in the case of L-ascorbate. This is probably due to that the electron transfer process follows an adsorptive mechanism. The combination of simulation with experiments is commended as a general strategy of authentification, or not, of nanoelectrocatalytic effects. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. The electrode as organolithium reagent: catalyst-free covalent attachment of electrochemically active species to an azide-terminated glassy carbon electrode surface.

    PubMed

    Das, Atanu K; Engelhard, Mark H; Liu, Fei; Bullock, R Morris; Roberts, John A S

    2013-12-02

    The reaction of a lithium acetylide-ethylenediamine complex with azide-terminated glassy carbon surfaces affords 1,2,3-triazolyllithium surface groups that are active toward covalent C-C coupling reactions, including salt metathesis with an aliphatic halide and nucleophilic addition at an aldehyde. Surface ferrocenyl groups were introduced by reaction with (6-iodohexyl)ferrocene; the voltammetry of electrode samples shows narrow, symmetric peaks indicating uniform attachment. X-ray photoelectron and reflectance infrared spectroscopic data provide further support for the surface-attached products. Formation of the 1,2,3-triazolyllithium linkage requires neither a catalyst nor a strained alkyne. Coverages obtained by this route are similar to those obtained by the more common Cu(I)-catalyzed alkyne-azide coupling (CuAAC) of ethynylferrocene with surface azides. Preconditioning of the glassy carbon disk electrodes at ambient temperature under nitrogen affords coverages comparable to those reported with preconditioning at 1000 °C under hydrogen/nitrogen.

  7. Electrochemical sensing of doxorubicin in unprocessed whole blood, cell lysate, and human plasma samples using thin film of poly-arginine modified glassy carbon electrode.

    PubMed

    Soleymani, Jafar; Hasanzadeh, Mohammad; Eskandani, Morteza; Khoubnasabjafari, Maryam; Shadjou, Nasrin; Jouyban, Abolghasem

    2017-08-01

    A thin film of poly-arginine fabricated on glassy carbon electrode by one step electrodeposition method is applied for detection of doxorubicin hydrochloride in whole blood, cell lysate, and untreated-plasma samples. Cyclic voltammetry results indicated that the doxorubicin is oxidized via two electrons and two protons at physiological pH (pH=7.4) using poly-arginine thin film modified glassy carbon. More importantly, electrostatic repulsion takes place between the prepared polymer film-modified electrode and selected drug resulting in the signal amplification on oxidation of doxorubicin and lowering its over potential and thereby selective detection of doxorubicin in real samples. The apparent electron transfer rate constant and transfer coefficient were determined by cyclic voltammetry and were approximately 10.1s(-1) and 0.82, respectively. Also, using differential-pulse voltammetric technique for sensitive detection of doxorubicin in whole blood and plasma samples, the lower limit of quantification was 69nM and 103nM, respectively. Also, application of this amino acid based biocompatible polymeric electrode was tested to the determination of doxorubicin in unprocessed whole blood and the results show that this sensor could be applied in online and real time monitoring of this anti-cancer drug in real samples which is important for clinical research. Copyright © 2017. Published by Elsevier B.V.

  8. Suppression of oxidation enhanced boron diffusion in silicon by carbon implantation and characterization of MOSFETs with carbon implanted channels

    SciTech Connect

    Ban, I.; Oeztuerk, M.C.; Demirlioglu, E.

    1996-12-31

    Scaling of MOSFETs into the deep submicron regime requires shallow doping profiles with abrupt doping transitions in the MOSFET active region. In NMOS transistors with boron doped channels, oxidation enhanced diffusion is a key contributor to boron profile broadening. Starting from the arguments presented in several recent reports on the role of carbon in silicon as a sink for self-interstitials, we have explored the feasibility of using carbon in the MOSFET in the active region to retard boron diffusion during gate oxidation. MOSFETs with carbon and boron implanted channels have been fabricated. Boron diffusion, activation, and critical electrical parameters such as subthreshold swing, threshold voltage, and off-state leakage current have been evaluated as a function of the carbon dose. We have shown that carbon can effectively suppress boron diffusion during gate oxidation. However, at dose levels around 10{sup 14}cm{sup -2} carbon results in poor boron activation and degradation in MOSFET performance.

  9. Simultaneous electrochemical determination of dopamine and paracetamol on multiwalled carbon nanotubes/graphene oxide nanocomposite-modified glassy carbon electrode.

    PubMed

    Cheemalapati, Srikanth; Palanisamy, Selvakumar; Mani, Veerappan; Chen, Shen-Ming

    2013-12-15

    In the present study, multiwalled carbon nanotubes (MWCNT)/graphene oxide (GO) nanocomposite was prepared by homogenous dispersion of MWCNT and GO and used for the simultaneous voltammetric determination of dopamine (DA) and paracetamol (PA). The TEM results confirmed that MWCNT walls were wrapped well with GO sheets. The MWCNT/GO nanocomposite showed superior electrocatalytic activity towards the oxidation of DA and PA, when compared with either pristine MWCNT or GO. The major reason for the efficient simultaneous detection of DA and PA at nanocomposite was the synergistic effect between MWCNT and GO. The electrochemical oxidation of DA and PA was investigated by cyclic voltammetry, differential pulse voltammetry and amperometry. The nanocomposite modified electrode showed electrocatalytic oxidation of DA and PA in the linear response range from 0.2 to 400 µmol L(-1) and 0.5 to 400 µmol L(-1) with the detection limit of 22 nmol L(-1) and 47 nmol L(-1) respectively. The proposed sensor displayed good selectivity, sensitivity, stability with appreciable consistency and precision.

  10. Comparison of impedimetric detection of DNA hybridization on the various biosensors based on modified glassy carbon electrodes with PANHS and nanomaterials of RGO and MWCNTs.

    PubMed

    Benvidi, Ali; Tezerjani, Marzieh Dehghan; Jahanbani, Shahriar; Mazloum Ardakani, Mohammad; Moshtaghioun, Seyed Mohammad

    2016-01-15

    In this research, we have developed lable free DNA biosensors based on modified glassy carbon electrodes (GCE) with reduced graphene oxide (RGO) and carbon nanotubes (MWCNTs) for detection of DNA sequences. This paper compares the detection of BRCA1 5382insC mutation using independent glassy carbon electrodes (GCE) modified with RGO and MWCNTs. A probe (BRCA1 5382insC mutation detection (ssDNA)) was then immobilized on the modified electrodes for a specific time. The immobilization of the probe and its hybridization with the target DNA (Complementary DNA) were performed under optimum conditions using different electrochemical techniques such as cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). The proposed biosensors were used for determination of complementary DNA sequences. The non-modified DNA biosensor (1-pyrenebutyric acid-N- hydroxysuccinimide ester (PANHS)/GCE), revealed a linear relationship between ∆Rct and logarithm of the complementary target DNA concentration ranging from 1.0×10(-16)molL(-1) to 1.0×10(-10)mol L(-1) with a correlation coefficient of 0.992, for DNA biosensors modified with multi-wall carbon nanotubes (MWCNTs) and reduced graphene oxide (RGO) wider linear range and lower detection limit were obtained. For ssDNA/PANHS/MWCNTs/GCE a linear range 1.0×10(-17)mol L(-1)-1.0×10(-10)mol L(-1) with a correlation coefficient of 0.993 and for ssDNA/PANHS/RGO/GCE a linear range from 1.0×10(-18)mol L(-1) to 1.0×10(-10)mol L(-1) with a correlation coefficient of 0.985 were obtained. In addition, the mentioned biosensors were satisfactorily applied for discriminating of complementary sequences from noncomplementary sequences, so the mentioned biosensors can be used for the detection of BRCA1-associated breast cancer. Copyright © 2015. Published by Elsevier B.V.

  11. Electrocatalytic oxidation of 2-mercaptoethanol using modified glassy carbon electrode by MWCNT in combination with unsymmetrical manganese (II) Schiff base complexes

    SciTech Connect

    Mohebbi, Sajjad Eslami, Saadat

    2015-06-15

    Highlights: • High electocatalytic efficiency and stability of modified hybrid electrode GC/MWCNTs/MnSaloph. • Direct reflection of catalytic activity of manganese complexes on electrocatalytic oxidation of 2-ME. • Decreasing overpotential and increasing catalytic peak current toward oxidation of 2-ME. • Deposition of range of novel substituted N{sub 2}O{sub 2} Saloph complexes of manganese(II) on GCE/MWCNT. • Enhancement of electrocatalytic oxidation activity upon electron donating substitutions on the Saloph. - Abstract: The performance of modified hybrid glassy carbon electrode with composite of carbon nanotubes and manganese complexes for the electrocatalytic oxidation of 2-mercaptoethanol is developed. GC electrode was modified using MWCNT and new N{sub 2}O{sub 2} unsymmetrical tetradentate Schiff base complexes of manganese namely Manganese Saloph complexes 1-5, with general formula Mn[(5-x-4-y-Sal)(5-x′-4-y′-Sal) Ph], where x, x′ = H, Br, NO{sub 2} and y, y′ = H, MeO. Direct immobilization of CNT on the surface of GCE is performed by abrasive immobilization, and then modified by manganese(II) complexes via direct deposition method. These novel modified electrodes clearly demonstrate the necessity of modifying bare carbon electrodes to endow them with the desired behavior and were identified by HRTEM. Also complexes were characterized by elemental analyses, MS, UV–vis and IR spectroscopy. Modified hybrid GC/MWCNT/MnSaloph electrode exhibits strong and stable electrocatalytic activity towards the electrooxidation of 2-mercaptoethanol molecules in comparison with bare glassy carbon electrode with advantages of very low over potential and high catalytic current. Such ability promotes the thiol’s electron transfer reaction. Also, electron withdrawing substituent on the Saloph was enhanced electrocatalytic oxidation activity.

  12. Enhanced life ion source for germanium and carbon ion implantation

    SciTech Connect

    Hsieh, Tseh-Jen; Colvin, Neil; Kondratenko, Serguei

    2012-11-06

    Germanium and carbon ions represent a significant portion of total ion implantation steps in the process flow. Very often ion source materials that used to produce ions are chemically aggressive, especially at higher temperatures, and result in fast ion source performance degradation and a very limited lifetime [B.S. Freer, et. al., 2002 14th Intl. Conf. on Ion Implantation Technology Proc, IEEE Conf. Proc., p. 420 (2003)]. GeF{sub 4} and CO{sub 2} are commonly used to generate germanium and carbon beams. In the case of GeF{sub 4} controlling the tungsten deposition due to the de-composition of WF{sub 6} (halogen cycle) is critical to ion source life. With CO{sub 2}, the materials oxidation and carbon deposition must be controlled as both will affect cathode thermionic emission and anti-cathode (repeller) efficiencies due to the formation of volatile metal oxides. The improved ion source design Extended Life Source 3 (Eterna ELS3) together with its proprietary co-gas material implementation has demonstrated >300 hours of stable continuous operation when using carbon and germanium ion beams. Optimizing cogas chemistries retard the cathode erosion rate for germanium and carbon minimizes the adverse effects of oxygen when reducing gas is introduced for carbon. The proprietary combination of hardware and co-gas has improved source stability and the results of the hardware and co-gas development are discussed.

  13. Nanotechnology for implantable sensors: carbon nanotubes and graphene in medicine.

    PubMed

    Wujcik, Evan K; Monty, Chelsea N

    2013-01-01

    Implantable sensors utilizing nanotechnology are at the forefront of diagnostic, medical monitoring, and biological technologies. These sensors are often equipped with nanostructured carbon allotropes, such as graphene or carbon nanotubes (CNTs), because of their unique and often enhanced properties over forms of bulk carbon, such as diamond or graphite. Because of these properties, the fundamental and applied research of these carbon nanomaterials have become some of the most cited topics in scientific literature in the past decades. The age of carbon nanomaterials is simply budding, however, and is expected to have a major impact in many areas. These areas include electronics, photonics, plasmonics, energy capture (including batteries, fuel cells, and photovoltaics), and--the emphasis of this review--biosensors and sensor technologies. The following review will discuss future prospects of the two most commonly used carbon allotropes in implantable sensors for nanomedicine and nanobiotechnology, CNTs and graphene. Sufficient further reading and resources have been provided for more in-depth and specific reading that is outside the scope of this general review. Copyright © 2013 Wiley Periodicals, Inc.

  14. Characterization of carbon ion implantation induced graded microstructure and phase transformation in stainless steel

    SciTech Connect

    Feng, Kai; Wang, Yibo; Li, Zhuguo; Chu, Paul K.

    2015-08-15

    Austenitic stainless steel 316L is ion implanted by carbon with implantation fluences of 1.2 × 10{sup 17} ions-cm{sup −} {sup 2}, 2.4 × 10{sup 17} ions-cm{sup −} {sup 2}, and 4.8 × 10{sup 17} ions-cm{sup −} {sup 2}. The ion implantation induced graded microstructure and phase transformation in stainless steel is investigated by X-ray diffraction, X-ray photoelectron spectroscopy and high resolution transmission electron microscopy. The corrosion resistance is evaluated by potentiodynamic test. It is found that the initial phase is austenite with a small amount of ferrite. After low fluence carbon ion implantation, an amorphous layer and ferrite phase enriched region underneath are formed. Nanophase particles precipitate from the amorphous layer due to energy minimization and irradiation at larger ion implantation fluence. The morphology of the precipitated nanophase particles changes from circular to dumbbell-like with increasing implantation fluence. The corrosion resistance of stainless steel is enhanced by the formation of amorphous layer and graphitic solid state carbon after carbon ion implantation. - Highlights: • Carbon implantation leads to phase transformation from austenite to ferrite. • The passive film on SS316L becomes thinner after carbon ion implantation. • An amorphous layer is formed by carbon ion implantation. • Nanophase precipitate from amorphous layer at higher ion implantation fluence. • Corrosion resistance of SS316L is improved by carbon implantation.

  15. In-situ observation of sputtered particles for carbon implanted tungsten during energetic isotope ion implantation

    SciTech Connect

    Oya, Y.; Sato, M.; Uchimura, H.; Okuno, K.; Ashikawa, N.; Sagara, A.; Yoshida, N.; Hatano, Y.

    2015-03-15

    Tungsten is a candidate for plasma facing materials in future fusion reactors. During DT plasma operations, carbon as an impurity will bombard tungsten, leading to the formation of tungsten-carbon (WC) layer and affecting tritium recycling behavior. The effect of carbon implantation for the dynamic recycling of deuterium, which demonstrates tritium recycling, including retention and sputtering, has been investigated using in-situ sputtered particle measurements. The C{sup +} implanted W, WC and HOPG were prepared and dynamic sputtered particles were measured during H{sub 2}{sup +} irradiation. It has been found that the major hydrocarbon species for C{sup +} implanted tungsten is CH{sub 3}, while for WC and HOPG (Highly Oriented Pyrolytic Graphite) it is CH{sub 4}. The chemical state of hydrocarbon is controlled by the H concentration in a W-C mixed layer. The amount of C-H bond and the retention of H trapped by carbon atom should control the chemical form of hydrocarbon sputtered by H{sub 2}{sup +} irradiation and the desorption of CH{sub 3} and CH{sub 2} are due to chemical sputtering, although that for CH is physical sputtering. The activation energy for CH{sub 3} desorption has been estimated to be 0.4 eV, corresponding to the trapping process of hydrogen by carbon through the diffusion in W. It is concluded that the chemical states of hydrocarbon sputtered by H{sub 2}{sup +} irradiation for W is determined by the amount of C-H bond on the W surface. (authors)

  16. Construction of TiO2 nanosheets modified glassy carbon electrode (GCE/TiO2) for the detection of hydrazine

    NASA Astrophysics Data System (ADS)

    Ahmad, Khursheed; Mohammad, Akbar; Rajak, Richa; Mobin, Shaikh M.

    2016-07-01

    TiO2 nanosheets were synthesized via solvothermal method and characterized using powder x-ray diffraction (PXRD), UV-vis spectroscopy, scanning electron microscopy (SEM) and energy dispersive x-ray (EDX) mapping. A binder free hydrazine sensor was fabricated by modifying the glassy carbon electrode (GCE) with TiO2 nanosheets, using simple drop casting method (GCE/TiO2). The modified GCE/TiO2 was employed for detection of hydrazine which exhibited a very high sensitivity of 70 μA mM-1 cm-2 with a limit of detection (LOD), 28 μM using cyclic voltammetry whereas a highest sensitivity 330 μA mM-1 cm-2 and LOD, 150 μM was obtained by employing square wave voltammetry.

  17. Enhanced amperometric detection of metronidazole in drug formulations and urine samples based on chitosan protected tetrasulfonated copper phthalocyanine thin-film modified glassy carbon electrode.

    PubMed

    Meenakshi, S; Pandian, K; Jayakumari, L S; Inbasekaran, S

    2016-02-01

    An enhanced electrocatalytic reduction of metronidazole antibiotic drug molecule using chitosan protected tetrasulfonated copper phthalocyanine (Chit/CuTsPc) thin-film modified glassy carbon electrode (GCE) has been developed. An irreversible reduction occurs at -0.47V (vs. Ag/AgCl) using Chit/CuTsPc modified GCE. A maximum peak current value is obtained at pH1 and the electrochemical reduction reaction is a diffusion controlled one. The detection limit is found to be 0.41nM from differential pulse voltammetry (DPV) method. This present investigation method is adopted for electrochemical detection of metronidazole in drug formulation and urine samples by using DPV method.

  18. High-performance carbon nanotube-implanted mesoporous carbon spheres for supercapacitors with low series resistance

    SciTech Connect

    Yi, Bin; Chen, Xiaohua; Guo, Kaimin; Xu, Longshan; Chen, Chuansheng; Yan, Haimei; Chen, Jianghua

    2011-11-15

    Research highlights: {yields} CNTs-implanted porous carbon spheres are prepared by using gelatin as soft template. {yields} Homogeneously distributed CNTs form a well-develop network in carbon spheres. {yields} CNTs act as a reinforcing backbone assisting the formation of pore structure. {yields} CNTs improve electrical conductivity and specific capacitance of supercapacitor. -- Abstract: Carbon nanotube-implanted mesoporous carbon spheres were prepared by an easy polymerization-induced colloid aggregation method using gelatin as a soft template. Scanning electron microscopy, transmission electron microscopy and nitrogen adsorption-desorption measurements reveal that the materials are mesoporous carbon spheres, with a diameter of {approx}0.5-1.0 {mu}m, a specific surface area of 284 m{sup 2}/g and average pore size of 3.9 nm. Using the carbon nanotube-implanted mesoporous carbon spheres as electrode material for supercapacitors in an aqueous electrolyte solution, a low equivalent series resistance of 0.83 {Omega} cm{sup 2} and a maximum specific capacitance of 189 F/g with a measured power density of 8.7 kW/kg at energy density of 6.6 Wh/kg are obtained.

  19. PdCo porous nanostructures decorated on polypyrrole @ MWCNTs conductive nanocomposite-Modified glassy carbon electrode as a powerful catalyst for ethanol electrooxidation

    NASA Astrophysics Data System (ADS)

    Fard, Leyla Abolghasemi; Ojani, Reza; Raoof, Jahan Bakhsh; Zare, Ehsan Nazarzadeh; Lakouraj, Moslem Mansour

    2017-04-01

    In the current study, well-defined PdCo porous nanostructure (PdCo PNS) is prepared by a simple one-pot wet-chemical method and polypyrrole@multi-walled carbon nanotubes (PPy@MWCNTs) nanocomposite is used as a catalyst support. The morphology and the structural properties of the prepared catalyst were studied by scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDS). The electrocatalytic performance of PdCo PNS/PPy@MWCNTs on glassy carbon electrode has been evaluated by cyclic voltammetry (CV), chronoamperometry (CA) and electrochemical impedance spectroscopy (EIS) techniques. The specific activity of PdCo PNS/PPy@MWCNTs for ethanol electrooxidation (1.65 mA cm-2) is higher than those of other compared electrocatalysts. Also, PdCo PNS/PPy@MWCNTs catalyst represented higher electrocatalytic activity, better long-term stability and high level of poisoning tolerance to the carbonaceous oxidative intermediates for ethanol electrooxidation reaction in alkaline media. Furthermore, the presence of PPY@MWCNTs on the surface of GCE produce a high activity to electrocatalyst, which might be due to the easier charge transfer at polymer/carbon nanotubes interfaces, higher electrochemically accessible surface areas and electronic conductivity. The superior catalytic activity of PdCo PNS/PPy@MWCNTs suggests it to be as a promising electrocatalyst for future direct ethanol fuel cells.

  20. Development of sensitive amperometric hydrogen peroxide sensor using a CuNPs/MB/MWCNT-C60-Cs-IL nanocomposite modified glassy carbon electrode.

    PubMed

    Roushani, Mahmoud; Bakyas, Kobra; Zare Dizajdizi, Behruz

    2016-07-01

    A sensitive hydrogen peroxide (H2O2) sensor was constructed based on copper nanoparticles/methylene blue/multiwall carbon nanotubes-fullerene-chitosan-ionic liquid (CuNPs/MB/MWCNTs-C60-Cs-IL) nanocomposites. The MB/MWCNTs-C60-Cs-IL and CuNPs were modified glassy carbon electrode (GCE) by the physical adsorption and electrodeposition of copper nitrate solution, respectively. The physical morphology and chemical composition of the surface of modified electrode was investigated by scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDS), respectively. The electrochemical properties of CuNPs/MB/MWCNTs-C60-Cs-IL/GCE were investigated by cyclic voltammetry (CV) and amperometry techniques and the sensor exhibited remarkably strong electrocatalytic activities toward the reduction of hydrogen peroxide. The peak currents possess a linear relationship with the concentration of H2O2 in the range of 0.2μM to 2.0mM, and the detection limit is 55.0nM (S/N=3). In addition, the modified electrode was used to determine H2O2 concentration in human blood serum sample with satisfactory results. Copyright © 2016 Elsevier B.V. All rights reserved.

  1. Covalent attachment of diphosphine ligands to glassy carbon electrodes via Cu-catalyzed alkyne-azide cycloaddition. Metallation with Ni(II).

    PubMed

    Das, Atanu K; Engelhard, Mark H; Lense, Sheri; Roberts, John A S; Bullock, R Morris

    2015-07-21

    Covalent tethering of P(Ph)2N(C6H4C≡CH)2 ligands (P(Ph)2N(C6H4C≡CH)2 = 1,5-di-(4-ethynylphenyl)-3,7-diphenyl-1,5-diaza-3,7-diphosphacyclooctane) to planar, azide-terminated glassy carbon electrode surfaces has been accomplished using a Cu(I)-catalyzed alkyne-azide cycloaddition (CuAAC) coupling reaction, using a BH3←P protection-deprotection strategy. Deprotected, surface-confined ligands were metallated using [Ni(II)(MeCN)6](BF4)2. X-ray photoelectron spectroscopic measurements demonstrate that metallation introduced 1.3 equivalents Ni(II) per diphosphine onto the electrode surface. Exposure of the surface to a second diphosphine ligand, P(Ph)2N(Ph)2, resulted in the removal of Ni from the surface. Protection, coupling, deprotection, and metallation conditions were optimized using solution-phase model systems, with benzyl azide as a model for the azide-terminated carbon surface; these reactions generate a [Ni(II)(diphosphine)2](2+) complex.

  2. Ultra-smooth glassy graphene thin films for flexible transparent circuits

    PubMed Central

    Dai, Xiao; Wu, Jiang; Qian, Zhicheng; Wang, Haiyan; Jian, Jie; Cao, Yingjie; Rummeli, Mark H.; Yi, Qinghua; Liu, Huiyun; Zou, Guifu

    2016-01-01

    Large-area graphene thin films are prized in flexible and transparent devices. We report on a type of glassy graphene that is in an intermediate state between glassy carbon and graphene and that has high crystallinity but curly lattice planes. A polymer-assisted approach is introduced to grow an ultra-smooth (roughness, <0.7 nm) glassy graphene thin film at the inch scale. Owing to the advantages inherited by the glassy graphene thin film from graphene and glassy carbon, the glassy graphene thin film exhibits conductivity, transparency, and flexibility comparable to those of graphene, as well as glassy carbon–like mechanical and chemical stability. Moreover, glassy graphene–based circuits are fabricated using a laser direct writing approach. The circuits are transferred to flexible substrates and are shown to perform reliably. The glassy graphene thin film should stimulate the application of flexible transparent conductive materials in integrated circuits. PMID:28138535

  3. Carbon and fluorine co-implantation for boron diffusion suppression in extremely ultra shallow junctions

    NASA Astrophysics Data System (ADS)

    Miakonkikh, Andrey V.; Rogozhin, Aleksander E.; Rudakov, Valeriy I.; Rudenko, Konstantin V.; Lukichev, Vladimir F.

    2014-12-01

    Formation of ultra shallow p+-junctions in silicon by plasma immersion ion implantation were investigated. The effect of carbon and fluorine coimplantation were studied experimentally. Dependence of this effect from carbon concentration was studied, as well as positive role of multistep annealing for pure boron implanted samples.

  4. Study of the overall behavior of thin films of the 7,7,8,8-tetracyanoquinodimethane neutral/anion couple on glassy carbon electrodes in the presence of cesium ion.

    PubMed

    Gómez, L; Rodríguez-Amaro, R

    2008-10-07

    The overall electrochemistry of 7,7,8,8-tetracyanoquinodimethane thin films on glassy carbon electrodes in media containing Cs+ ions is explained in light of a layer-by-layer nucleation and growth model, and kinetic data for the processes involved are reported. Using in situ UV-vis spectroelectrochemistry allowed available mechanistic knowledge on such processes to be expanded and the presence of various intermediates in the redox reactions confirmed.

  5. Hexagonal cobalt carbide formed by carbon ion implantation

    NASA Astrophysics Data System (ADS)

    Liu, B. X.; Wang, J.; Fang, Z. Z.

    1991-05-01

    Thin films of ferromagnetic metals, i.e., bcc Fe, hcp Co, and fcc Ni, were subjected to 50-keV carbon ion implantation at room temperature. At the dose of 2.5×1017 ions/cm2, the formation of hexagonal Fe3C and Ni3C phases was confirmed by transmission electron microscopy selected area electron diffraction patterns; and more interestingly a similar pattern for Co was also observed for the first time. The phase was identified as hexagonal Co3C with a=2.685 Å and c=4.335 Å based on the spacings and intensities of the diffraction rings. The carbide formation was also confirmed by Auger electron spectra. The stoichiometry of the hexagonal structure may be extended in the range of Co3-2C as estimated from the experiments performed up to the dose of 9×1017 ions/cm2.

  6. Characterization of few-layered graphene grown by carbon implantation

    SciTech Connect

    Lee, Kin Kiong; McCallum, Jeffrey C.; Jamieson, David N.

    2014-02-21

    Graphene is considered to be a very promising material for applications in nanotechnology. The properties of graphene are strongly dependent on defects that occur during growth and processing. These defects can be either detrimental or beneficial to device performance depending on defect type, location and device application. Here we present experimental results on formation of few-layered graphene by carbon ion implantation into nickel films and characteristics of graphene devices formed by graphene transfer and lithographic patterning. Micro-Raman spectroscopy was used to determine the number of graphene layers formed and identify defects arising from the device processing. The graphene films were cleaned by annealing in vacuum. Transport properties of cleaned graphene films were investigated by fabrication of back-gated field-effect transistors, which exhibited high hole and electron mobility of 1935 and 1905 cm2/Vs, respectively.

  7. Hierarchical Co(OH)2 nanostructures/glassy carbon electrode derived from Co(BTC) metal-organic frameworks for glucose sensing

    NASA Astrophysics Data System (ADS)

    He, Juan; Lu, Xingping; Yu, Jie; Wang, Li; Song, Yonghai

    2016-07-01

    A novel Co(OH)2/glassy carbon electrode (GCE) has been fabricated via metal-organic framework (MOF)-directed method. In the strategy, the Co(BTC, 1,3,5-benzentricarboxylic acid) MOFs/GCE was firstly prepared by alternately immersing GCE in Co2+ and BTC solution based on a layer-by-layer method. And then, the Co(OH)2 with hierarchical flake nanostructure/GCE was constructed by immersing Co(BTC) MOFs/GCE into 0.1 M NaOH solution at room temperature. Such strategy improves the distribution of hierarchical Co(OH)2 nanostructures on electrode surface greatly, enhances the stability of nanomaterials on the electrode surface, and increases the use efficiency of the Co(OH)2 nanostructures. Scanning electron microscopy, energy dispersive X-ray spectroscopy, X-ray powder diffraction, energy dispersive spectroscopy, Fourier transform infrared spectroscopy, and Raman spectra were used to characterize the Co(BTC) MOFs/GCE and Co(OH)2/GCE. Based on the hierarchical Co(OH)2 nanostructures/GCE, a novel and sensitive nonenzymatic glucose sensor was developed. The good performance of the resulted sensor toward the detection of glucose was ascribed to hierarchical flake nanostructures, good mechanical stability, excellent distribution, and large specific surface area of Co(OH)2 nanostructures. The proposed preparation method is simple, efficient, and cheap .

  8. Simultaneous determination of caffeine and paracetamol by square wave voltammetry at poly(4-amino-3-hydroxynaphthalene sulfonic acid)-modified glassy carbon electrode.

    PubMed

    Tefera, Molla; Geto, Alemnew; Tessema, Merid; Admassie, Shimelis

    2016-11-01

    Poly(4-amino-3-hydroxynaphthalene sulfonic acid)-modified glassy carbon electrode (poly(AHNSA)/GCE) was prepared for simultaneous determination of caffeine and paracetamol using square-wave voltammetry. The method was used to study the effects of pH and scan rate on the voltammetric response of caffeine and paracetamol. Linear calibration curves in the range of 10-125μM were obtained for both caffeine and paracetamol in acetate buffer solution of pH 4.5 with a correlation coefficient of 0.9989 and 0.9986, respectively. The calculated detection limits (S/N=3) were 0.79μM for caffeine and 0.45μM for paracetamol. The effects of some interfering substances in the determination of caffeine and paracetamol were also studied and their interferences were found to be negligible which proved the selectivity of the modified electrode. The method was successfully applied for the quantitative determination of caffeine and paracetamol in Coca-Cola, Pepsi-Cola and tea samples.

  9. Determination of vitamin E in margarines and edible oils using square wave anodic stripping voltammetry with a glassy carbon paste electrode.

    PubMed

    Sýs, Milan; Švecová, Blanka; Švancara, Ivan; Metelka, Radovan

    2017-08-15

    A new electroanalytical method for determination of vitamin E in the form of the total content of tocopherols present in margarines and edible oils has been developed. The method is based on extraction of these biologically active compounds into silicone oil, acting as lipophilic binder of glassy carbon paste electrode, with subsequent electrochemical detection by square wave anodic stripping voltammetry (SWASV) in 0.1M HNO3. The values of vitamin E contents were expressed as mass equivalent of α-tocopherol known as the most active form of this lipophilic vitamin. The linear ranges for α-tocopherol determination were 5×10(-7)-4×10(-5) and 5×10(-8)-1×10(-5)molL(-1) with the detection limits of 1×10(-7) and 3.3×10(-9)molL(-1) for 5 and 15min accumulation, respectively. The results have shown that SWASV with extraction step is very sensitive method for the determination of vitamin E, being comparable to reversed-phase high performance liquid chromatography chosen as reference method. Copyright © 2017 Elsevier Ltd. All rights reserved.

  10. Electrocatalytic simultaneous determination of ascorbic acid, uric acid and L-Cysteine in real samples using quercetin silver nanoparticles-graphene nanosheets modified glassy carbon electrode

    NASA Astrophysics Data System (ADS)

    Zare, Hamid R.; Jahangiri-Dehaghani, Fahime; Shekari, Zahra; Benvidi, Ali

    2016-07-01

    By immobilizing of quercetin at the surface of a glassy carbon electrode modified with silver nanoparticles and graphene nanosheets (Q-AgNPs-GNs-GCE) a new sensor has been fabricated. The cyclic voltammogram of Q-AgNPs-GNs-GCE shows a stable redox couple with surface confined characteristics. Q-AgNPs-GNs-GCE demonstrated a high catalytic activity for L-Cysteine (L-Cys) oxidation. Results indicated that L-Cys peak potential at Q-AgNPs-GNs-GCE shifted to less positive values compared to GNs-GCE or AgNPs-GCE. Also, the kinetic parameters such as the electron transfer coefficient,, and the heterogeneous electron transfer rate constant, k‧, for the oxidation of L-Cys at the Q-AgNPs-GNs-GCE surface were estimated. In differential pulse voltammetric determination, the detection limit of L-Cys was obtained 0.28 μM, and the calibration plots were linear within two ranges of 0.9-12.4 μM and 12.4-538.5 μM of L-Cys. Also, the proposed modified electrode is used for the simultaneous determinations of ascorbic acid (AA), uric acid (UA), and L-Cys. Finally, this study has demonstrated the practical analytical utility of the sensor for determination of AA in vitamin C tablet, L-Cys in a milk sample and UA in a human urine sample.

  11. Differential pulse voltammetric determination of P(V) following adsorptive accumulation of alpha-[PMo(12)O(40)](3-) on a polypyrrole-modified glassy carbon electrode.

    PubMed

    Takamoto, Masayo; Himeno, Sadayuki

    2003-03-01

    On the basis of the formation and pre-concentration of an alpha-Keggin-type [PMo(12)O(40)](3-) complex, a novel voltammetric method was developed for the determination of trace levels of P(V). The alpha-[PMo(12)O(40)](3-) complex was formed by heating a 5x10(-4) M Mo(VI)-0.2 M HCl-40% (v/v) CH(3)CN system containing a trace amount of P(V) at 70 degrees C for 30 min. During the electrochemical polymerization of pyrrole in the alpha-[PMo(12)O(40)](3-) solution, the alpha-[PMo(12)O(40)](3-) complex was accumulated into the polypyrrole film on a glassy carbon electrode. The differential pulse voltammetric peak current due to the alpha-[PMo(12)O(40)](3-) complex incorporated in the polypyrrole film was linearly dependent on the P(V) concentration in the range of 5x10(-9)-5x10(-7) M; a detection limit of 2x10(-9) M was achieved.

  12. Electron transfer study on graphene modified glassy carbon substrate via electrochemical reduction and the application for tris(2,2'-bipyridyl)ruthenium(II) electrochemiluminescence sensor fabrication.

    PubMed

    Xu, Yuanhong; Cao, Mengmei; Liu, Huihui; Zong, Xidan; Kong, Na; Zhang, Jizhen; Liu, Jingquan

    2015-07-01

    In this study, electron transfer behavior of the graphene nanosheets attachment on glassy carbon electrode (GCE) via direct electrochemical reduction of graphene oxide (GO) is investigated for the first time. The graphene modified electrode was achieved by simply dipping the GCE in GO suspension, followed by cyclic voltammetric scanning in the potential window from 0V to -1.5V. Tris(2,2'-bipyridyl)ruthenium(II) [Ru(bpy)3(2+)] was immobilized on the graphene modified electrode and used as the redox probe to evaluate the electron transfer behavior. The electron transfer rate constant (Ks) was calculated to be 61.9±5.8s(-1), which is much faster than that of tiled graphene modified GCE (7.1±0.6s(-1)). The enhanced electron transfer property observed with the GCE modified by reductively deposited graphene is probably due to its standing configuration, which is beneficial to the electron transfer comparing with the tiled one. Because the abundant oxygen-containing groups are mainly located at the edges of GO, which should be much easier for the reduction to start from, the reduced GO should tend to stand on the electrode surface as evidenced by scanning electron microscopy analysis. In addition, due to the favored electron transfer and standing configuration, the Ru(bpy)3(2+) electrochemiluminescence sensor fabricated with standing graphene modified GCE provided much higher and more stable efficiency than that fabricated with tiled graphene.

  13. A novel voltammetric sensor for sensitive detection of mercury(II) ions using glassy carbon electrode modified with graphene-based ion imprinted polymer.

    PubMed

    Ghanei-Motlagh, Masoud; Taher, Mohammad Ali; Heydari, Abolfazl; Ghanei-Motlagh, Reza; Gupta, Vinod K

    2016-06-01

    In this paper, a novel strategy was proposed to prepare ion-imprinted polymer (IIP) on the surface of reduced graphene oxide (RGO). Polymerization was performed using methacrylic acid (MAA) as the functional monomer, ethylene glycol dimethacrylate (EGDMA) as the cross-linker, 2,2'-((9E,10E)-1,4-dihydroxyanthracene-9,10-diylidene) bis(hydrazine-1-carbothioamide) (DDBHCT) as the chelating agent and ammonium persulfate (APS) as initiator, via surface imprinted technique. The RGO-IIP was characterized by means of Fourier transform infrared spectroscopy (FT-IR), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM) and thermogravimetric analysis (TGA). The electrochemical procedure was based on the accumulation of Hg(II) ions at the surface of a modified glassy carbon electrode (GCE) with RGO-IIP. The prepared RGO-IIP sensor has higher voltammetric response compared to the non-imprinted polymer (NIP), traditional IIP and RGO. The RGO-IIP modified electrode exhibited a linear relationship toward Hg(II) concentrations ranging from 0.07 to 80 μg L(-1). The limit of detection (LOD) was found to be 0.02 μg L(-1) (S/N=3), below the guideline value from the World Health Organization (WHO). The applicability of the proposed electrochemical sensor to determination of mercury(II) ions in different water samples was reported.

  14. A novel electrochemical sensor based on Au@PANI composites film modified glassy carbon electrode binding molecular imprinting technique for the determination of melamine.

    PubMed

    Rao, Hanbing; Chen, Min; Ge, Hongwei; Lu, Zhiwei; Liu, Xin; Zou, Ping; Wang, Xianxiang; He, Hua; Zeng, Xianyin; Wang, Yanying

    2017-01-15

    A novel molecularly imprinted electrochemical sensor for the rapid detection of melamine was reported in this paper. Glassy carbon electrode (GCE) was modified by Au and polyaniline composites (Au@PANI) deposited on the surface of GCE and were used to increase the electrode sensitivity and to amplify the sensor signal. Melamine template molecule was further assembled onto Au@PANI by the formation of hydrogen bonds, can implement the selective detection of melamine. This simple but efficient electrochemistry analysis platform presents a low detection limit of 1.39×10(-6)µmolL(-1) for detection of melamine, which is remarkably lower than the currently used methods and the previous reports. So, this method may open a new way for the determination of melamine which enables low cost, effective and sensitive determination. This shows the sensor can be potentially utilized for the detection of melamine in food, which allows the sensitive and selective determination of melamine from milk and feed.

  15. Synergy of Cobalt and Silver Microparticles Electrodeposited on Glassy Carbon for the Electrocatalysis of the Oxygen Reduction Reaction: An Electrochemical Investigation.

    PubMed

    Zafferoni, Claudio; Cioncoloni, Giacomo; Foresti, Maria Luisa; Dei, Luigi; Carretti, Emiliano; Vizza, Francesco; Lavacchi, Alessandro; Innocenti, Massimo

    2015-08-07

    The combination of two different metals, each of them acting on different steps of the oxygen reduction reaction (ORR), yields synergic catalytic effects. In this respect, the electrocatalytic effect of silver is enhanced by the addition of cobalt, which is able to break the O-O bond of molecular oxygen, thus accelerating the first step of the reduction mechanism. At the same time, research is to further reduce the catalyst's cost, reducing the amount of Ag, which, even though being much less expensive than Pt, is still a noble metal. From this point of view, using a small amount of Ag together with an inexpensive material, such as graphite, represents a good compromise. The aim of this work was to verify if the synergic effects are still operating when very small amounts of cobalt (2-10 μg·cm(-2)) are added to the microparticles of silver electrodeposited on glassy carbon, described in a preceding paper from us. To better stress the different behaviour observed when cobalt and silver are contemporarily present in the deposit, the catalytic properties of cobalt alone were investigated. The analysis was completed by the Levich plots to evaluate the number of electrons involved and by Tafel plots to show the effects on the reaction mechanism.

  16. Electrochemical behavior and voltammetric determination of acetaminophen based on glassy carbon electrodes modified with poly(4-aminobenzoic acid)/electrochemically reduced graphene oxide composite films.

    PubMed

    Zhu, Wencai; Huang, Hui; Gao, Xiaochun; Ma, Houyi

    2014-12-01

    Poly(4-aminobenzoic acid)/electrochemically reduced graphene oxide composite film modified glassy carbon electrodes (4-ABA/ERGO/GCEs) were fabricated by a two-step electrochemical method. The electrochemical behavior of acetaminophen at the modified electrode was investigated by means of cyclic voltammetry. The results indicated that 4-ABA/ERGO composite films possessed excellent electrocatalytic activity towards the oxidation of acetaminophen. The electrochemical reaction of acetaminophen at 4-ABA/ERGO/GCE is proved to be a surface-controlled process involving the same number of protons and electrons. The voltammetric determination of acetaminophen performed with the 4-ABA/ERGO modified electrode presents a good linearity in the range of 0.1-65 μM with a low detection limit of 0.01 μM (S/N=3). In the case of using the 4-ABA/ERGO/GCE, acetaminophen and dopamine can be simultaneously determined without mutual interference. Furthermore, the 4-ABA/ERGO/GCE has good reproducibility and stability, and can be used to determine acetaminophen in tablets.

  17. Simultaneous determination of N-acetyl-p-aminophenol and p-aminophenol with poly(3,4-ethylenedioxythiophene) modified glassy carbon electrode.

    PubMed

    Mehretie, Solomon; Admassie, Shimelis; Hunde, Tadele; Tessema, Merid; Solomon, Theodros

    2011-09-15

    A sensitive and selective method was developed for the determination of N-acetyl-p-aminophenol (APAP) and p-aminophenol (PAP) using poly(3,4-ethylenedioxythiophene) (PEDOT)-modified glassy carbon electrode (GCE). Cyclic voltammetry and differential pulse voltammetry were used to investigate the electrochemical reaction of APAP and PAP at the modified electrode. Both APAP and PAP showed quasireversible redox reactions with formal potentials of 367 mV and 101 mV (vs. Ag/AgCl), respectively, in phosphate buffer solution of pH 7.0. The significant peak potential difference (266 mV) between APAP and PAP enabled the simultaneous determination both species based on differential pulse voltammetry. The voltammetric responses gave linear ranges of 1.0×10(-6)-1.0×10(-4) mol L(-1) and 4.0×10(-6)-3.2×10(-4) mol L(-1), with detection limits of 4.0×10(-7) mol L(-1) and 1.2×10(-6) mol L(-1) for APAP and PAP, respectively. The method was successfully applied for the determination of APAP and PAP in pharmaceutical formulations and biological samples.

  18. Nano-assemblies consisting of Pd/Pt nanodendrites and poly (diallyldimethylammonium chloride)-coated reduced graphene oxide on glassy carbon electrode for hydrogen peroxide sensors.

    PubMed

    Zhang, Yanyan; Zhang, Cong; Zhang, Di; Ma, Min; Wang, Weizhen; Chen, Qiang

    2016-01-01

    Non-enzymatic hydrogen peroxide (H2O2) sensors were fabricated on the basis of glassy carbon (GC) electrode modified with palladium (Pd) core-platinum (Pt) nanodendrites (Pt-NDs) and poly (diallyldimethylammonium chloride) (PDDA)-coated reduced graphene oxide (rGO). A facile wet-chemical method was developed for preparing Pd core-Pt nanodendrites. In this approach, the growth of Pt NDs was directed by Pd nanocrystal which could be regarded as seed. The PDDA-coated rGO could form uniform film on the surface of GC electrode, which provided a support for Pd core- Pt NDs adsorption by self-assembly. The morphologies of the nanocomposites were characterized by transmission electron microscopy, energy-dispersive X-ray spectroscopy and X-ray diffraction (spectrum). Electrocatalytic ability of the nanocomposites was evaluated by cyclic voltammetry and chronoamperometric methods. The sensor fabricated by Pd core-Pt NDs/PDDA-rGO/GCE exhibited high sensitivity (672.753 μA mM(-1) cm(-2)), low detection limit (0.027 μM), wider linear range (0.005-0.5mM) and rapid response time (within 5s). Besides, it also exhibited superior reproducibility, excellent anti-interference performance and long-term stability. The present work could afford a viable method and efficient platform for fabricating all kinds of amperometric sensors and biosensors.

  19. A sensitive electrochemical DNA biosensor for antineoplastic drug 5-fluorouracil based on glassy carbon electrode modified with poly(bromocresol purple).

    PubMed

    Koyuncu Zeybek, Derya; Demir, Burcu; Zeybek, Bülent; Pekyardımcı, Şule

    2015-11-01

    This paper describes an electrochemical sensor for the first time based on poly(bromocresol purple) (P(BCP)) developed to observe the interaction between 5-fluorouracil (5-FU) and fish sperm double strand DNA (dsDNA). The P(BCP) film was electrosynthesized by cyclic voltammetry method on the glassy carbon electrode (GCE). The dsDNA was electrochemically immobilized on the surface of P(BCP) modified GCE and the DNA biosensor was prepared. The interaction mechanism of dsDNA with 5-FU was investigated by differential pulse voltammetry using this biosensor. A decrease in the guanine oxidation peak current of the biosensor was observed after the interaction of dsDNA and 5-FU in 0.5 mol L(-1) acetate buffer (pH 4.8) containing 0.02 mol L(-1) NaCl. The accumulation time and dsDNA concentration were optimized to obtain the best peak current response. Under optimum conditions, the linear response on the guanine signal decreasing curve was observed in the 5-FU concentration range of 1.0-50 mg L(-1). The interaction mechanism between dsDNA and 5-FU was further investigated by UV-vis spectroscopy and viscometer. The results reveal that intercalation is the primary mode of interaction between 5-FU and dsDNA.

  20. A novel electrochemical sensor for the analysis of β-agonists: the poly(acid chrome blue K)/graphene oxide-nafion/glassy carbon electrode.

    PubMed

    Lin, Xiaoyun; Ni, Yongnian; Kokot, Serge

    2013-09-15

    A novel modified electrode was constructed by the electro-polymerization of 4,5-dihydroxy-3-[(2-hydroxy-5-sulfophenyl)azo]-2,7-naphthalenedisulfonic acid trisodium salt (acid chrome blue K (ACBK)) at a graphene oxide (GO)-nafion modified glassy carbon electrode (GCE). The characterization of an electrochemically synthesized poly-ACBK/GO-nafion film was investigated by electrochemical impedance spectroscopy (EIS), cyclic voltammetry (CV), atomic force microscopy (AFM) and scanning electron microscopy (SEM) techniques, and the results were interpreted and compared at each stage of the electrode construction. Electrochemical oxidation of eight β-agonists - clenbuterol, salbutamol, terbutaline, ractopamine, dopamine, dobutamine, adrenaline, and isoprenaline, was investigated by CV at the different electrodes. At the poly-ACBK/GO-nafion/GCE, the linear sweep voltammetry peak currents of the eight β-agonists increased linearly with their concentrations in the range of 1.0-36.0 ng mL(-1), respectively, and their corresponding limits of detection (LODs) were within the 0.58-1.46 ng mL(-1) range. This electrode showed satisfactory reproducibility and stability, and was used successfully for the quantitative analysis of clenbuterol in pork samples.

  1. Electrodeposition From Acidic Solutions of Nickel Bis(benzenedithiolate) Produces a Hydrogen-Evolving Ni-S Film on Glassy Carbon

    SciTech Connect

    Fang, Ming; Engelhard, Mark H.; Zhu, Zihua; Helm, Monte L.; Roberts, John A.

    2014-01-03

    Films electrodeposited onto glassy carbon electrodes from acidic acetonitrile solutions of [Bu4N][Ni(bdt)2] (bdt = 1,2-benzenedithiolate) are active toward electrocatalytic hydrogen production at potentials 0.2-0.4 V positive of untreated electrodes. This activity is preserved on rinsing the electrode and transfer to fresh acid solution. X-ray photoelectron spectra indicate that the deposited material contains Ni and S. Correlations between voltammetric and spectroscopic results indicate that the deposited material is active, i.e. that catalysis is heterogeneous rather than homogeneous. Control experiments establish that obtaining the observed catalytic response requires both Ni and the 1,2 benzenedithiolate ligand to be present during deposition. This research was supported as part of the Center for Molecular Electrocatalysis, an Energy Frontier Research Center funded by the US Department of Energy, Office of Science, Office of Basic Energy Sciences. Pacific Northwest National Laboratory is operated by Battelle for the US Department of Energy. A portion of the research was performed using EMSL, a 17 national scientific user facility sponsored by the Department of Energy's Office of Biological and Environmental Research and located at Pacific Northwest National Laboratory.

  2. Fuel blends: Enhanced electro-oxidation of formic acid in its blend with methanol at platinum nanoparticles modified glassy carbon electrodes

    NASA Astrophysics Data System (ADS)

    El-Deab, Mohamed S.; El-Nagar, Gumaa A.; Mohammad, Ahmad M.; El-Anadouli, Bahgat E.

    2015-07-01

    The current study addresses, for the first time, the enhanced direct electro-oxidation of formic acid (FA) at platinum-nanoparticles modified glassy carbon (nano-Pt/GC) electrode in the presence of methanol (MeOH) as a blending fuel. This enhancement is probed by: (i) the increase of the direct oxidation current of FA to CO2 (Ipd, dehydrogenation pathway), (ii) suppressing the dehydration pathway (Ipind, producing the poisoning intermediate CO) and (iii) a favorable negative shift of the onset potential of Ipd with increasing the mole fraction of MeOH in the blend. Furthermore, the charge of the direct FA oxidation in 0.3 M FA + 0.3 M MeOH blend is by 14 and 21times higher than that observed for 0.3 M FA and 0.3 M MeOH, respectively. MeOH is believed to adsorb at the Pt surface sites and thus disfavor the "non-faradaic" dissociation of FA (which produces the poisoning CO intermediate), i.e., MeOH induces a high CO tolerance of the Pt catalyst. The enhanced oxidation activity indicates that FA/MeOH blend is a promising fuel system.

  3. Mercury(II) trace detection by a gold nanoparticle-modified glassy carbon electrode using square-wave anodic stripping voltammetry including a chloride desorption step.

    PubMed

    Laffont, Laure; Hezard, Teddy; Gros, Pierre; Heimbürger, Lars-Eric; Sonke, Jeroen E; Behra, Philippe; Evrard, David

    2015-08-15

    Gold nanoparticles (AuNPs) were deposited on a glassy carbon (GC) substrate by constant potential electrolysis and characterized by cyclic voltammetry in H2SO4 and field emission gun scanning electron microscopy (FEG-SEM). The modified AuNPs-GC electrode was used for low Hg(II) concentration detection using a Square Wave Anodic Stripping Voltammetry (SWASV) procedure which included a chloride desorption step. The comparison of the obtained results with our previous work in which no desorption step was used showed that this latter step significantly improved the analytical performances, providing a three time higher sensitivity and a limit of detection of 80pM for 300s preconcentration, as well as a lower average standard deviation. The influence of chloride concentration on the AuNPs-GC electrode response to Hg(II) trace amounts was also studied and its optimal value confirmed to be in the 10(-2)M range. Finally, the AuNPs-GC electrode was used for the determination of Hg(II) in a natural groundwater sample from south of France. By using a preconcentration time of 3000s, a Hg(II) concentration of 19±3pM was found, which compared well with the result obtained by cold vapor atomic fluorescence spectroscopy (22±2pM).

  4. Differential pulse anodic stripping voltammetry for detection of As (III) by Chitosan-Fe(OH)3 modified glassy carbon electrode: A new approach towards speciation of arsenic.

    PubMed

    Saha, Suparna; Sarkar, Priyabrata

    2016-09-01

    An efficient electrochemical sensor for As(III) was developed based on adsorption of arsenic on a specially modified electrodes at some applied potential and subsequent i) stripping at a fixed potential by anodic stripping voltammetry ii) analysis by generating surface plasmon resonance (SPR). The working glassy carbon electrode was modified by Chitosan-Fe(OH)3 composite and a reducing agent L-cysteine. The composite enhanced adsorption of As(III) and subsequent reduction to As(O) moieties and measurement by anodic stripping. The surface property of modified electrode was characterized by SEM, AFM, FTIR, XPS and electrochemistry was analyzed by impedance spectroscopy (EIS). Surface Plasmon resonance (SPR) was also employed to investigate the As(III) binding capability of polymer matrix. Several optimum voltammetric parameters e.g supporting electrolyte; 0.1M acetate buffer (pH 5.2) deposition potential, -0.9V; deposition time, 100s were established for anodic stripping voltammetry (ASV). A linear correlation was obtained in the range of 2-100ppb for ASV (R(2) 0.974) with limit of detection 0.072ppb. A variety of common coexistent ions such as Mn, Zn, Pb, Cu, Cd in water samples showed no interferences on the As (III) determination. The method was applied successfully to real samples collected from arsenic affected areas of West Bengal, India.

  5. Determination of guanine and adenine by high-performance liquid chromatography with a self-fabricated wall-jet/thin-layer electrochemical detector at a glassy carbon electrode.

    PubMed

    Zhou, Yaping; Yan, Hongling; Xie, Qingji; Yao, Shouzhuo

    2015-03-01

    A sensitive wall-jet/thin-layer amperometric electrochemical detector (ECD) coupled to high-performance liquid chromatography (HPLC) was developed for simultaneous determination of guanine (G) and adenine (A). The analytes were detected at a glassy carbon electrode (GCE) and the HPLC-ECD calibration curves showed good linearity (R(2)>0.997) under optimized conditions. Limits of detection for G and A are 0.6 nM and 1.4 nM (S/N=3), respectively, which are lower than those obtained with an UV-vis detector and a commercial electrochemical detector. We have successfully applied this HPLC-ECD to assess the contents of G and A in hydrochloric acid-digested calf thymus double-stranded DNA. In addition, we compared in detail the analysis of G and A by cyclic voltammetry (CV) and by the HPLC-ECD system on both bare GCE and electroreduced graphene oxide (ERGO) modified GCE. We found that the adsorption of G and A on the electrode surfaces can vary their anodic CV peaks and the competitive adsorption of G and A on the limited sites of the electrode surfaces can cause crosstalk effects on their anodic CV peak signals, but the HPLC-ECD system is insensitive to such electrode-adsorption and can give more reliable analytical results. Copyright © 2014 Elsevier B.V. All rights reserved.

  6. Reductive Electropolymerization of a Vinyl-containing Poly-pyridyl Complex on Glassy Carbon and Fluorine-doped Tin Oxide Electrodes

    PubMed Central

    Harrison, Daniel P.; Carpenter, Logan S.; Hyde, Jacob T.

    2015-01-01

    Controllable electrode surface modification is important in a number of fields, especially those with solar fuels applications. Electropolymerization is one surface modification technique that electrodeposits a polymeric film at the surface of an electrode by utilizing an applied potential to initiate the polymerization of substrates in the Helmholtz layer. This useful technique was first established by a Murray-Meyer collaboration at the University of North Carolina at Chapel Hill in the early 1980s and utilized to study numerous physical phenomena of films containing inorganic complexes as the monomeric substrate. Here, we highlight a procedure for coating electrodes with an inorganic complex by performing reductive electropolymerization of the vinyl-containing poly-pyridyl complex onto glassy carbon and fluorine doped tin oxide coated electrodes. Recommendations on electrochemical cell configurations and troubleshooting procedures are included. Although not explicitly described here, oxidative electropolymerization of pyrrole-containing compounds follows similar procedures to vinyl-based reductive electropolymerization but are far less sensitive to oxygen and water. PMID:25741745

  7. A novel lable-free electrochemical immunosensor for carcinoembryonic antigen based on gold nanoparticles-thionine-reduced graphene oxide nanocomposite film modified glassy carbon electrode.

    PubMed

    Kong, Fen-Ying; Xu, Mao-Tian; Xu, Jing-Juan; Chen, Hong-Yuan

    2011-10-15

    In this paper, gold nanoparticle-thionine-reduced graphene oxide (GNP-THi-GR) nanocomposites were prepared to design a label-free immunosensor for the sensitive detection of carcinoembryonic antigen (CEA). The nanocomposites with good biocompatibility, excellent redox electrochemical activity and large surface area were coated onto the glassy carbon electrode (GCE) surface and then CEA antibody (anti-CEA) was immobilized on the electrode to construct the immunosensor. The morphologies and electrochemistry of the formed nanocomposites were investigated by using scanning electron microscopy (SEM), ultraviolet-visible (UV-vis) spectrometry, electrochemical impedance spectroscopy (EIS) and cyclic voltammetry (CV). CV and differential pulse voltammetry (DPV) studies demonstrated that the formation of antibody-antigen complexes decreased the peak current of THi in the GNP-THi-GR nanocomposites. The decreased currents were proportional to the CEA concentration in the range of 10-500 pg/mL with a detection limit of 4 pg/mL. The proposed method was simple, fast and inexpensive for the determination of CEA at very low levels.

  8. Immobilization of Ni-Pd/core-shell nanoparticles through thermal polymerization of acrylamide on glassy carbon electrode for highly stable and sensitive glutamate detection.

    PubMed

    Yu, Huicheng; Ma, Zhenzhen; Wu, Zhaoyang

    2015-10-08

    The preparation of a persistently stable and sensitive biosensor is highly important for practical applications. To improve the stability and sensitivity of glutamate sensors, an electrode modified with glutamate dehydrogenase (GDH)/Ni-Pd/core-shell nanoparticles was developed using the thermal polymerization of acrylamide (AM) to immobilize the synthesized Ni-Pd/core-shell nanoparticles onto a glassy carbon electrode (GCE). The modified electrode was characterized by scanning electron microscopy (SEM), Fourier transform infrared (FTIR) spectroscopy, cyclic voltammetry (CV), and electrochemical impedance spectroscopy (EIS). Electrochemical data showed that the prepared biosensor had remarkably enhanced electrocatalytic activity toward glutamate. Moreover, superior reproducibility and excellent stability were observed (relative average deviation was 2.96% after continuous use of the same sensor for 60 times, and current responses remained at 94.85% of the initial value after 60 d). The sensor also demonstrated highly sensitive amperometric detection of glutamate with a low limit of detection (0.052 μM, S/N = 3), high sensitivity (4.768 μA μM(-1) cm(-2)), and a wide, useful linear range (0.1-500 μM). No interference from potential interfering species such as l-cysteine, ascorbic acid, and l-aspartate were noted. The determination of glutamate levels in actual samples achieved good recovery percentages.

  9. Dopamine and uric acid electrochemical sensor based on a glassy carbon electrode modified with cubic Pd and reduced graphene oxide nanocomposite.

    PubMed

    Wang, Jin; Yang, Beibei; Zhong, Jiatai; Yan, Bo; Zhang, Ke; Zhai, Chunyang; Shiraishi, Yukihide; Du, Yukou; Yang, Ping

    2017-03-02

    A cubic Pd and reduced graphene oxide modified glassy carbon electrode (Pd/RGO/GCE) was fabricated to simultaneously detect dopamine (DA) and uric acid (UA) by cyclic voltammetry (CV) and different pulse voltammetry (DPV) methods. Compared with Pd/GCE and RGO/GCE, the Pd/RGO/GCE exhibited excellent electrochemical activity in electrocatalytic behaviors. Performing the Pd/RGO/GCE in CV measurement, the well-defined oxidation peak potentials separation between DA and UA reached to 145mV. By using the differential pulse voltammetry (DPV) technique, the calibration curves for DA and UA were found linear with the concentration range of 0.45-421μM and 6-469.5μM and the detection limit (S/N =3) were calculated to be 0.18μM and 1.6μM, respectively. Furthermore, the Pd/RGO/GCE displayed high selectivity when it was applied into the determination of DA and UA even though in presence of high concentration of interferents. Additionally, the prepared electrochemical sensor of Pd/RGO/GCE demonstrated a practical feasibility in rat urine and serum samples determination.

  10. Electrochemical study of the antiplatelet agent clopidogrel and its determination using differential pulse voltammetry in bulk form and pharmaceutical preparations with a glassy carbon electrode.

    PubMed

    Dermiş, S; Aydoğan, E

    2010-03-01

    In the present study, the electroanalytical behaviour of clopidogrel (CLP) bisulfate, an antithrombotic drug, was investigated by cyclic voltammetry (CV) and differential pulse voltammetry (DPV) techniques using a glassy carbon electrode (GCE). The anodic oxidation of clopidogrel bisulfate was investigated with a GCE to determine the oxidation conditions. The voltammograms of solutions having various concentrations of clopidogrel were recorded in order to obtain the optimum oxidation conditions of this drug on a GCE. To determine the effects of the nature of the supporting electrolyte, pH and scan rate on the anodic oxidation reactions, the experiments were performed in 0.2 M sulphuric acid, and in Britton-Robinson (BR) (pH 2-5) and acetate (pH 3.5-5.63) buffers with a 10-400 mVs(-1) scan rate interval. The oxidation of clopidogrel bisulfate was found to be diffusion-controlled over a concentration range of 0.08 mM-1.0 mM in pH 3.7 acetate buffer by an optimized DPV technique. The voltammetric method developed was applied to the tablet form of pharmaceutical preparation of this compound and the accuracy, precision, selectivity, sensitivity, repeatibility within and between days and reproducibility of the proposed method was investigated statistically. The results were compared with the spectrophotometric and HPLC methods developed in our laboratory and found to be in good agreement. No interference was observed from common pharmaceutical adjuvants.

  11. Molecularly imprinted poly(4-amino-5-hydroxy-2,7-naphthalenedisulfonic acid) modified glassy carbon electrode as an electrochemical theophylline sensor.

    PubMed

    Aswini, K K; Vinu Mohan, A M; Biju, V M

    2016-08-01

    Theophylline is an inexpensive drug employed in asthma and chronic obstructive pulmonary disorder medications and is toxic at higher concentration. The development of a molecularly imprinted polymer based theophylline electrochemical sensor on glassy carbon electrode by the electropolymerization of 4-amino-5-hydroxy-2,7-naphthalenedisulfonic acid is being discussed in this work. The MIP modification enhances the theophylline recognition ability and the electron transfer kinetics of the bare electrode. The parameters, controlling the performance of the imprinted polymer based sensor, like number of electropolymerization cycles, composition of the pre-polymerization mixture, pH and immersion time were investigated and optimized. The interaction energy and the most stable conformation of the template-monomer complex in the pre-polymerization mixture were determined computationally using ab initio calculations based on density functional theory. The amperometric measurements showed that the developed sensor has a method detection limit of 0.32μM for the dynamic range of 0.4 to 17μM, at optimized conditions. The transducer possesses appreciable selectivity in the presence of structurally similar interferents such as theobromine, caffeine and doxofylline. The developed sensor showed remarkable stability and reproducibility and was also successfully employed in theophylline detection from commercially available tablets. Copyright © 2016 Elsevier B.V. All rights reserved.

  12. A new kinetic-mechanistic approach to elucidate electrooxidation of doxorubicin hydrochloride in unprocessed human fluids using magnetic graphene based nanocomposite modified glassy carbon electrode.

    PubMed

    Soleymani, Jafar; Hasanzadeh, Mohammad; Shadjou, Nasrin; Khoubnasab Jafari, Maryam; Gharamaleki, Jalil Vaez; Yadollahi, Mehdi; Jouyban, Abolghasem

    2016-04-01

    A novel magnetic nanocomposite was synthesized in one step using polymerization of magnetic graph oxide grafted with chlorosulfonic acid (Fe3O4-GO-SO3H) in the presence of polystyrene. The prepared magnetic nanocomposite was characterized using transmission electron microscopy (TEM), dynamic differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), (Thermo-gravimetric/differential thermal analysis (DTA)), Fourier transform infrared (FTIR), and UV-Vis techniques. Magnetic nanocomposite was casted on the surface of the glassy carbon electrode (PS/Fe3O4-GO-SO3H/GCE) and used for the detection and determination of doxorubicin hydrochloride (DOX) in human biological fluids. The cyclic voltammograms (CVs) of the modified electrode in aqueous solution displayed a pair of well-defined, stable and irreversible reductive/oxidation redox systems. CV study indicated that the oxidation process is irreversible and adsorption controlled. In addition, CV results indicated that DOX is oxidized via two electrons and three protons which is an unusual approach for the oxidation of DOX. A sensitive and time-saving procedure was developed for the analysis of DOX in plasma, cerebrospinal fluid, and urine with detection limit of 4.9 nM, 14 nM and 4.3 nM, respectively.

  13. Electrochemical determination of Sudan I in food samples at graphene modified glassy carbon electrode based on the enhancement effect of sodium dodecyl sulphonate.

    PubMed

    Ma, Xinying; Chao, Mingyong; Wang, Zhaoxia

    2013-06-01

    This paper describes a novel electrochemical method for the determination of Sudan I in food samples based on the electrochemical catalytic activity of graphene modified glassy carbon electrode (GMGCE) and the enhancement effect of an anionic surfactant: sodium dodecyl sulphonate (SDS). Using pH 6.0 phosphate buffer solution (PBS) as supporting electrolyte and in the presence of 1.5 × 10(-4)mol L(-1) SDS, Sudan I yielded a well-defined and sensitive oxidation peak at a GMGCE. The oxidation peak current of Sudan I remarkably increased in the presence of SDS. The experimental parameters, such as supporting electrolyte, concentration of SDS, and accumulation time, were optimised for Sudan I determination. The oxidation peak current showed a linear relationship with the concentrations of Sudan I in the range of 7.50 × 10(-8)-7.50 × 10(-6)mol L(-1), with the detection limit of 4.0 × 10(-8)mol L(-1). This new voltammetric method was successfully used to determine Sudan I in food products such as ketchup and chili sauce with satisfactory results.

  14. Adsorption and deposition-assisted anodic stripping voltammetry for determination of antimony(III) in presence of hematoxylin on glassy carbon electrode.

    PubMed

    Sezgin, Hanife Vardar; Dilgin, Yusuf; Gökçel, H İsmet

    2017-03-01

    A validated simple, reliable and sensitive adsorptive anodic stripping voltammetric procedure is suggested for the accurate determination of antimony(III) on a glassy carbon electrode (GCE) in the presence of hematoxylin (HT), used as a chemical receptor in antimony analysis for the first time. Under optimized conditions, the plot of stripping peak current versus Sb(III) concentration showed two dynamic linear ranges, 1.0×10(-4) - 0.01µm (R(2) =0.9986) and 0.01 - 1.0µm (R(2) =0.9973) with a detection limit of 9.5×10(-11)molL(-1) (11.57ngL(-1)). The RSD values of intra-day precision and inter-day precision (n =5) for 5.0×10(-7)molL(-1) Sb(III) were calculated as 1.63% and 2.27%, respectively, indicating that the proposed method has a good precision. Recoveries for Sb(III) in water samples were found to be between 97% and 102% for the 5.0×10(-7)molL(-1) Sb(III), proving the reliability and accuracy of the method proposed. Copyright © 2016 Elsevier B.V. All rights reserved.

  15. Amperometric biosensor for hydrogen peroxide based on direct electrocatalysis by hemoglobin immobilized on gold nanoparticles/1,6-diaminohexane modified glassy carbon electrode.

    PubMed

    Tang, Mingyu; Chen, Shihong; Yuan, Ruo; Chai, Yaqin; Gao, Fengxian; Xie, Yi

    2008-04-01

    A facile strategy of an amperometric biosensor for hydrogen peroxide based on the direct electrocatalysis of hemoglobin (Hb) immobilized on gold nanoparticles (GNPs)/1,6-diaminohexane (DAH) modified glassy carbon electrode (GCE) has been described. A uniform monolayer film of DAH was initially covalently bound on a GCE surface by virtue of the electrooxidation of one amino group of DAH, and another amino group was modified with GNPs and Hb, successively. The fabrication process was characterized by cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS) and scanning electron microscopy (SEM). The proposed biosensor exhibited an effective and fast catalytic response to the reduction of H2O2 with good reproducibility and stability. A linear relationship existed between the catalytic current and the H2O2 concentration in the range of 1.5x10(-6) to 2.1x10(-3) M with a correlation coefficient of 0.998 (n=24). The detection limit (S/N=3) was 8.8x10(-7) M.

  16. The electrodeposition of Ag nanoparticles on a type I collagen-modified glassy carbon electrode and their applications as a hydrogen peroxide sensor.

    PubMed

    Song, Yonghai; Cui, Kang; Wang, Li; Chen, Shouhui

    2009-03-11

    Silver nanoparticles (Ag NPs) attached to type I collagen-modified glassy carbon (GC) electrodes were successfully synthesized by the electrodepositing method. Atomic force microscopy images showed that many Ag NPs with homogeneous size were formed and uniformly distributed on the type I collagen/GC electrode. The amount, size and distribution of Ag NPs could be controlled by the collagen. The results of electrochemical experiments showed that Ag NPs had an excellent catalytic ability for the reduction of hydrogen peroxide (H(2)O(2)), suggesting that they could be used as a sensor to determine H(2)O(2). The good catalytic activity of the Ag NPs was ascribed to the type I collagen that resulted in the homogeneous distribution of Ag NPs with small size. The effects of type I collagen concentration and electrodeposition time on Ag NPs were investigated. When the Ag NPs were used as a sensor to determine H(2)O(2), the sensor could achieve 95% of the steady-state current in less than 2 s and had a linear range of 5.0 microM to 40.6 mM and a 0.7 microM detection limit of H(2)O(2) at a signal-to-noise ratio of 3.

  17. A Third Generation Glucose Biosensor Based on Cellobiose Dehydrogenase Immobilized on a Glassy Carbon Electrode Decorated with Electrodeposited Gold Nanoparticles: Characterization and Application in Human Saliva.

    PubMed

    Bollella, Paolo; Gorton, Lo; Ludwig, Roland; Antiochia, Riccarda

    2017-08-18

    Efficient direct electron transfer (DET) between a cellobiose dehydrogenase mutant from Corynascus thermophilus (CtCDH C291Y) and a novel glassy carbon (GC)-modified electrode, obtained by direct electrodeposition of gold nanoparticles (AuNPs) was realized. The electrode was further modified with a mixed self-assembled monolayer of 4-aminothiophenol (4-APh) and 4-mercaptobenzoic acid (4-MBA), by using glutaraldehyde (GA) as cross-linking agent. The CtCDH C291Y/GA/4-APh,4-MBA/AuNPs/GC platform showed an apparent heterogeneous electron transfer rate constant (ks) of 19.4 ± 0.6 s-1, with an enhanced theoretical and real enzyme surface coverage (Γtheor and Γreal) of 5287 ± 152 pmol cm-2 and 27 ± 2 pmol cm-2, respectively. The modified electrode was successively used as glucose biosensor exhibiting a detection limit of 6.2 μM, an extended linear range from 0.02 to 30 mM, a sensitivity of 3.1 ± 0.1 μA mM-1 cm-2 (R2 = 0.995), excellent stability and good selectivity. These performances compared favourably with other glucose biosensors reported in the literature. Finally, the biosensor was tested to quantify the glucose content in human saliva samples with successful results in terms of both recovery and correlation with glucose blood levels, allowing further considerations on the development of non-invasive glucose monitoring devices.

  18. Adsorptive stripping voltammetric determination of imipramine, trimipramine and desipramine employing titanium dioxide nanoparticles and an Amberlite XAD-2 modified glassy carbon paste electrode.

    PubMed

    Sanghavi, Bankim J; Srivastava, Ashwini K

    2013-03-07

    An Amberlite XAD-2 (XAD2) and titanium dioxide nanoparticles (TNPs) modified glassy carbon paste electrode (XAD2-TNP-GCPE) was developed for the determination of imipramine (IMI), trimipramine (TRI) and desipramine (DES). The electrochemical behavior of these molecules was investigated employing cyclic voltammetry (CV), chronocoulometry (CC), electrochemical impedance spectroscopy (EIS) and adsorptive stripping differential pulse voltammetry (AdSDPV). After optimization of analytical conditions using a XAD2-TNP-GCPE electrode at pH 6.0 phosphate buffer (0.1 M), the peak currents were found to vary linearly with its concentration in the range of 1.30 × 10(-9) to 6.23 × 10(-6) M for IMI, 1.16 × 10(-9) to 6.87 × 10(-6) M for TRI and 1.43 × 10(-9) to 5.68 × 10(-6) M for DES. The detection limits (S/N = 3) of 3.93 × 10(-10), 3.51 × 10(-10) and 4.35 × 10(-10) M were obtained for IMI, TRI and DES respectively using AdSDPV. The prepared modified electrode showed several advantages such as a simple preparation method, high sensitivity, very low detection limits and excellent reproducibility. The proposed method was employed for the determination of IMI, TRI and DES in pharmaceutical formulations, blood serum and urine samples.

  19. Electrochemical DNA biosensor based on poly(2,6-pyridinedicarboxylic acid) modified glassy carbon electrode for the determination of anticancer drug gemcitabine.

    PubMed

    Tığ, Gözde Aydoğdu; Zeybek, Bülent; Pekyardımcı, Şule

    2016-07-01

    In this study, a simple methodology was used to develop a new electrochemical DNA biosensor based on poly(2,6-pyridinedicarboxylic acid) (P(PDCA)) modified glassy carbon electrode (GCE). This modified electrode was used to monitor for the electrochemical interaction between the dsDNA and gemcitabine (GEM) for the first time. A decrease in oxidation signals of guanine after the interaction of the dsDNA with the GEM was used as an indicator for the selective determination of the GEM via differential pulse voltammetry (DPV). The guanine oxidation peak currents were linearly proportional to the concentrations of the GEM in the range of 1-30mgL(‒1). Limit of detection (LOD) and limit of quantification (LOQ) were found to be 0.276mgL(‒1) and 0.922mgL(‒1), respectively. The reproducibility, repeatability, and applicability of the analysis to pharmaceutical dosage forms and human serum samples were also examined. In addition to DPV method, UV-vis and viscosity measurements were utilized to propose the interaction mechanism between the GEM and the dsDNA. The novel DNA biosensor could serve for sensitive, accurate and rapid determination of the GEM.

  20. A molecularly-imprinted electrochemical sensor based on a graphene-Prussian blue composite-modified glassy carbon electrode for the detection of butylated hydroxyanisole in foodstuffs.

    PubMed

    Cui, Min; Liu, Su; Lian, Wenjing; Li, Jie; Xu, Wei; Huang, Jiadong

    2013-10-21

    In this study, we developed a novel molecularly-imprinted electrochemical sensor based on a glassy carbon electrode (GCE) decorated by graphene-Prussian blue (GR-PB) composites for the selective and sensitive determination of butylated hydroxyanisole (BHA). The molecularly-imprinted polymers (MIPs) were synthesized by BHA and pyrrole as the template molecule and functional monomer, respectively. Also, the MIPs were assembled on the surface of the GR-PB/GCE by electropolymerization. The sensor was characterized by cyclic voltammetry (CV), scanning electron microscopy (SEM), electrochemical impedance spectroscopy (EIS) and chronoamperometry. It was confirmed that the synergistic effects of GR and PB could improve the electrochemical response and the sensitivity of the sensor. The linear range of the sensor was from 9 × 10(-8) mol L(-1) to 7 × 10(-5) mol L(-1), with a limit of detection (LOD) of 7.63 × 10(-8) mol L(-1) (S/N = 3). The proposed sensor displayed high selectivity, excellent stability and good reproducibility for the determination of BHA. It was successfully applied to the determination of BHA in real samples.

  1. Determination of Silver(I) by Differential Pulse Voltammetry Using a Glassy Carbon Electrode Modified with Synthesized N-(2-Aminoethyl)-4,4′-Bipyridine

    PubMed Central

    Radulescu, Maria-Cristina; Chira, Ana; Radulescu, Medeea; Bucur, Bogdan; Bucur, Madalina Petruta; Radu, Gabriel Lucian

    2010-01-01

    A new modified glassy carbon electrode (GCE) based on a synthesized N-(2-aminoethyl)-4,4′-bipyridine (ABP) was developed for the determination of Ag(I) by differential pulse voltammetry (DPV). ABP was covalently immobilized on GC electrodes surface using 4-nitrobenzendiazonium (4-NBD) and glutaraldehyde (GA). The Ag(I) ions were preconcentrated by chemical interaction with bipyridine under a negative potential (−0.6 V); then the reduced ions were oxidized by differential pulse voltammetry and a peak was observed at 0.34 V. The calibration curve was linear in the concentration range from 0.05 μM to 1 μM Ag(I) with a detection limit of 0.025 μM and RSD = 3.6%, for 0.4 μM Ag(I). The presence of several common ions in more than 125-fold excess had no effect on the determination of Ag(I). The developed sensor was applied to the determination of Ag(I) in water samples using a standard addition method. PMID:22163530

  2. Development of an analytical method for the determination of polyphenolic compounds in vegetable origin samples by liquid chromatography and pulsed amperometric detection at a glassy carbon electrode.

    PubMed

    Natale, Anna; Nardiello, Donatella; Palermo, Carmen; Muscarella, Marilena; Quinto, Maurizio; Centonze, Diego

    2015-11-13

    A sensitive and accurate method for the determination of polyphenolic compounds in artichoke bract extracts and olive mill wastewaters by liquid chromatography coupled with pulsed amperometric detection at a glassy carbon working electrode was developed. Preliminary experiments were carried out by cyclic voltammetry to investigate the electrochemical behavior of polyphenols under different mobile phase compositions, and to test the detection and cleaning electrode potentials. Chromatographic separations were performed by using a core-shell C18 column, eluted with acetic acid and acetonitrile, by combined concave-linear binary gradients. Under the optimized experimental conditions, a good column efficiency and peak symmetry were observed, also for stereo and positional isomeric compounds. The developed three-step potential waveform for pulsed amperometric detection was successfully applied for the sensitive chromatographic determination of polyphenols in artichoke extracts and olive mill wastewaters. Linearity, precision and sensitivity of the proposed method have been evaluated. A wide linear range of response (up to 20 mg/L) has been obtained for all the investigated compounds. Detection and quantification limits in the vegetable origin sample extracts were in the range 0.004-0.6 mg/L and 0.01-2mg/L, respectively, while the injection-to-injection repeatability (n=6) ranged from 5 to 13%. The obtained results confirmed the excellent sensitivity of the electrochemical detection, and its suitability for the determination of electroactive polyphenolic compounds at low concentration levels.

  3. Amperometric cholesterol biosensor based on the direct electrochemistry of cholesterol oxidase and catalase on a graphene/ionic liquid-modified glassy carbon electrode.

    PubMed

    Gholivand, Mohammad Bagher; Khodadadian, Mehdi

    2014-03-15

    Cholesterol oxidase (ChOx) and catalase (CAT) were co-immobilized on a graphene/ionic liquid-modified glassy carbon electrode (GR-IL/GCE) to develop a highly sensitive amperometric cholesterol biosensor. The H2O2 generated during the enzymatic reaction of ChOx with cholesterol could be reduced electrocatalytically by immobilized CAT to obtain a sensitive amperometric response to cholesterol. The direct electron transfer between enzymes and electrode surface was investigated by cyclic voltammetry. Both enzymes showed well-defined redox peaks with quasi-reversible behaviors. An excellent sensitivity of 4.163 mA mM(-1)cm(-2), a response time less than 6s, and a linear range of 0.25-215 μM (R(2)>0.99) have been observed for cholesterol determination using the proposed biosensor. The apparent Michaelis-Menten constant (KM(app)) was calculated to be 2.32 mM. The bienzymatic cholesterol biosensor showed good reproducibility (RSDs<5%) with minimal interference from the coexisting electroactive compounds such as ascorbic acid and uric acid. The CAT/ChOx/GR-IL/GCE showed excellent analytical performance for the determination of free cholesterol in human serum samples.

  4. Direct electrochemistry of glucose oxidase immobilized on NdPO4 nanoparticles/chitosan composite film on glassy carbon electrodes and its biosensing application.

    PubMed

    Sheng, Qinglin; Luo, Kai; Li, Lei; Zheng, Jianbin

    2009-02-01

    The direct electrochemistry of glucose oxidase (GOx) immobilized on a composite matrix based on chitosan (CHIT) and NdPO(4) nanoparticles (NPs) underlying on glassy carbon electrode (GCE) was achieved. The cyclic voltammetry and electrochemical impedance spectroscopy were used to characterize the modified electrode. In deaerated buffer solutions, the cyclic voltammetry of the composite films of GOx/NdPO(4) NPs/CHIT showed a pair of well-behaved redox peaks that are assigned to the redox reaction of GOx, confirming the effective immobilization of GOx on the composite film. The electron transfer rate constant was estimated to be 5.0 s(-1). The linear dynamic range for the detection of glucose was 0.15-10 mM with a correlation coefficient of 0.999 and the detection limit was estimated at about 0.08 mM (S/N=3). The calculated apparent Michaelis-Menten constant was 2.5 mM, which suggested a high affinity of the enzyme-substrate. The immobilized GOx in the NdPO(4) NPs/CHIT composite film retained its bioactivity. Furthermore, the method presented here can be easily extended to immobilize and obtain the direct electrochemistry of other redox enzymes or proteins.

  5. Carbon-carbon composites for orthopedic prosthesis and implants. CRADA final report

    SciTech Connect

    Burchell, T D; Klett, J W; Strizak, J P; Baker, C

    1998-01-21

    The prosthetic implant market is extensive. For example, because of arthritic degeneration of hip and knee cartilage and osteoporotic fractures of the hip, over 200,000 total joint replacements (TJRs) are performed in the United States each year. Current TJR devices are typically metallic (stainless steel, cobalt, or titanium alloy) and are fixed in the bone with polymethylacrylate (PMMA) cement. Carbon-carbon composite materials offer several distinct advantages over metals for TJR prosthesis. Their mechanical properties can be tailored to match more closely the mechanical properties of human bone, and the composite may have up to 25% porosity, the size and distribution of which may be controlled through processing. The porous nature of carbon-carbon composites will allow for the ingrowth of bone, achieving biological fixation, and eliminating the need for PMMA cement fixation.

  6. X-ray photoelectron spectroscopy characterization of high dose carbon-implanted steel and titanium alloys

    NASA Astrophysics Data System (ADS)

    Viviente, J. L.; García, A.; Alonso, F.; Braceras, I.; Oñate, J. I.

    1999-04-01

    A study has been made of the depth dependence of the atomic fraction and chemical bonding states of AISI 440C martensitic stainless steel and Ti-6Al-4V alloy implanted with 75 keV C + at very high doses (above 10 18 ions cm -2), by means of X-ray photoelectron spectroscopy combined with an Ar + sputtering. A Gaussian-like carbon distribution was observed on both materials at the lowest implanted dose. More trapezoidal carbon depth-profiles were found with increasing implanted doses, and a pure carbon layer was observed only on the titanium alloy implanted at the highest dose. The implanted carbon was combined with both base metal and carbon itself to form metallic carbides and graphitic carbon. Furthermore, carbon-enriched carbides were also found by curve fitting the C 1s spectra. The titanium alloy showed a higher carbidic contribution than the steel implanted at the same C + doses. A critical carbon concentrations of about 33 at.% and 23 at.% were measured for the formation of C-C bonds in Ti-6Al-4V and steel samples, respectively. The carbon atoms were bound with metal to form carbidic compounds until these critical concentrations were reached; when this C concentration was exceeded the proportion of C-C bonds increased and resulted in the growth of carbonaceous layers.

  7. Intellectual modifying a bare glassy carbon electrode to fabricate a novel and ultrasensitive electrochemical biosensor: Application to determination of acrylamide in food samples.

    PubMed

    Varmira, Kambiz; Abdi, Omid; Gholivand, Mohammad-Bagher; Goicoechea, Hector C; Jalalvand, Ali R

    2018-01-01

    Acrylamide (AA) is a neurotoxin and carcinogen which is mainly formed in foods containing large quantities of starch processed at high temperatures and its determination is very important to control the quality of foods. In this work, a novel electrochemical biosensor based on hemoglobin-dimethyldioctadecylammonium bromide (HG-DDAB)/platinum-gold-palladium three metallic alloy nanoparticles (PtAuPd NPs)/chitosan-1-ethyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide (Ch-IL)/multiwalled carbon nanotubes-IL (MWCNTs-IL)/glassy carbon electrode (GCE) is proposed for ultrasensitive determination of AA in food samples. Development of the biosensor is based on forming an adduct by the reaction of AA with α-NH2 group of N-terminal valine of HG which decreases the peak current of HG-Fe(+3) reduction. The modifications were characterized by electrochemical impedance spectroscopy (EIS), cyclic voltammetry (CV), energy dispersive X-ray spectroscopic (EDS) and scanning electron microscopy (SEM). Under optimized conditions, the biosensor detected AA by square wave voltammetry (SWV) in two linear concentration ranges of 0.03-39.0nM and 39.0-150.0nM with a limit of detection (LOD) of 0.01nM. The biosensor was able to selective detection of AA even in the presence of high concentrations of common interferents which confirmed that the biosensor is highly selective. Also, the results obtained from further studies confirmed that the proposed biosensor has a short response time (less than 8s), good sensitivity, long term stability, repeatability, and reproducibility. Finally, the proposed biosensor was successfully applied to determine AA in potato chips and its results were comparable to those obtained by gas chromatography-mass spectrometry (GC-MS) as reference method. Copyright © 2017 Elsevier B.V. All rights reserved.

  8. Removal of a mixture tetracycline-tylosin from water based on anodic oxidation on a glassy carbon electrode coupled to activated sludge.

    PubMed

    Yahiaoui, Idris; Aissani-Benissad, Farida; Fourcade, Florence; Amrane, Abdeltif

    2015-01-01

    The purpose of this study was first to examine the electrochemical oxidation of two antibiotics, tetracycline (TC) and tylosin (Tylo), considered separately or in mixture, on a glassy carbon electrode in aqueous solutions; and then to assess the relevance of such electrochemical process as a pre-treatment prior to a biological treatment (activated sludge) for the removal of these antibiotics. The influence of the working potential and the initial concentration of TC and Tylo on the electrochemical pre-treatment process was also investigated. It was noticed that antibiotics degradation was favoured at high potential (2.4 V/ saturated calomel electrode (SCE)), achieving total degradation after 50 min for TC and 40 min for Tylo for 50 mg L(-1) initial concentration, with a higher mineralization efficiency in the case of TC. The biological oxygen demand in 5 days (BOD5)/Chemical oxygen demand (COD) ratio increased substantially, from 0.033 to 0.39 and from 0.038 to 0.50 for TC and Tylo, respectively. Regarding the mixture (TC and Tylo), the mineralization yield increased from 10.6% to 30.0% within 60 min of reaction time when the potential increased from 1.5 to 2.4 V/SCE and the BOD5/COD ratio increased substantially from 0.010 initially to 0.29 after 6 h of electrochemical pre-treatment. A biological treatment was, therefore, performed aerobically during 30 days, leading to an overall decrease of 72% of the dissolved organic carbon by means of the combined process.

  9. RBS and GAXRD contributions to yttrium implanted extra low carbon steel characterization

    SciTech Connect

    Caudron, E.; Buscail, H.; Jacob, Y.P.; Stroosnijder, M.F.

    1999-02-01

    Extra low carbon steel samples were yttrium implanted using an ion implantation method. Composition and structural studies were carried out before and after yttrium implantations by several analytical and structural techniques (Rutherford backscattering spectrometry, reflection high energy electron diffraction, scanning electron microscopy, X-ray diffraction, and glancing angle X-ray diffraction) to characterize the yttrium implantation effect on extra low carbon steel. The aim of this article is to show the contributions of Rutherford back-scattering spectrometry (RBS) and glancing angle X-ray diffraction (GAXRD) to the determination of yttrium depth profiles in the samples. The results obtained by these techniques are compared to those of the other analyses performed in this work to show the existing correlation between composition and structural studies. Their results allow a better understanding of the effect of yttrium implantation in extra low carbon steel before studying their corrosion resistance at high temperature.

  10. Carbon offers advantages as implant material in human body

    NASA Technical Reports Server (NTRS)

    Benson, J.

    1969-01-01

    Because of such characteristics as high strength and long-term biocompatability, aerospace carbonaceous materials may be used as surgical implants to correct pathological conditions in the body resulting from disease or injury. Examples of possible medical uses include bone replacement, implantation splints and circulatory bypass implants.

  11. Estimation of Protein Absorption on Polymer Material by Carbon-Negative Ion Implantation

    NASA Astrophysics Data System (ADS)

    Yamada, Tetsuya; Tsuji, Hiroshi; Hattori, Mitsutaka; Sommani, Piyanuch; Sato, Hiroko; Gotoh, Yasuhito; Ishikawa, Junzo

    Selective cell attachment on carbon-negative-ion implanted region of polystyrene was already reported by the authors. However, the selectivity and adhesion strength in the cell pattering were partially insufficient. The adhesive proteins called extracellular matrix (ECM), in general, intervene between cell and substrate surface in the cell attachment on the solid surface. Therefore, we considered to obtain clearer selective cell attachment with tighter binding strength on the implanted region of polystyrene when these adhesive proteins precedently adsorbed on the implanted region of polystyrene. In this paper, we have investigated adsorption properties of three kinds of adhesive proteins (gelatin, fibronectin, laminin) and cell attachment properties on precedent protein adsorbed surface of polystyrene modified by carbon negative-ion implantation. Carbon negative ions were implanted into polystyrene at energy of 10 keV with dose in a range of 1×1014~1×1016 ions/cm2. After implantation, the samples were dipped in the protein solutions for 2 hours. Then, the protein adsorption ratio between implanted and unimplanted regions was evaluated by detecting amount of nitrogen atoms on the surface by X-ray photoelectron spectroscopy (XPS). As a result, the protein-precedently-absorbed sample implanted at dose more than 3×1015 ions/cm2 showed the large gelatin adsorption ratio of more than 2, where the much densely populated cell-attachment was observed more than that on the implanted region of polystyrene without precedent adsorption of protein after cell culture.

  12. Carbon, nitrogen, and oxygen ion implantation of stainless steel

    SciTech Connect

    Rej, D.J.; Gavrilov, N.V.; Emlin, D.

    1995-12-31

    Ion implantation experiments of C, N, and O into stainless steel have been performed, with beam-line and plasma source ion implantation methods. Acceleration voltages were varied between 27 and 50 kV, with pulsed ion current densities between 1 and 10 mA/cm{sup 2}. Implanted doses ranged from 0.5 to 3 {times} 10{sup 18}cm{sup -2}, while workpiece temperatures were maintained between 25 and 800 C. Implant concentration profiles, microstructure, and surface mechanical properties of the implanted materials are reported.

  13. Glassy carbon electrode modified with a graphene oxide/poly(o-phenylenediamine) composite for the chemical detection of hydrogen peroxide.

    PubMed

    Nguyen, Van Hoa; Tran, Trung Hieu; Shim, Jae-Jin

    2014-11-01

    Conducting poly(o-phenylenediamine) (POPD)/graphene oxide (GO) composites were prepared using a facile and efficient method involving the in-situ polymerization of OPD in the presence of GO in an aqueous medium. Copper sulfate was used as an oxidative initiator for the polymerization of OPD. Scanning electron microscopy and transmission electron microscopy images showed that POPD microfibrils were formed and distributed relatively uniformly with GO sheets in the obtained composites. X-ray diffraction results revealed the highly crystal structure of POPD. This composite exhibited good catalytic activity and stability. These results highlight the potential applications of POPD/GO composites as excellent electrochemical sensors. The composites were used to modify glass carbon electrodes for the chemical detection of hydrogen peroxide in aqueous media.

  14. A novel third generation uric acid biosensor using uricase electro-activated with ferrocene on a Nafion coated glassy carbon electrode.

    PubMed

    Ghosh, Tanushree; Sarkar, Priyabrata; Turner, Anthony P F

    2015-04-01

    A new uric acid biosensor was constructed using ferrocene (Fc) induced electro-activated uricase (UOx) deposited within Nafion (Naf) on glassy carbon electrode (GCE). Electro-activation of UOx was successfully achieved by cyclic voltammetry through the electrostatic interaction of Fc with Trp residues within the hydrophobic pockets in UOx. The Naf/UOx/Fc composite was characterised by AFM, FTIR and EDX to ensure proper immobilisation. The interaction of Fc with the enzyme was analysed by Trp fluorescence spectroscopy and the α-helicity of the protein was measured by CD spectropolarimetry. The charge transfer resistance (Rct), calculated from electrochemical impedance spectroscopy, for the modified sensor was lowered (1.39 kΩ) and the enzyme efficiency was enhanced by more than two fold as a result of Fc incorporation. Cyclic voltammetry, differential pulse voltammetry and amperometry all demonstrated the excellent response of the Naf/UOx/Fc/GCE biosensor to uric acid. The sensor system generated a linear response over a range of 500 nM to 600 μM UA, with a sensitivity and limit of detection of 1.78 μA μM(-1) and 230 nM, respectively. The heterogeneous rate constant (ks) for UA oxidation was much higher for Naf/UOx/Fc/GCE (1.0 × 10(-4) cm s(-1)) than for Naf/UOx/GCE (8.2 × 10(-5) cm s(-1)). Real samples, i.e. human blood, were tested for serum UA and the sensor yielded accurate results at a 95% confidence limit. Copyright © 2014 Elsevier B.V. All rights reserved.

  15. The Electrode as Organolithium Reagent: Catalyst-Free Covalent Attachment of Electrochemically Active Species to an Azide-Terminated Glassy Carbon Electrode Surface

    SciTech Connect

    Das, Atanu K.; Engelhard, Mark H.; Liu, Fei; Bullock, R. Morris; Roberts, John A.

    2013-12-02

    Glassy carbon electrodes have been activated for modification with azide groups and subsequent coupling with ferrocenyl reagents by a catalyst-free route using lithium acetylide-ethylenediamine complex, and also by the more common Cu(I)-catalyzed alkyne-azide coupling (CuAAC) route, both affording high surface coverages. Electrodes were preconditioned at ambient temperature under nitrogen, and ferrocenyl surface coverages obtained by CuAAC were comparable to those reported with preconditioning at 1000 °C under hydrogen/nitrogen. The reaction of lithium acetylide-ethylenediamine with the azide-terminated electrode affords a 1,2,3-triazolyllithium-terminated surface that is active toward covalent C-C coupling reactions including displacement at an aliphatic halide and nucleophilic addition at an aldehyde. For example, surface ferrocenyl groups were introduced by reaction with (6-iodohexyl)ferrocene; the voltammetry shows narrow, symmetric peaks indicating uniform attachment. Coverages are competitive with those obtained by the CuAAC route. X-ray photoelectron spectroscopic data, presented for each synthetic step, are consistent with the proposed reactions. This research was supported as part of the Center for Molecular Electrocatalysis, an Energy Frontier Research Center funded by the US Department of Energy, Office of Science, Office of Basic Energy Sciences. Pacific Northwest National Laboratory is operated by Battelle for the US Department of Energy. A portion of the research was performed using EMSL, a national scientific user facility sponsored by the Department of Energy's Office of Biological and Environmental Research and located at Pacific Northwest National Laboratory.

  16. Protein/ionic liquid/glassy carbon sensors following analyte focusing by ionic liquid micelle collapse for simultaneous determination of water soluble vitamins in plasma matrices.

    PubMed

    Abd El-Hady, D; Albishri, H M

    2015-07-01

    Two novel sensors based on human serum albumin (HSA)-ionic liquid (IL) and bovine serum albumin (BSA)-ionic liquid (IL) composites modified glassy carbon electrode (GCE) were produced for simultaneous determination of water soluble vitamins B2, B6 and C in human plasma following analytes focusing by IL micelles collapse (AFILMC). For selective and efficient extraction, vitamins were dissolved in 3.0molL(-1) micellar solution of 1-octyl-3-methyl imidazolium bromide IL. The extracted vitamins were hydrodynamically injected by 25mbar for 20s into a running buffer of 12.5mmolL(-1) phosphate at pH 6.0 followed by electrochemical detection (ECD) on protein/1-octyl-3-methyl imidazolium hexafluorophosphate IL/GC sensors. The chemical stability of proposed sensors was achieved up to 7 days without any decomposition of PF6-based IL/protein and adsorption of interfering ions. In the current work, the sensitivity enhancement factor (SEF) up to 5000-fold was achieved using the AFILMC/ECD setup compared to conventional CE/UV. Under optimal conditions, linear calibration graphs were obtained from 0.5, 0.5 and 1.0 to 1500.0µgmL(-1) of vitamins B2, B6 and C, respectively. Detection limits of analytes were ranged from 180.0 to 520.0ngmL(-1). The proposed AFILMC/ECD setup was successfully applied to the assay of trace level quantification of vitamins in human plasma samples and also their binding constants with HSA and BSA were determined. The concurrent use of IL micelles for the proposed separation and detection processes exhibited some advantages, such as, a reduction of use toxic solvents, an efficient extraction and a direct injection of samples with a short-single run. Furthermore, IL micelles, having variable possibility of interactions, facilitated the successful achievements of AFILMC/ECD setup for the quantification of vitamins in plasma matrices.

  17. EDTA assisted highly selective detection of As(3+) on Au nanoparticle modified glassy carbon electrodes: facile in situ electrochemical characterization of Au nanoparticles.

    PubMed

    Chen, Hsiao-Hua; Huang, Jing-Fang

    2014-12-16

    A facile electrochemical characterization technique of Au nanoparticles (AuNPs) developed by Wang et al. ( Wang, Y.; Laborda, E.; Salter, C.; Crossley, A.; Compton, R. G. Analyst 2012 , 137 , 4693 - 4697 ) was used to track the variation in the particle size and density of AuNPs in situ and to assist in optimizing the conditions of analysis and catalysis. In this method, the combination of total surface area determined by Pb underpotential deposition (UPD) and the amount of Au obtained by anodic stripping of Au in HCl solution was used to evaluate the average diameter of AuNPs and the number of particles on the electrode. The detection of As(3+) in aqueous solution by a AuNP modified glassy carbon electrode (Aunano@GCE) using the electrochemical characterization technique was examined. The AuNPs with a uniform shape and size, deposited onto the GCEs using multiple-scan cyclic voltammetry (MSCV), were suitable for the electrochemical evaluation. The calibration curve for the detection of As(3+) had a dynamic range of 0.1-15.0 μg L(-1) (from 1.30 to 200 nM, y = 0.21x (in μA L μg(-1)) + 0.01 (R(2) = 0.999)) and showed a sensitivity of 0.21 μA L μg(-1) (16.15 μA μM(-1)). A detection limit as low as 0.0025 μg L(-1) (32.5 pM) was achieved. The chelating agent ethylenediaminetetraacetate (EDTA) selectively chelated with the interfering metal ions and effectively inhibited the interfering ions from competing with the ion of interest (As(3+)), in the preconcentration process. The presence of EDTA effectively eliminated interference from several metal ions, especially Cu(2+) and Hg(2+). This method was validated by analyzing the As(3+) content in real water samples.

  18. Chemometric determination of rabeprazole sodium in presence of its acid induced degradation products using spectrophotometry, polarography and anodic voltammetry at a glassy carbon electrode.

    PubMed

    Moneeb, Marwa S

    2008-07-01

    Chemometric stability indicating methods are presented for the determination of rabeprazole sodium in presence of its acid induced degradation products using spectrophotometry, differential pulse polarography and differential pulse anodic voltammetry at a glassy carbon electrode. The applied chemometric techniques are multivariate ones including classical least squares (CLS), principal component regression (PCR) and partial least squares (PLS). A difference spectrophotometric (DeltaA) method has also been applied. To develop the multivariate calibrations, a training set was used, consisting of 20 mixture solutions of rabeprazole sodium and its degradation products. These mixtures show percentage degradation ranging from 0.5-65%, 0.5-95% and 0.6-75% for the spectrophotometric, polarographic and anodic voltammetric calibrations, respectively. The UV absorbances were recorded in 0.1 M NaOH within the wavelength range 220-340 nm at 2 nm intervals. The polarograms and anodic voltammograms were recorded in Britton-Robinson buffer (pH 8.0) within the potential range -500 to -1508 and 400 to 1192 mV at 6 mV intervals with a pulse amplitude of -100 and 50 mV, sweep rate of 15 and 10 mV s(-1) and pulse interval of 0.4 and 0.6 s for the polarographic and anodic voltammetric methods, respectively. All the studied methods have been validated and successfully applied to the determination of rabeprazole sodium in tablet dosage form. The results were statistically compared to those obtained using a published HPLC method. No significant difference has been found.

  19. Electrochemical determination of Ga(III) through formation of Ga(III)-deferrioxamine B nanostructures on the glassy carbon electrode surface.

    PubMed

    Karimi Shervedani, Reza; Garavand, Somayeh; Samiei Foroushani, Marzieh; Yaghoobi, Fatemeh

    2016-03-01

    Selective and sensitive determination of Ga(III) in the presence of Fe(III), as the main interfering ion is studied by using glassy carbon electrode modified with deferrioxamine B (GC-DFO). Characterization and analytical application are performed by different methods including cyclic and differential pulse voltammetry (CV and DPV), electrochemical impedance spectroscopy (EIS), and Field Emission Scanning Electron Microscopy (FESEM). The DPV measurements showed two reduction peaks around -0.630 and -0.830V. While the current of both peaks varied linearly with Ga(III) concentration of the accumulation solution, the latter was more sensitive and used for construction of the calibration curve. The experimental parameters are studied and optimized. A dynamic calibration curve (6.0×10(-11) to 1.4×10(-9)molL(-1)), including a linear part, from 6.0×10(-11) to 1.0×10(-9)molL(-1) with mean RSDs of 5.3% for n=3 at 4.0×10(-10)molL(-1) Ga(III), and a detection limit of 2.0×10(-11) mol L(-1) Ga(III) is observed at the optimized conditions. The validity of the method and applicability of the sensor are successfully tested by determining of Ga(III) in natural (river) waters, rice and coal samples. The experimental data are presented and discussed from which the new sensor is characterized.

  20. Wafer-scale synthesis of multi-layer graphene by high-temperature carbon ion implantation

    NASA Astrophysics Data System (ADS)

    Kim, Janghyuk; Lee, Geonyeop; Kim, Jihyun

    2015-07-01

    We report on the synthesis of wafer-scale (4 in. in diameter) high-quality multi-layer graphene using high-temperature carbon ion implantation on thin Ni films on a substrate of SiO2/Si. Carbon ions were bombarded at 20 keV and a dose of 1 × 1015 cm-2 onto the surface of the Ni/SiO2/Si substrate at a temperature of 500 °C. This was followed by high-temperature activation annealing (600-900 °C) to form a sp2-bonded honeycomb structure. The effects of post-implantation activation annealing conditions were systematically investigated by micro-Raman spectroscopy and transmission electron microscopy. Carbon ion implantation at elevated temperatures allowed a lower activation annealing temperature for fabricating large-area graphene. Our results indicate that carbon-ion implantation provides a facile and direct route for integrating graphene with Si microelectronics.

  1. Surface and corrosion characteristics of carbon plasma implanted and deposited nickel-titanium alloy

    SciTech Connect

    Poon, R.W.Y.; Liu, X.Y.; Chung, C.Y.; Chu, P.K.; Yeung, K.W.K.; Lu, W.W.; Cheung, K.M.C.

    2005-05-01

    Nickel-titanium shape memory alloys (NiTi) are potentially useful in orthopedic implants on account of their super-elastic and shape memory properties. However, the materials are prone to surface corrosion and the most common problem is out-diffusion of harmful Ni ions from the substrate into body tissues and fluids. In order to improve the corrosion resistance and related surface properties, we used the technique of plasma immersion ion implantation and deposition to deposit an amorphous hydrogenated carbon coating onto NiTi and implant carbon into NiTi. Both the deposited amorphous carbon film and carbon plasma implanted samples exhibit much improved corrosion resistances and surface mechanical properties and possible mechanisms are suggested.

  2. The effect of carbon and nitrogen implantation on the abrasion resistance of type IIa (110) diamond

    NASA Astrophysics Data System (ADS)

    Anderson, Gregory C.; Prawer, Steven; Johnston, Peter; McCulloch, Dougal

    1993-06-01

    The possibility of enhancing the wear characteristics of diamond has generated considerable interest. In the present study type IIa diamond has been implanted with 100 keV carbon and nitrogen ions at temperatures of 150, 470 and 920 K. These temperatures correspond to different defect mobility regimes, whilst nitrogen and carbon were chosen in an attempt to examine possible chemical effects of the ion species on the abrasion resistance of type IIa diamond. The results of abrasion testing using low load multiple pass scratch testing with a Rockwell diamond indenter are presented. These indicate that there is an increase in wear rate in both the soft <100> and hard < overline110> directions following ion implantation. For a given dose the wear rate increases as the implant temperature is reduced. Optical transmission spectra taken in the wavelength region 200 to 750 nm show a corresponding trend in that the implantation induced absorption increases with decreasing implant temperature.

  3. Biological properties of carbon/carbon implant composites with unique manufacturing processes.

    PubMed

    Wang, Guo-Hui; Yu, Shu; Zhu, Shai-Hong; Gao, Chang-Qing; Liu, Yong; Miu, Yun-Liang; Huang, Bo-Yun

    2009-12-01

    The goal was to manufacture carbon/carbon (C/C) composites through a unique procedure with improved biocompatibility and reduced debris release. C/C composites were prepared by chemical vapor deposition, and their biological properties were analyzed. With regard to mechanical properties, compressive strength/modulus was 219.1 MPa/9.72 GPa, flexural strength/modulus was 121.63 MPa/21.9 GPa, and interlaminar sheer was 15.13 GPa. Biocompatibility testing revealed: (1) the extract liquid from the C/C composites had no effect on cell proliferation; (2) the extract had no impact on micronucleus frequency as compared with the control groups (P > 0.05); (3) in vivo, there was mild tissue inflammation after implantation within the first 2 weeks, but there was no significant difference compared with the control group (P > 0.05); (4) the implants were well integrated into the host tissue, and debris was limited. The tested samples have excellent biocompatibilities and reduced release of debris. The demonstrated changes in manufacturing procedures are promising.

  4. Formation of complex Al-N-C layer in aluminium by successive carbon and nitrogen implantation

    NASA Astrophysics Data System (ADS)

    Uglov, V. V.; Cherenda, N. N.; Khodasevich, V. V.; Sokol, V. A.; Abramov, I. I.; Danilyuk, A. L.; Wenzel, A.; Gerlach, J.; Rauschenbach, B.

    1999-01-01

    The results of Auger electron spectroscopy and transmission electron microscopy of the surface layer of aluminium after successive implantation by carbon and nitrogen ions are presented in this work. The energy of implanted ions is 40 keV. The implantation dose varies in the range (3.3-6.5) × 10 17 ions/cm 2. The findings show that successive implantation leads to the formation of two main layers in aluminium. The first layer is AlNC x (0 < x < 0.5) layer with violated hcp. AlN structure, where carbon atoms form bonds with nitrogen atoms. The second layer contains disoriented Al 4C 3 precipitates and carbon atoms migrated from the first layer. The mechanism of migration is discussed.

  5. Enzymatic biosensor based on entrapment of d-amino acid oxidase on gold nanofilm/MWCNTs nanocomposite modified glassy carbon electrode by sol-gel network: Analytical applications for d-alanine in human serum.

    PubMed

    Shoja, Yalda; Rafati, Amir Abbas; Ghodsi, Javad

    2017-05-01

    Sensing and determination of d-alanine is studied by using an enzymatic biosensor which was constructed on the basis of d-amino acid oxidase (DAAO) immobilization by sol-gel film onto glassy carbon electrode surface modified with nanocomposite of gold nanofilm (Au-NF) and multiwalled carbon nanotubes (MWCNTs). The Au-NF/MWCNT nanocomposite was prepared by applying the potentiostatic technique for electrodeposition of Au-NF on the MWCNT immobilized on glassy carbon electrode surface. The modified electrode is investigated by scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), linear sweep voltammetry (LSV) and cyclic voltammetry(CV) techniques. The linear sweep voltammetry was used for determination of d-alanine and the results showed an excellent linear relationship between biosensor response and d-alanine concentration ranging from 0.25μM to 4.5μM with correction coefficient of 0.999 (n=20). Detection limit for the fabricated sensor was calculated about 20nM (for S/N=3) and sensitivity was about 56.1μAμM(-1)cm(-2). The developed biosensor exhibited rapid and accurate response to d-alanine, a good stability (4 weeks) and an average recovery of 98.9% in human serum samples. Copyright © 2017 Elsevier Inc. All rights reserved.

  6. Biological and mechanical characterization of carbon fiber frameworks for dental implant applications.

    PubMed

    Menini, Maria; Pesce, Paolo; Pera, Francesco; Barberis, Fabrizio; Lagazzo, Alberto; Bertola, Ludovica; Pera, Paolo

    2017-01-01

    The aim of the present study was to investigate the biocompatibility and mechanical characteristics of dental implant frameworks made of carbon fiber composite. The biocompatibility of intact samples and fragments was evaluated by cell count and MTT test according to EN-ISO 10993-5:2009 directions. Destructive and non-destructive mechanical tests were performed in order to evaluate: porosity, static and dynamic elastic modulus of carbon fiber samples. These tests were conducted on different batches of samples manufactured by different dental technicians. The samples were evaluated by optical microscope and by SEM. A compression test was performed to compare complete implant-supported fixed dentures, provided with a metal or carbon fiber framework. Carbon fiber intact and fragmented samples showed optimal biocompatibility. Manufacture technique strongly influenced the mechanical characteristics of fiber-reinforced composite materials. The implant-supported full-arch fixed denture provided with a carbon fiber framework, showed a yield strength comparable to the implant-supported full-arch fixed denture, provided with a metal framework. Carbon fiber-reinforced composites demonstrated optimal biocompatibility and mechanical characteristics. They appear suitable for the fabrication of frameworks for implant-supported full-arch dentures. Great attention must be paid to manufacture technique as it strongly affects the material mechanical characteristics. Copyright © 2016 Elsevier B.V. All rights reserved.

  7. Ellipsometric and Electrochemical Characterization of Charge Transport in Electroactive Polymers and of the Surface Phase Produced by Electrochemical Activation of Glassy Carbon Electrodes

    NASA Astrophysics Data System (ADS)

    Kepley, Larry Joe

    1990-01-01

    In situ ellipsometry was used to study the electrodeposition of polymer films formed by oxidation of bipyrazine, polyvinylferrocene (PVF), and aniline; the deposition of a viologen-containing siloxane polymer (PQ^{2+/+}) formed by electroreduction of N,N^' -bis (-3-(trimethoxysilyl)propyl) -4,4^ '-bipyridinium dichloride (I) solutions and by spin-casting solutions of I; and the oxidation-dependent swelling of spin-cast films of two structurally similar, ferrocene-containing polyamides. Electrodeposited films displayed good optical characteristics (i.e., high reflectivity, uniform coverage, and homogeneity) for thicknesses up to 400 nm in some cases. Nonideal illipsometric behavior was observed when film morphology varied with film growth. The complex refractive index, film thickness, and the viologen and ferrocene concentrations in the films were measured as a function of oxidation state, both during depositions and after transferring coated-electrodes into blank electrolyte solutions. The voltammetry of the redox polymers was studied and charge-transport modeled by finite -difference simulations of charge diffusion and diffusion coupled to dimerization/monomerization reactions. Equations were derived for linear-sweep voltammetry of a reversible couple in equilibrium with its dimer in a thin-layer cell. Ellipsometric data during electrolysis of the redox films by potential sweeps and steps were compared to theoretical curves for diffusional transport to determine the mechanism of charge transport and to optically measure its rate. The influence of redox-induced thickness changes and solvent sorption on charge transport and voltammetric behavior is described. The electrochemical activation of glassy carbon electrodes for electrolysis of aromatic molecules, such as catechol and hydroquinone, was studied by combined ellipsometric and voltammetric measurements. Ellipsometry was used to detect the anodic growth of nearly transparent layer which activated the surface. X

  8. A novel sensor made of Antimony Doped Tin Oxide-silica composite sol on a glassy carbon electrode modified by single-walled carbon nanotubes for detection of norepinephrine.

    PubMed

    Wang, Zhao; Wang, Kai; Zhao, Lu; Chai, Shigan; Zhang, Jinzhi; Zhang, Xiuhua; Zou, Qichao

    2017-11-01

    In this study, we designed a novel molecularly imprinted polymer (MIP), Antimony Doped Tin Oxide (ATO)-silica composite sol, which was made using a sol-gel method. Then a sensitive and selective imprinted electrochemical sensor was constructed with the ATO-silica composite sol on a glassy carbon electrode modified by single-walled carbon nanotubes (SWNTs). The introduction of SWNTs increased the sensitivity of the MIP sensor. The surface morphology of the MIP and MIP/SWNTs were characterized by scanning electron microscopy (SEM), and the optimal conditions for detection were determined. The oxidative peak current increased linearly with the concentration of norepinephrine in the range of 9.99×10(-8)M to 1.50×10(-5)M, as detected by cyclic voltammetry (CV), the detection limit was 3.33×10(-8)M (S/N=3). In addition, the proposed electrochemical sensors were successfully applied to detect the norepinephrine concentration in human blood serum samples. The recoveries of the sensors varied from 99.67% to 104.17%, indicating that the sensor has potential for the determination of norepinephrine in clinical tests. Moreover, the imprinted electrochemical sensor was used to selectively detect norepinephrine. The analytical application was conducted successfully and yielded accurate and precise results. Copyright © 2017. Published by Elsevier B.V.

  9. Indirect determination of sulfite using a polyphenol oxidase biosensor based on a glassy carbon electrode modified with multi-walled carbon nanotubes and gold nanoparticles within a poly(allylamine hydrochloride) film.

    PubMed

    Sartori, Elen Romão; Vicentini, Fernando Campanhã; Fatibello-Filho, Orlando

    2011-12-15

    The modification of a glassy carbon electrode with multi-walled carbon nanotubes and gold nanoparticles within a poly(allylamine hydrochloride) film for the development of a biosensor is proposed. This approach provides an efficient method used to immobilize polyphenol oxidase (PPO) obtained from the crude extract of sweet potato (Ipomoea batatas (L.) Lam.). The principle of the analytical method is based on the inhibitory effect of sulfite on the activity of PPO, in the reduction reaction of o-quinone to catechol and/or the reaction of o-quinone with sulfite. Under the optimum experimental conditions using the differential pulse voltammetry technique, the analytical curve obtained was linear in the concentration of sulfite in the range from 0.5 to 22 μmol L(-1) with a detection limit of 0.4 μmol L(-1). The biosensor was applied for the determination of sulfite in white and red wine samples with results in close agreement with those results obtained using a reference iodometric method (at a 95% confidence level).

  10. Square-wave adsorptive stripping voltammetric determination of nanomolar levels of bezafibrate using a glassy carbon electrode modified with multi-walled carbon nanotubes within a dihexadecyl hydrogen phosphate film.

    PubMed

    Ardila, Jorge Armando; Oliveira, Geiser Gabriel; Medeiros, Roberta Antigo; Fatibello-Filho, Orlando

    2014-04-07

    A highly sensitive method for bezafibrate determination using a glassy carbon electrode (GCE) modified with multi-walled carbon nanotubes within a dihexadecyl hydrogen phosphate film based on square-wave adsorptive stripping voltammetry (SWAdSV) is proposed. The electrochemical behaviour of bezafibrate has been studied by cyclic voltammetry, showing an irreversible anodic peak at a potential of 1.09 V in 0.1 mol L(-1) phosphate buffer solution (pH 2.0). A study of the scan rate showed that the oxidation of bezafibrate is an adsorptive-controlled process, involving the transfer of two electrons and two protons per molecule. The analytical curve was linear over a bezafibrate concentration range from 50 to 910 nmol L(-1), with a detection limit of 16 nmol L(-1). This analytical method was successfully applied for benzafibrate determination in pharmaceutical formulations, with results showing good agreement with those obtained using a comparative spectrophotometric method, and has the potential for field application.

  11. Simultaneous voltammetric determination of dopamine and epinephrine in human body fluid samples using a glassy carbon electrode modified with nickel oxide nanoparticles and carbon nanotubes within a dihexadecylphosphate film.

    PubMed

    Figueiredo-Filho, Luiz C S; Silva, Tiago A; Vicentini, Fernando C; Fatibello-Filho, Orlando

    2014-06-07

    A simple and highly selective electrochemical method was developed for the single or simultaneous determination of dopamine (DA) and epinephrine (EP) in human body fluids using a glassy carbon electrode modified with nickel oxide nanoparticles and carbon nanotubes within a dihexadecylphosphate film using square-wave voltammetry (SWV) or differential-pulse voltammetry (DPV). Using DPV with the proposed electrode, a separation of ca. 360 mV between the peak reduction potentials of DA and EP present in binary mixtures was obtained. The analytical curves for the simultaneous determination of dopamine and epinephrine showed an excellent linear response, ranging from 7.0 × 10(-8) to 4.8 × 10(-6) and 3.0 × 10(-7) to 9.5 × 10(-6) mol L(-1) for DA and EP, respectively. The detection limits for the simultaneous determination of DA and EP were 5.0 × 10(-8) mol L(-1) and 8.2 × 10(-8) mol L(-1), respectively. The proposed method was successfully applied in the simultaneous determination of these analytes in human body fluid samples of cerebrospinal fluid, human serum and lung fluid.

  12. Electrochemically selective determination of dopamine in the presence of ascorbic and uric acids on the surface of the modified Nafion/single wall carbon nanotube/poly(3-methylthiophene) glassy carbon electrodes.

    PubMed

    Quan, Do Phuc; Tuyen, Do Phuc; Lam, Tran Dai; Tram, Phan Thi Ngoc; Binh, Nguyen Hai; Viet, Pham Hung

    2011-12-01

    A voltammetric method based on a combination of incorporated Nafion, single-walled carbon nanotubes and poly(3-methylthiophene) film-modified glassy carbon electrode (NF/SWCNT/PMT/GCE) has been successfully developed for selective determination of dopamine (DA) in the ternary mixture of dopamine, ascorbic acid (AA) and uric acid (UA) in 0.1M phosphate buffer solution (PBS) pH 4. It was shown that to detect DA from binary DA-AA mixture, the use of NF/PMT/GCE was sufficient, but to detect DA from ternary DA-AA-UA mixture NF/SWCNT/PMT/GCE was required. The later modified electrode exhibits superior electrocatalytic activity towards AA, DA and UA thanks to synergic effect of NF/SWCNT (combining unique properties of SWCNT such as high specific surface area, electrocatalytic and adsorptive properties, with the cation selectivity of NF). On the surface of NF/SWCNT/PMT/GCE AA, DA, UA were oxidized respectively at distinguishable potentials of 0.15, 0.37 and 0.53 V (vs. Ag/AgCl), to form well-defined and sharp peaks, making possible simultaneous determination of each compound. Also, it has several advantages, such as simple preparation method, high sensitivity, low detection limit and excellent reproducibility. Thus, the proposed NF/SWCNT/PMT/GCE could be advantageously employed for the determination of DA in real pharmaceutical formulations.

  13. Poly-Alizarin red S/multiwalled carbon nanotube modified glassy carbon electrode for the boost up of electrocatalytic activity towards the investigation of dopamine and simultaneous resolution in the presence of 5-HT: A voltammetric study.

    PubMed

    Reddaiah, K; Madhusudana Reddy, T; Venkata Ramana, D K; Subba Rao, Y

    2016-05-01

    Poly-Alizarin red S/multiwalled carbon nanotube film on the surface of glassy carbon electrode (poly-AzrS/MWCNT/GCE) was synthesized by electrochemical process and was used for the sensitive and selective determination of dopamine (DA) by employing voltammetric techniques. The electrocatalytic response of the modified electrode was found to exhibit admirable activity. The simultaneous determination of dopamine in the presence of serotonin (5-HT) was found to exhibit very good response at poly-AzrS/MWCNTs/GCE. The effect of pH, scan rate, accumulation time and concentration of dopamine was studied at the developed poly-AzrS/MWCNTs/GCE. The poly-AzrS/MWCNTs/GCE exhibited an efficient electron mediating behavior together with well resolved peaks for dopamine, in 0.1 mol/dm(3) phosphate buffer (PBS) solution of pH 7.0. The limit of detection (LOD) and limit of quantification (LOQ) were found to be as 1.89 × 10(-7) mol/dm(3) and 6.312 × 10(-7) mol/dm(3) respectively with a dynamic range from 1 × 10(-6) to 1.8 × 10(-5) mol/dm(3). The interfacial electron transfer behavior of DA was studied by electrochemical impedance spectroscopy (EIS); the studies showed that the charge transfer rate was enhanced at poly-AzrS/MWCNTs/GCE when compared with bare GCE and poly-AzrS/GCE.

  14. Improved device performance by multistep or carbon Co-implants

    SciTech Connect

    Liefting, R. . MESA Research Inst. FOM Inst. for Atomic and Molecular Physics, Amsterdam ); Wijburg, R.C.M.; Wallinga, H. . MESA Research Inst.); Custer, J.S.; Saris, F.W. )

    1994-01-01

    High-energy ion implantation is used for forming the collector in vertical bipolar transistors in a BiCMOS process. Secondary defects, remaining after annealing the implant damage, give rise to an increased leakage current and to collector-emitter shorts. These shorts reduce the transistor yield. The use of multiple step implants or the introduction of a C gettering layer are demonstrated to avoid dislocation formation. Experimental results show that these schemes subsequently lower the leakage current and dramatically increase device yield. The presence of C can cause increased collector/substrate leakage, indicating that the C profile needs to be optimized with respect to the doping profiles.

  15. Mossbauer effect in the ion-implanted iron-carbon alloys

    NASA Technical Reports Server (NTRS)

    Han, K. S.

    1976-01-01

    The concentration dependence of Mossbauer effect in four carbon ion-implanted iron absorbers, which contain carbon as the solute atoms, has been investigated over the range of concentration 0.05 through 1 atomic percent. The specimens were prepared by implanting carbon atoms on each reference iron foil with four different bombarding energies of 250 keV, 160 keV, 140 keV and 80 keV, respectively. Thus, the specimen contains a uniform dosage of carbon atoms which penetrated up to 3,000 A depth of the reference iron. In the measurement of Mossbauer spectra, the backscattering conversion electron counting geometry was used. Typical results of Mossbauer parameters of iron-carbon alloys show that the isomer shift, quadrupole shift, the effective hyperfine splitting of Fe-57, and the intensity ratio exhibit a large variation with the increase of carbon concentration in the environment of iron atoms.

  16. A preliminary biomechanical study of a novel carbon-fibre hip implant versus standard metallic hip implants.

    PubMed

    Bougherara, Habiba; Zdero, Rad; Dubov, Anton; Shah, Suraj; Khurshid, Shaheen; Schemitsch, Emil H

    2011-01-01

    Total hip arthroplasty is a widespread surgical approach for treating severe osteoarthritis of the human hip. Aseptic loosening of standard metallic hip implants due to stress shielding and bone loss has motivated the development of new materials for hip prostheses. Numerically, a three-dimensional finite element (FE) model that mimicked hip implants was used to compare a new hip stem to two commercially available implants. The hip implants simulated were a novel CF/PA12 carbon-fibre polyamide-based composite hip stem, the Exeter hip stem (Stryker, Mahwah, NJ, USA), and the Omnifit Eon (Stryker, Mahwah, NJ, USA). A virtual axial load of 3 kN was applied to the FE model. Strain and stress distributions were computed. Experimentally, the three hip stems had their distal portions rigidly mounted and had strain gauges placed along the surface at 3 medial and 3 lateral locations. Axial loads of 3 kN were applied. Measurements of axial stiffness and strain were taken and compared to FE analysis. The overall linear correlation between FE model versus experimental strains showed reasonable results for the lines-of-best-fit for the Composite (Pearson R(2)=0.69, slope=0.82), Exeter (Pearson R(2)=0.78, slope=0.59), and Omnifit (Pearson R(2)=0.66, slope=0.45), with some divergence for the most distal strain locations. From FE analysis, the von Mises stress range for the Composite stem was much lower than that in the Omnifit and Exeter implants by 200% and 45%, respectively. The preliminary experiments showed that the Composite stem stiffness (1982 N/mm) was lower than the metallic hip stem stiffnesses (Exeter, 2460 N/mm; Omnifit, 2543 N/mm). This is the first assessment of stress, strain, and stiffness of the CF/PA12 carbon-fibre hip stem compared to standard commercially-available devices.

  17. Structural disorder in hard amorphous carbon films implanted with nitrogen ions

    SciTech Connect

    Freire, F.L. Jr.; Franceschini, D.F.; Achete, C.A.; Brusa, R.S.; Mariotto, G.; Karwasz, G.P.; Canteri, R.

    1996-12-31

    Hard amorphous hydrogenated carbon films deposited by self-bias glow discharge were implanted at room temperature with 70 keV-nitrogen ions at fluences between 2.0 and 9.0 {times} 10{sup 16} N/cm{sup 2}. The implanted samples were analyzed by Raman spectroscopy, SIMS and positron annihilation spectroscopy (Doppler broadening technique with the determination of the parameter S). For samples implanted with 2.0 {times} 10{sup 16} N/cm{sup 2} the S parameter follows the vacancies depth profile predicted by Monte Carlo simulation. For higher fluences the authors observed a reduction in the measured value of S. This result is discussed in terms of both hydrogen loss and structural modifications (increase of disorder at local scale and of the number of graphitic domains) induced in the carbon film by ion implantation.

  18. Investigation of electrochemical behavior of lipid lowering agent atorvastatin calcium in aqueous media and its determination from pharmaceutical dosage forms and biological fluids using boron-doped diamond and glassy carbon electrodes.

    PubMed

    Dogan-Topal, Burcu; Uslu, Bengi; Ozkan, Sibel A

    2007-08-01

    The electrochemical behavior of atorvastatin calcium at glassy carbon and boron-doped diamond electrodes has been studied using voltammetric techniques. The possible mechanism of oxidation was discussed with model compounds. The dependence of the peak current and potentials on pH, concentration, scan rate and nature of the buffer were investigated for both electrodes. The oxidation of atorvastatin was irreversible and exhibited a diffusion-controlled fashion on the diamond electrode. A linear response was obtained within the range of 9.65 x 10(-7) - 3.86 x 10(-5) M in 0.1 M H(2)SO(4) solution for both electrodes. The detection limits of a standard solution are estimated to be 2.11 x 10(-7) M with differential pulse voltammetry (DPV) and 2.05 x 10(-7)M with square wave voltammetry (SWV) for glassy carbon electrode, and 2.27 x 10(-7) M with DPV and 1.31 x 10(-7)M with SWV for diamond electrodes in 0.1 M H(2)SO(4) solution. The repeatability of the methods was found good for both electrodes. The methods were fully validated and successfully applied to the high-throughput determination of the drug in tablets, human serum and human urine with good recoveries.

  19. Strength and tribology of bulk and electroformed nickel amorphized by implantation of titanium and carbon

    SciTech Connect

    Myers, S.M.; Knapp, J.A.; Follstaedt, D.M.; Dugger, M.T.; Christenson, T.R.

    1997-10-01

    Dual ion implantation of titanium and carbon was shown to produce an amorphous layer of exceptional strength within annealed bulk Ni and electroformed Ni and Ni{sub 80}Fe{sub 20} materials used in micro-electromechanical systems. The intrinsic elastic and plastic mechanical properties of the implanted region were quantified using nanoindentation testing in conjunction with finite-element modeling, and the results were interpreted in the light of microstructures observed by electron microscopy. The implantation treatment was found to produce substantial reductions in unlubricated friction and wear.

  20. Carbon plasma immersion ion implantation of nickel-titanium shape memory alloys.

    PubMed

    Poon, R W Y; Yeung, K W K; Liu, X Y; Chu, P K; Chung, C Y; Lu, W W; Cheung, K M C; Chan, D

    2005-05-01

    Nickel-titanium (NiTi) shape memory alloys possess super-elasticity in addition to the well-known shape memory effect and are potentially suitable for orthopedic implants. However, a critical concern is the release of harmful Ni ions from the implants into the living tissues. We propose to enhance the corrosion resistance and other surface and biological properties of NiTi using carbon plasma immersion ion implantation and deposition (PIII&D). Our corrosion and simulated body fluid tests indicate that either an ion-mixed amorphous carbon coating fabricated by PIII&D or direct carbon PIII can drastically improve the corrosion resistance and block the out-diffusion of Ni from the materials. Our tribological tests show that the treated surfaces are mechanically more superior and cytotoxicity tests reveal that both sets of plasma-treated samples favor adhesion and proliferation of osteoblasts.

  1. Mechanism for diamond nucleation and growth on single crystal copper surfaces implanted with carbon

    NASA Technical Reports Server (NTRS)

    Ong, T. P.; Xiong, Fulin; Chang, R. P. H.; White, C. W.

    1992-01-01

    The nucleation and growth of diamond crystals on single-crystal copper surfaces implanted with carbon ions is studied. Microwave plasma-enhanced chemical-vapor deposition is used for diamond growth. The single-crystal copper substrates were implanted either at room or elevated temperature with carbon ions prior to diamond nucleation. This procedure leads to the formation of a graphite film on the copper surface which greatly enhances diamond crystallite nucleation. A simple lattice model is constructed for diamond growth on graphite as 111 line (diamond) parallel to 0001 line (graphite) and 110 line (diamond) parallel to 1 1 -2 0 (graphite).

  2. Mechanism for diamond nucleation and growth on single crystal copper surfaces implanted with carbon

    NASA Technical Reports Server (NTRS)

    Ong, T. P.; Xiong, Fulin; Chang, R. P. H.; White, C. W.

    1992-01-01

    The nucleation and growth of diamond crystals on single-crystal copper surfaces implanted with carbon ions is studied. Microwave plasma-enhanced chemical-vapor deposition is used for diamond growth. The single-crystal copper substrates were implanted either at room or elevated temperature with carbon ions prior to diamond nucleation. This procedure leads to the formation of a graphite film on the copper surface which greatly enhances diamond crystallite nucleation. A simple lattice model is constructed for diamond growth on graphite as 111 line (diamond) parallel to 0001 line (graphite) and 110 line (diamond) parallel to 1 1 -2 0 (graphite).

  3. Titanium Implant Osseointegration Problems with Alternate Solutions Using Epoxy/Carbon-Fiber-Reinforced Composite.

    PubMed

    Petersen, Richard C

    2014-12-01

    The aim of the article is to present recent developments in material research with bisphenyl-polymer/carbon-fiber-reinforced composite that have produced highly influential results toward improving upon current titanium bone implant clinical osseointegration success. Titanium is now the standard intra-oral tooth root/bone implant material with biocompatible interface relationships that confer potential osseointegration. Titanium produces a TiO2 oxide surface layer reactively that can provide chemical bonding through various electron interactions as a possible explanation for biocompatibility. Nevertheless, titanium alloy implants produce corrosion particles and fail by mechanisms generally related to surface interaction on bone to promote an inflammation with fibrous aseptic loosening or infection that can require implant removal. Further, lowered oxygen concentrations from poor vasculature at a foreign metal surface interface promote a build-up of host-cell-related electrons as free radicals and proton acid that can encourage infection and inflammation to greatly influence implant failure. To provide improved osseointegration many different coating processes and alternate polymer matrix composite (PMC) solutions have been considered that supply new designing potential to possibly overcome problems with titanium bone implants. Now for important consideration, PMCs have decisive biofunctional fabrication possibilities while maintaining mechanical properties from addition of high-strengthening varied fiber-reinforcement and complex fillers/additives to include hydroxyapatite or antimicrobial incorporation through thermoset polymers that cure at low temperatures. Topics/issues reviewed in this manuscript include titanium corrosion, implant infection, coatings and the new epoxy/carbon-fiber implant results discussing osseointegration with biocompatibility related to nonpolar molecular attractions with secondary bonding, carbon fiber in vivo properties, electrical

  4. Titanium Implant Osseointegration Problems with Alternate Solutions Using Epoxy/Carbon-Fiber-Reinforced Composite

    PubMed Central

    Petersen, Richard C.

    2014-01-01

    The aim of the article is to present recent developments in material research with bisphenyl-polymer/carbon-fiber-reinforced composite that have produced highly influential results toward improving upon current titanium bone implant clinical osseointegration success. Titanium is now the standard intra-oral tooth root/bone implant material with biocompatible interface relationships that confer potential osseointegration. Titanium produces a TiO2 oxide surface layer reactively that can provide chemical bonding through various electron interactions as a possible explanation for biocompatibility. Nevertheless, titanium alloy implants produce corrosion particles and fail by mechanisms generally related to surface interaction on bone to promote an inflammation with fibrous aseptic loosening or infection that can require implant removal. Further, lowered oxygen concentrations from poor vasculature at a foreign metal surface interface promote a build-up of host-cell-related electrons as free radicals and proton acid that can encourage infection and inflammation to greatly influence implant failure. To provide improved osseointegration many different coating processes and alternate polymer matrix composite (PMC) solutions have been considered that supply new designing potential to possibly overcome problems with titanium bone implants. Now for important consideration, PMCs have decisive biofunctional fabrication possibilities while maintaining mechanical properties from addition of high-strengthening varied fiber-reinforcement and complex fillers/additives to include hydroxyapatite or antimicrobial incorporation through thermoset polymers that cure at low temperatures. Topics/issues reviewed in this manuscript include titanium corrosion, implant infection, coatings and the new epoxy/carbon-fiber implant results discussing osseointegration with biocompatibility related to nonpolar molecular attractions with secondary bonding, carbon fiber in vivo properties, electrical

  5. Electrochemical behavior and voltammetric determination of 2,4,6-triaminopyrimidine at glassy carbon electrode modified with multi-walled carbon nanotubes/nafion.

    PubMed

    Yang, Baocheng; Wang, Fei; Guo, Sujuan; Ye, Baoxian

    2010-01-01

    A multi-wall carbon nanotubes (MWCNTs) composite with Nafion was modified on a glass carbon electrode. The modified electrode was then used as a voltammetric sensor in detecting 2,4,6-triaminopyrimidine (TAP). The surface morphology of the Nafion/MWCNTs composite film was characterized by atomic force microscopy (AFM), and the electrochemical behavior of TAP at this sensor was investigated in detail. The results indicated that the Nafion/MWCNTs modified electrode exhibited efficient electrocatalytic oxidation for TAP with relatively high sensitivity, stability and lifetime. Under the optimized condition using linear sweep voltammetry (LSV), the Nafion/MWCNTs modified electrode exhibited a linear voltammetric response for TAP in the concentration range of 2.0 × 10(-7) to 3.6 × 10(-5) mol L(-1), with a detection limit of 5.0 × 10(-8) mol L(-1). The electrode was applied to detect TAP added to human blood serum, with an average recovery value of 101.3%.

  6. Biological and biochemical properties of the carbon composite and polyethylene implant materials.

    PubMed

    Pesáková, V; Smetana, K; Balík, K; Hruska, J; Petrtýl, M; Hulejová, H; Adam, M

    2003-06-01

    We studied the biocompatibility of the carbon composites and polyethylene materials with and without collagen or collagen and proteoglycan cover. We used the in vitro technology to study the adhesion of model cells evalution, their metabolic activity and the production of TNF-alpha as a cytokine model. Under in vivo condition, the biocompatibility of tested polymers were studied in the implantation experiment, subcutaneously in the interscapular region in the laboratory rat. We have found in the in vitro assay favorable proliferation and the smallest production of pro-inflammatory TNF-alpha cytokine in cells adherent to the hydrophobic polyethylene material coated with biological macromolecules. Using in vivo tests performed by the implantation of materials to the rat we demonstrated that the materials are not cytotoxic. The tissue capsule surrounding the implants was not significantly influenced by the type of the implant and the pre-treatment by the biological molecules. However, the foreign-body giant multinucleated cells were observed only in the vicinity of the collagen - covered hydrophobic polyethylene implant. Interestingly, while the collagen coating improved the biocompatibility of tested polymers in vitro, the inflammatory reaction against this covered materials was higher under in vivo conditions. The pre-treatment of carbon composites by both types of biological macromolecules reduced the occurrence of carbon debris in the implantation site. The tested carbon composites and polyethylene materials are not toxic. The pre-treatment of the materials by extracellular matrix components increased their biological tolerance in vitro and reduced implant wears in animal experiment, which can be important for the medical application.

  7. Simultaneous voltammetric detection of dopamine and uric acid at their physiological level in the presence of ascorbic acid using poly(acrylic acid)-multiwalled carbon-nanotube composite-covered glassy-carbon electrode.

    PubMed

    Liu, Aihua; Honma, Itaru; Zhou, Haoshen

    2007-08-30

    The use of poly(acrylic acid) (PAA)-multiwalled carbon-nanotubes (MWNTs) composite-coated glassy-carbon disk electrode (GCE) (PAA-MWNTs/GCE) for the simultaneous determination of physiological level dopamine (DA) and uric acid (UA) in the presence of an excess of ascorbic acid (AA) in a pH 7.4 phosphate-buffered solution was proposed. PAA-MWNTs composite was prepared by mixing of MWNTs powder into 1 mg/ml PAA aqueous solution under sonication. GCE surface was modified with PAA-MWNTs film by casting. AA demonstrates no voltammetric peak at PAA-MWNTs/GCE. The PAA-MWNTs composite is of a high surface area and of affinity for DA and UA adsorption. DA exhibits greatly improved electron-transfer rate and is electro-catalyzed at PAA-MWNTs/GCE. Moreover, the electro-catalytic oxidation of UA at PAA-MWNTs/GCE is observed, which makes it possible to detect lower level UA. Therefore, the enhanced electrocatalytic currents for DA and UA were observed. The anodic peak currents at approximately 0.18 V and 0.35 V increase with the increasing concentrations of DA and UA, respectively, which correspond to the voltammetric peaks of DA and UA, respectively. The linear ranges are 40 nM to 3 microM DA and 0.3 microM to 10 microM UA in the presence of 0.3 mM AA. The lowest detection limits (S/N=3) were 20 nM DA and 110 nM UA.

  8. Selective detection of dopamine in the presence of uric acid using a gold nanoparticles-poly(luminol) hybrid film and multi-walled carbon nanotubes with incorporated β-cyclodextrin modified glassy carbon electrode.

    PubMed

    Jia, Dong; Dai, Jianyuan; Yuan, Hongyan; Lei, Ling; Xiao, Dan

    2011-10-15

    Gold nanoparticles-poly(luminol) (Plu-AuNPs) hybrid film and multi-walled carbon nanotubes with incorporated β-cyclodextrin modified glassy carbon electrode (β-CD-MWCNTs/Plu-AuNPs/GCE) was successfully prepared for simultaneous determination of dopamine (DA) and uric acid (UA). The surface of the modified electrode has been characterized by X-ray photo-electron spectroscopy (XPS), energy dispersive X-ray spectroscopy (EDS), field-emission scanning electron microscope (SEM) and transmission electron microscope (TEM). Cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS) and differential pulse voltammetry (DPV) have been used to investigate the β-CD-MWCNTs/Plu-AuNPs composite film. Gold nanoparticles anchored into poly(luminol) film exhibited catalytic activity for DA. MWCNTs with incorporated β-CD can greatly promote the direct electron transfer. In 0.10 M phosphate buffer solution (PBS, pH 7.0), the DPV response of the β-CD-MWCNTs/Plu-AuNPs/GCE sensor to DA is about 8-fold as compared with the Plu-AuNPs/GCE sensor, and the detection limit for DA is about one order of magnitude lower than the Plu-AuNPs/GCE sensor. The steady-state current response increases linearly with DA concentration from 1.0 × 10(-6) to 5.6 × 10(-5)M with a low detection limit (S/N=3) of 1.9 × 10(-7)M. Moreover, the interferences of ascorbic acid (AA) and uric acid (UA) are effectively diminished. The applicability of the prepared electrode has been demonstrated by measuring DA contents in dopamine hydrochloride injection.

  9. TCAD modeling and simulation of boron deactivation in NMOS carbon-implanted channel

    NASA Astrophysics Data System (ADS)

    Mok, K. R. C.; Benistant, F.; Teo, R. S.; Chu, S.

    2009-06-01

    Carbon co-implant is well known to suppress boron transient enhanced diffusion (TED) in silicon. The modeling of carbon-interstitial clusters (CICs) has been extensively studied and is now widely used in Technology Computer Aided Design (TCAD). It has already been reported in literature that carbon implant in the channel of NMOS transistor is highly effective for the suppression of oxidation-enhanced diffusion (OED) of boron while leading to poor boron activation. In order to account for this deactivation, we need to consider that the active boron equilibrium concentration is modified by the presence of carbon in non-amorphized silicon region with high concentration of interstitials. In this paper, for the first time, we show the effective TCAD modeling of boron deactivation in the presence of carbon in a NMOS transistor. The model is based on boron-carbon-interstitial clusters formed in the non-amorphized silicon region, thereby reducing active boron concentration. The model can be applied to accurately predict variations of threshold voltage as a function of channel length for NMOS devices with carbon implanted into the channel or halo regions. The tool used in this work is a commercial simulator based on the continuum approach.

  10. Suppression of tin precipitation in SiSn alloy layers by implanted carbon

    SciTech Connect

    Gaiduk, P. I.; Lundsgaard Hansen, J. Nylandsted Larsen, A.

    2014-06-09

    By combining transmission electron microscopy and Rutherford backscattering spectrometry, we have identified carbon related suppression of dislocations and tin precipitation in supersaturated molecular-beam epitaxial grown SiSn alloy layers. Secondary ion mass spectrometry has exposed the accumulation of carbon in the SiSn layers after high temperature carbon implantation and high temperature thermal treatment. Strain-enhanced separation of point defects and formation of dopant-defect complexes are suggested to be responsible for the effects. The possibility for carbon assisted segregation-free high temperature growth of heteroepitaxial SiSn/Si and GeSn/Si structures is argued.

  11. Effects of Mo ion implantation on rolling contact fatigue behavior of carbon steel

    SciTech Connect

    Yang, D.; Zhou, J.

    1996-11-01

    Rolling Contact Fatigue (RCF) is one of the most serious material surface damage problems encountered by many critical components, especially in ball-bearing applications. RCF is sensitive to the material strength, hardness, surface morphology, microstructure and stress status, which may be dramatically changed by surface modifications. In present work, the surface modification of molybdenum ion implantation into quenched carbon steel was employed, and RCF tests on the implanted specimens, as well as the unimplanted, were performed. It was found out that carbon steel specimens, with and without ion implantation, have the same fatigue damage characteristics. They both have circular and fan-like pits on the fatigue failed surfaces, with many spherical debris existing in the fan-like pits. However, molybdenum ion implantation reduced the rolling contact fatigue life of quenched carbon steel. The possible reasons are the following: the ion beam current is too large, which causes the specimen to undergo the annealing process and soften during the implantation process; the incident angles of ions are different for different spots of curve specimen surface, which causes the uneven distribution of residual stress. These will promote the crack initiation and propagation.

  12. Suppression of boron diffusion using carbon co-implantation in DRAM

    SciTech Connect

    Lee, Suk Hun; Park, Se Geun; Kim, Shin Deuk; Jung, Hyuck-Chai; Kim, Il Gweon; Kang, Dong-Ho; Kim, Dae Jung; Lee, Kyu Pil; Choi, Joo Sun; Baek, Jung-Woo; Choi, Moonsuk; Park, Yongkook; Choi, Changhwan; Park, Jin-Hong

    2016-10-15

    Highlights: • The impact of Ge + C co-implantation on dopant diffusion was investigated. • DIBL and V{sub TH} variation was improved by Ge + C co-implantation. • The V{sub TH} mismatch and the write characteristics were improved in the DRAM device. - Abstract: In this paper, germanium pre-amorphization implantation (PAI) and carbon co-implantation (Ge + C co-IIP) were applied to suppress boron diffusion. The corresponding characteristics were investigated in terms of the dopant diffusion, device performance, and its application to dynamic random access memory (DRAM). A shallow dopant profile was indicated and the threshold voltage (V{sub TH}) was reduced by approximately 45 mV by Ge + C co-IIP. In the DRAM device, the V{sub TH} mismatch of the sense amplifier NMOS pairs was reduced by approximately 15% and the write characteristics were improved two-fold.

  13. Study of nitrogen implanted amorphous hydrogenated carbon thin films by variable-energy positron annihilation spectroscopy

    SciTech Connect

    Freire, F.L. Jr.; Franceschini, D.F.; Brusa, R.S.; Karwasz, G.R.; Mariotto, G.; Zecca, A.; Achete, C.A.

    1997-03-01

    Hard amorphous hydrogenated carbon ({ital a}-C:H) films deposited by self-bias glow discharge were implanted at room temperature with 70 keV nitrogen ions at fluences between 2.0 and 9.0{times}10{sup 16} N/cm{sup 2}. The implanted samples were analyzed by positron Doppler broadening annihilation spectroscopy to determine the voids distribution. For samples implanted with 2.0{times}10{sup 16} N/cm{sup 2} the defect distribution is broader than the vacancies depth profile predicted by Monte Carlo simulation. For higher fluences we observed a reduction of the defect density. These results are discussed in terms of a competition between two processes: ion induced defects and structural modifications induced in the films due to ion implantation. {copyright} {ital 1997 American Institute of Physics.}

  14. Improvement of the corrosion and tribological properties of CSS-42L aerospace bearing steel using carbon ion implantation

    NASA Astrophysics Data System (ADS)

    Wang, Fangfang; Zhou, Chungen; Zheng, Lijing; Zhang, Hu

    2017-01-01

    The aerospace bearings steel CSS-42L was ion implanted by carbon with implantation fluxes of 5 × 1016 ions cm-2. The composition, microstructure and hardness of the carbon implanted samples were characterized using X-ray photoelectron spectroscopy, Auger electron spectroscopy, X-ray diffraction, and nanoindentation tests. The corrosion and tribological properties were also evaluated in the present work. The results shown that carbon implantation produced an amorphous layer and graphitic bounds formed at the near surface of CSS-42L steel. In the electrochemical test, the carbon implanted samples suggested lower current densities and corrosion rates. Carbon ion implanted samples shown a relative Cr-enrichment at the surface as compared with nonimplanted samples. The improved corrosion resistance is believed to be related to the formed amorphous layer, the enhancement of Cr diffusion in the carbon implantation layer which contributed the formation of passive film on the surface, the decrease of free electrons which caused by the increase of carbon fraction. The external hard layer had positive effect on the wear resistance, reducing strongly the friction coefficient about 30% and the abrasive-adhesive mechanism present in the unimplanted samples was not modified by the implantation process.

  15. Graphene on silicon dioxide via carbon ion implantation in copper with PMMA-free transfer

    NASA Astrophysics Data System (ADS)

    Lehnert, Jan; Spemann, Daniel; Hamza Hatahet, M.; Mändl, Stephan; Mensing, Michael; Finzel, Annemarie; Varga, Aron; Rauschenbach, Bernd

    2017-06-01

    In this work, a synthesis method for the growth of low-defect large-area graphene using carbon ion beam implantation into metallic Cu foils is presented. The Cu foils (1 cm2 in size) were pre-annealed in a vacuum at 950 °C for 2 h, implanted with 35 keV carbon ions at room temperature, and subsequently annealed at 850 °C for 2 h to form graphene layers with the layer number controlled by the implantation fluence. The graphene was then transferred to SiO2/Si substrates by a PMMA-free wet chemical etching process. The obtained regions of monolayer graphene are of ˜900 μm size. Raman spectroscopy, atomic force microscopy, scanning electron microscopy, and optical microscopy performed at room temperature demonstrated a good quality and homogeneity of the graphene layers, especially for monolayer graphene.

  16. A preparation approach of exploring cluster ion implantation: from ultra-thin carbon film to graphene

    PubMed Central

    2014-01-01

    Based on the extensive application of 2 × 1.7MV Tandetron accelerator, a low-energy cluster chamber has been built to explore for synthesizing graphene. Raman spectrum and atomic force microscopy (AFM) show that an amorphous carbon film in nanometer was deposited on the silicon by C4 cluster implantation. And we replaced the substrate with Ni/SiO2/Si and measured the thickness of Ni film by Rutherford backscattering spectrometry (RBS). Combined with suitable anneal conditions, these samples implanted by various small carbon clusters were made to grow graphene. Results from Raman spectrum reveal that few-layer graphene were obtained and discuss whether IG/I2D can contribute to explain the relationship between the number of graphene layers and cluster implantation dosage. PMID:24910570

  17. Wafer-scale synthesis of multi-layer graphene by high-temperature carbon ion implantation

    SciTech Connect

    Kim, Janghyuk; Lee, Geonyeop; Kim, Jihyun

    2015-07-20

    We report on the synthesis of wafer-scale (4 in. in diameter) high-quality multi-layer graphene using high-temperature carbon ion implantation on thin Ni films on a substrate of SiO{sub 2}/Si. Carbon ions were bombarded at 20 keV and a dose of 1 × 10{sup 15 }cm{sup −2} onto the surface of the Ni/SiO{sub 2}/Si substrate at a temperature of 500 °C. This was followed by high-temperature activation annealing (600–900 °C) to form a sp{sup 2}-bonded honeycomb structure. The effects of post-implantation activation annealing conditions were systematically investigated by micro-Raman spectroscopy and transmission electron microscopy. Carbon ion implantation at elevated temperatures allowed a lower activation annealing temperature for fabricating large-area graphene. Our results indicate that carbon-ion implantation provides a facile and direct route for integrating graphene with Si microelectronics.

  18. Bias in bonding behavior among boron, carbon, and nitrogen atoms in ion implanted a-BN, a-BC, and diamond like carbon films

    SciTech Connect

    Genisel, Mustafa Fatih; Uddin, Md. Nizam; Say, Zafer; Bengu, Erman; Kulakci, Mustafa; Turan, Rasit; Gulseren, Oguz

    2011-10-01

    In this study, we implanted N{sup +} and N{sub 2}{sup +} ions into sputter deposited amorphous boron carbide (a-BC) and diamond like carbon (DLC) thin films in an effort to understand the chemical bonding involved and investigate possible phase separation routes in boron carbon nitride (BCN) films. In addition, we investigated the effect of implanted C{sup +} ions in sputter deposited amorphous boron nitride (a-BN) films. Implanted ion energies for all ion species were set at 40 KeV. Implanted films were then analyzed using x-ray photoelectron spectroscopy (XPS). The changes in the chemical composition and bonding chemistry due to ion-implantation were examined at different depths of the films using sequential ion-beam etching and high resolution XPS analysis cycles. A comparative analysis has been made with the results from sputter deposited BCN films suggesting that implanted nitrogen and carbon atoms behaved very similar to nitrogen and carbon atoms in sputter deposited BCN films. We found that implanted nitrogen atoms would prefer bonding to carbon atoms in the films only if there is no boron atom in the vicinity or after all available boron atoms have been saturated with nitrogen. Implanted carbon atoms also preferred to either bond with available boron atoms or, more likely bonded with other implanted carbon atoms. These results were also supported by ab-initio density functional theory calculations which indicated that carbon-carbon bonds were energetically preferable to carbon-boron and carbon-nitrogen bonds.

  19. Microfracture technique versus carbon fibre rod implantation for treatment of knee articular cartilage lesions.

    PubMed

    Dasar, U; Gursoy, S; Akkaya, M; Algin, O; Isik, C; Bozkurt, M

    2016-08-01

    To compare the microfracture technique with carbon fibre rod implantation for treatment of knee articular cartilage lesions. 10 men and 30 women aged 22 to 56 (mean, 37.4) years underwent microfracture (n=20) or carbon fibre rod implantation (n=20) for International Cartilage Repair Society grade 3 to 4 knee articular cartilage lesions after a mean of 12.2 months of viscosupplementation and physiotherapy. Clinical outcome at 6 and 12 months was assessed using the Tegner-Lysholm score and modified Cincinnati score. Magnetic resonance imaging (MRI) outcome at 12 months was assessed by a radiologist. The modified magnetic resonance observation of cartilage repair tissue (MOCART) score was evaluated. The 2 groups were comparable in terms of age, body mass index, lesion location, lesion size, duration of symptoms, and coexisting pathology. The microfracture group had a higher preoperative Tegner-Lysholm score (39.4±7.3 vs. 34.4±4.9, p=0.015) and modified Cincinnati score (36.4±7.2 vs. 30.4±4.0, p=0.002) than the carbon fibre rod group. At 12 months, change in both scores was significant within each group (p<0.001) and was higher in the microfracture than carbon fibre rod group (p<0.001). MRI showed minimal regenerative tissue. Lobulation, oedema, and hypertrophy were more commonly found in the regeneration tissue after carbon fibre rod implantation than microfracture. At 12 months, the MOCART score was higher in the microfracture than carbon fibre rod group (59 vs. 47, p<0.001). Microfracture is superior to carbon fibre rod implantation in terms of clinical and radiological outcome.

  20. Glassy carbon electrodes sequentially modified by cysteamine-capped gold nanoparticles and poly(amidoamine) dendrimers generation 4.5 for detecting uric acid in human serum without ascorbic acid interference.

    PubMed

    Ramírez-Segovia, A S; Banda-Alemán, J A; Gutiérrez-Granados, S; Rodríguez, A; Rodríguez, F J; Godínez, Luis A; Bustos, E; Manríquez, J

    2014-02-17

    Glassy carbon electrodes (GCE) were sequentially modified by cysteamine-capped gold nanoparticles (AuNp@cysteamine) and PAMAM dendrimers generation 4.5 bearing 128-COOH peripheral groups (GCE/AuNp@cysteamine/PAMAM), in order to explore their capabilities as electrochemical detectors of uric acid (UA) in human serum samples at pH 2. The results showed that concentrations of UA detected by cyclic voltammetry with GCE/AuNp@cysteamine/PAMAM were comparable (deviation <±10%; limits of detection (LOD) and quantification (LOQ) were 1.7×10(-4) and 5.8×10(-4) mg dL(-1), respectively) to those concentrations obtained using the uricase-based enzymatic-colorimetric method. It was also observed that the presence of dendrimers in the GCE/AuNp@cysteamine/PAMAM system minimizes ascorbic acid (AA) interference during UA oxidation, thus improving the electrocatalytic activity of the gold nanoparticles.

  1. A Hydrogen-Evolving Ni(P2N2)2 Electrocatalyst Covalently Attached to a Glassy Carbon Electrode: Preparation, Characterization, and Catalysis. Comparisons With the Homogeneous Analog

    SciTech Connect

    Das, Atanu K.; Engelhard, Mark H.; Bullock, R. Morris; Roberts, John A.

    2014-07-07

    A hydrogen-evolving homogeneous Ni(P2N2)2 electrocatalyst with peripheral ester groups has been covalently attached to a 1,2,3-triazolyllithium-terminated glassy carbon electrode. The surface-confined complex is an electroctalyst for hydrogen evolution, showing onset of catalytic current at the same potential as the soluble parent complex. X-ray photoemission spectra show excellent agreement between the coupled and homogeneous species. Coverage approaches a dense monolayer. This research was supported as part of the Center for Molecular Electrocatalysis, an Energy Frontier Research Center funded by the US Department of Energy, Office of Science, Office of Basic Energy Sciences. Pacific Northwest National Laboratory is operated by Battelle for the US Department of Energy. The XPS measurements were performed at EMSL, a national scientific user facility sponsored by the Department of Energy's Office of Biological and Environmental Research and located at Pacific Northwest National Laboratory.

  2. Investigation of Wear and Corrosion of a High-Carbon Stellite Alloy for Hip Implants

    NASA Astrophysics Data System (ADS)

    Hu, P. S.; Liu, R.; Liu, J.; McRae, G.

    2014-04-01

    Low-carbon Stellite 21 has been used as hip implant material for a number of decades; however, its limited metal-on-metal bearing has resulted in loosening between the femoral head and the acetabular cup of hip implants. In order to improve the metal-on-metal bearing, it is proposed that a high-carbon alloy, Stellite 720, surface coating be applied on Stellite 21 hip implants to improve mechanical and tribological performance. For this coating to be practical, it must also meet the requirements of corrosion resistance for orthopedic implant materials. In this research, Stellite 720 is investigated with pin-on-disk wear tests, and electrochemical and immersion corrosion tests in simulated human body fluid (Hank's solution; pH 7.4 at temperature of 37°C). The experimental results demonstrate that Stellite 720 exhibits much better wear resistance than Stellite 21, and has the potential for better corrosion resistance as well. The applicability of coating Stellite 21 hip implants with Stellite 720 is discussed.

  3. Hyphenation of ionic liquid albumin glassy carbon biosensor or protein label-free sensor with differential pulse stripping voltammetry for interaction studies of human serum albumin with fenoprofen enantiomers.

    PubMed

    Abd El-Hady, Deia; Youssef, Ahmed K

    2013-04-15

    A new biosensor or protein label-free sensor composed of 1-butyl-3-methylimidazolium hexafluorophosphates (BMIMPF6)-human serum albumin (HSA) film on glassy carbon electrode (GCE) was produced. Unfortunately, the native proteins themselves are often unstable in physiological conditions. Here, we introduced conjugation with ionic liquid (IL) such as BMIMPF6 which improved the stability and binding affinity of protein onto GCE. A rapid, simple and reliable method for the chiral discrimination and real time protein binding studies of fenoprofen enantiomers with HSA was developed by hyphenating ionic liquid albumin glassy carbon (ILAGC) biosensor with differential pulse cathodic stripping voltammetry under physiological conditions. The electrochemical behavior of chiral fenoprofen was monitored by cyclic voltammetry, from which large response was obtained from l-fenoprofen. The surface coverage of fenoprofen enantiomers was calculated by double potential-step chronocoulometry. The binding constants of chiral fenoprofen with HSA were estimated to be 3.2×10(5)±0.3 L mol(-1) and 0.8×10(4)±0.4 L mol(-1) for L- and D-fenoprofen, respectively giving acceptable precision (SD ≤ 0.4) and good agreement with the literature values. The competitive interactions of ibuprofen with fenoprofen enantiomers-HSA were studied giving a significant decreasing in the binding degrees of analytes to HSA. The reciprocal competitive experiments indicated that L-fenoprofen replaced D-fenoprofen from HSA. The proposed electrochemical biosensor holds great potential for chiral discrimination and real time binding studies of drugs with protein. Copyright © 2013 Elsevier B.V. All rights reserved.

  4. Simultaneous determination of trace Cd(II), Pb(II) and Cu(II) by differential pulse anodic stripping voltammetry using a reduced graphene oxide-chitosan/poly-l-lysine nanocomposite modified glassy carbon electrode.

    PubMed

    Guo, Zhuo; Li, Dong-di; Luo, Xian-Ke; Li, Ya-Hui; Zhao, Qi-Nai; Li, Meng-Meng; Zhao, Yang-Ting; Sun, Tian-Shuai; Ma, Chi

    2017-03-15

    The reduced graphene oxide (RGO) and Chitosan (CS) hybrid matrix RGO-CS were coated onto the glassy carbon electrode (GCE) surface, then, poly-l-lysine films (PLL) were prepared by electropolymerization with cyclic voltammetry (CV) method to prepare RGO-CS/PLL modified glassy carbon electrode (RGO-CS/PLL/GCE) for the simultaneous electrochemical determination of heavy metal ions Cd(II), Pb(II) and Cu(II). Combining the advantageous features of RGO and CS, RGO and CS are used together because the positively charged CS can interact with the negatively changed RGO to prevent their aggregation. Furthermore, CS has many amino groups along its macromolecular chains and possessed strongly reactive with metal ions. Moreover, PLL modified electrodes have good stability, excellent permselectivity, more active sites and strong adherence to electrode surface, which enhanced electrocatalytic activity. The RGO-CS/PLL/GCE was characterized voltammetrically using redox couples (Fe(CN)6(3-/4-)), complemented with electrochemical impedance spectroscopy (EIS). Differential pulse anodic stripping voltammetry (DPASV) has been used for the detection of Cd(II), Pb(II) and Cu(II). The detection limit of RGO-CS/PLL/GCE toward Cd(II), Pb(II) and Cu(II) is 0.01μgL(-1), 0.02μgL(-1) and 0.02μgL(-1), respectively. The electrochemical parameters that exert influence on deposition and stripping of metal ions, such as supporting electrolytes, pH value, deposition potential, and deposition time, were carefully studied.

  5. A new material with atomized cobalt-multiwalled carbon nanotubes: a possible substitute for human implants.

    PubMed

    Joshi, Bharat; Gupta, Sachin; Kalra, Nitin; Gudyka, Russell; Santhanam, K S V

    2010-06-01

    A new material composed of atomized cobalt-multiwalled carbon nanotube has been produced and characterized by thermogravimetric analysis and polarization studies to estimate its lifetime. This does not show cobalt thermal oxidation suggesting that it is confined inside the carbon nanotube matrix. The density functional calculations in the literature predict a strong interaction leading to higher hybridization of cobalt atom and carbon nanotubes. A detailed investigation of the corrosion measurements shows that the new material of thickness 0.8 mm, 1 mm, 1.5 mm and 2 mm would last for 31, 39, 60 and 79 years and it would substitute with cobalt-chromium alloy that is used as a load bearing implant for patients with knee pain or partial denture implant.

  6. Kinetic Monte Carlo study on the suppression of boron transient enhanced diffusion with carbon pre-implant.

    PubMed

    Park, Soon-Yeol; Sung, Kun-Sik; Won, Taeyoung

    2011-07-01

    We report our kinetic Monte Carlo (kMC) study of the effect of carbon co-implantation on the pre-amorphization implant (PAI) process. We employed the BCA (binary collision approximation) approach for the acquisition of the initial as-implanted dopant profile and the kMC method for the simulation of the diffusion process during the annealing. The simulation results implied that carbon co-implantation suppress boron diffusion due to recombination with interstitials. Also, we could compare boron diffusion with carbon diffusion by calculating the reaction of carbon atoms with interstitials, and we found that boron diffusion was affected by the carbon co-implantation energy by enhancing the trapping of interstitials between boron atoms and interstitials. Our KMC simulation implies that the probability of boron's encounterance with interstitial is reduced due to the carbon trapping between boron and an interstitial and that the effectiveness of co-implanted carbon as a interstitial trap is maximized at an implantation energy of 3 keV.

  7. Near-infrared waveguide in gallium nitride single crystal produced by carbon ion implantation

    NASA Astrophysics Data System (ADS)

    Xiang, Bingxi; Wang, Lei

    2017-05-01

    We report on the fabrication of planar waveguides in gallium nitride by 5 MeV carbon ion implantation with different fluences at room temperature. The waveguides are characterized by prism coupling, Rutherford backscattering/channeling, and high-resolution X-ray diffraction analysis. A positive change in ordinary refractive index is confirmed in the waveguide region at a near-infrared waveband. The thermal stability of the ion-implanted GaN waveguides is investigated by annealing the samples at different temperatures.

  8. Bisphenyl-Polymer/Carbon-Fiber-Reinforced Composite Compared to Titanium Alloy Bone Implant

    PubMed Central

    Petersen, Richard C.

    2014-01-01

    Aerospace/aeronautical thermoset bisphenyl-polymer/carbon-fiber-reinforced composites are considered as new advanced materials to replace metal bone implants. In addition to well-recognized nonpolar chemistry with related bisphenol-polymer estrogenic factors, carbon-fiber-reinforced composites can offer densities and electrical conductivity/resistivity properties close to bone with strengths much higher than metals on a per-weight basis. In vivo bone-marrow tests with Sprague-Dawley rats revealed far-reaching significant osseoconductivity increases from bisphenyl-polymer/carbon-fiber composites when compared to state-of-the-art titanium-6-4 alloy controls. Midtibial percent bone area measured from the implant surface increased when comparing the titanium alloy to the polymer composite from 10.5% to 41.6% at 0.8 mm, P < 10−4, and 19.3% to 77.7% at 0.1 mm, P < 10−8. Carbon-fiber fragments planned to occur in the test designs, instead of producing an inflammation, stimulated bone formation and increased bone integration to the implant. In addition, low-thermal polymer processing allows incorporation of minerals and pharmaceuticals for future major tissue-engineering potential. PMID:25553057

  9. Bisphenyl-Polymer/Carbon-Fiber-Reinforced Composite Compared to Titanium Alloy Bone Implant.

    PubMed

    Petersen, Richard C

    2011-05-03

    Aerospace/aeronautical thermoset bisphenyl-polymer/carbon-fiber-reinforced composites are considered as new advanced materials to replace metal bone implants. In addition to well-recognized nonpolar chemistry with related bisphenol-polymer estrogenic factors, carbon-fiber-reinforced composites can offer densities and electrical conductivity/resistivity properties close to bone with strengths much higher than metals on a per-weight basis. In vivo bone-marrow tests with Sprague-Dawley rats revealed far-reaching significant osseoconductivity increases from bisphenyl-polymer/carbon-fiber composites when compared to state-of-the-art titanium-6-4 alloy controls. Midtibial percent bone area measured from the implant surface increased when comparing the titanium alloy to the polymer composite from 10.5% to 41.6% at 0.8 mm, P < 10(-4), and 19.3% to 77.7% at 0.1 mm, P < 10(-8). Carbon-fiber fragments planned to occur in the test designs, instead of producing an inflammation, stimulated bone formation and increased bone integration to the implant. In addition, low-thermal polymer processing allows incorporation of minerals and pharmaceuticals for future major tissue-engineering potential.

  10. Bioactive Agarose Carbon-Nanotube Composites are Capable of Manipulating Brain-Implant Interface.

    PubMed

    Lewitus, Dan Y; Smith, Karen L; Landers, John; Neimark, Alexander V; Kohn, Joachim

    2014-07-15

    Composite electrodes made of the polysaccharide agarose and carbon nanotube fibers (A-CNE) have shown potential to be applied as tissue-compatible, micro-electronic devices. In the present work, A-CNEs were functionalized using neuro-relevant proteins (laminin and alpha-melanocyte stimulating hormone) and implanted in brain tissue for 1 week (acute response) and 4 weeks (chronic response). Qualitative and quantitative analysis of neuronal and immunological responses revealed significant changes in immunological response to implanted materials depending on the type of biomolecule used. The potential to manipulate tissue response through the use of an anti-inflammatory protein, alpha-melanocyte stimulating hormone, was shown in the reduction of astroglia presence near the implant site during the glial scar formation. These results suggest that A-CNEs, which are soft, flexible, and easily made bioactive, have the ability to modify brain tissue response through surface modification as a function of the biomolecule used.

  11. Bioactive Agarose Carbon-Nanotube Composites are Capable of Manipulating Brain–Implant Interface

    PubMed Central

    Lewitus, Dan Y.; Smith, Karen L.; Landers, John; Neimark, Alexander V.; Kohn, Joachim

    2014-01-01

    Composite electrodes made of the polysaccharide agarose and carbon nanotube fibers (A-CNE) have shown potential to be applied as tissue-compatible, micro-electronic devices. In the present work, A-CNEs were functionalized using neuro-relevant proteins (laminin and alpha-melanocyte stimulating hormone) and implanted in brain tissue for 1 week (acute response) and 4 weeks (chronic response). Qualitative and quantitative analysis of neuronal and immunological responses revealed significant changes in immunological response to implanted materials depending on the type of biomolecule used. The potential to manipulate tissue response through the use of an anti-inflammatory protein, alpha-melanocyte stimulating hormone, was shown in the reduction of astroglia presence near the implant site during the glial scar formation. These results suggest that A-CNEs, which are soft, flexible, and easily made bioactive, have the ability to modify brain tissue response through surface modification as a function of the biomolecule used. PMID:25382868

  12. Friction and Wear Properties of As-Deposited and Carbon Ion-Implanted Diamond Films

    NASA Technical Reports Server (NTRS)

    Miyoshi, Kazuhisa

    1996-01-01

    Recent work on the friction and wear properties of as-deposited and carbon ion-implanted diamond films was reviewed. Diamond films were produced by the microwave plasma chemical vapor deposition (CVD) technique. Diamond films with various grain sizes and surface roughnesses were implanted with carbon ions at 60 keV ion energy, resulting in a dose of 1.2 x 10(exp 17) carbon ions per cm(exp 2). Various analytical techniques, including Raman spectroscopy, proton recoil analysis, Rutherford backscattering, transmission and scanning electron microscopy, X-ray photoelectron spectroscopy, and X-ray diffraction, were utilized to characterize the diamond films. Sliding friction experiments were conducted with a polished natural diamond pin in contact with diamond films in the three environments: humid air (40% relative humidity), dry nitrogen (less than 1 percent relative humidity), and ultrahigh vacuum (10(exp -7) Pa). The CVD diamond films indeed have friction and wear properties similar to those of natural diamond in the three environments. The as-deposited, fine-grain diamond films can be effectively used as self-lubricating, wear-resistant coatings that have low coefficients of friction (0.02 to 0.04) and low wear rates (10(exp -7) to lO(exp -8) mm(exp 3) N(exp -1) m(exp -1)) in both humid air and dry nitrogen. However, they have high coefficients of friction (1.5 to 1.7) and a high wear rate (10(exp -4) mm(exp 7) N(exp -1) m(exp -1)) in ultrahigh vacuum. The carbon ion implantation produced a thin surficial layer (less than 0.1 micron thick) of amorphous, non-diamond carbon on the diamond films. In humid air and dry nitrogen, the ion-implanted, fine and coarse-grain diamond films have a low coefficient of friction (around 0.1) and a low wear rate (10(exp -7) mm(exp 3) N(exp -1) m(exp-1)). Even in ultrahigh vacuum, the presence of the non-diamond carbon layer reduced the coefficient of friction of fine-grain diamond films to 0.1 or lower and the wear rate to 10(exp -6

  13. Nucleation and growth of diamond on carbon-implanted single crystal copper surfaces

    SciTech Connect

    Ong, T.P.; Xiong, F.; Chang, R.P.H. ); White, C.W. )

    1992-09-01

    The nucleation and growth of diamond crystals on single crystal copper surfaces has been studied. Microwave plasma enhanced chemical vapor deposition (MPECVD) was used for diamond nucleation and growth. Prior to diamond nucleation, the single crystal copper surface is modified by carbon ion implantation at an elevated temperature ({similar to}820 {degree}C). This procedure leads to the formation of a graphite film on the copper surface, resulting in an enhancement of diamond crystallite nucleation. A simple lattice model has been constructed to describe the mechanism of diamond nucleation on graphite as {l angle}111{r angle}{sub diamond} parallel to {l angle}0001{r angle}{sub graphite} and {l angle}110{r angle}{sub diamond} parallel to {l angle}1120{r angle}{sub graphite}. This leads to a good understanding of diamond growth on carbon-implanted copper surfaces.

  14. Room temperature diamond-like carbon coatings produced by low energy ion implantation

    NASA Astrophysics Data System (ADS)

    Markwitz, A.; Mohr, B.; Leveneur, J.

    2014-07-01

    Nanometre-smooth diamond-like carbon coatings (DLC) were produced at room temperature with ion implantation using 6 kV C3Hy+ ion beams. Ion beam analysis measurements showed that the coatings contain no heavy Z impurities at the level of 100 ppm, have a homogeneous stoichiometry in depth and a hydrogen concentration of typically 25 at.%. High resolution TEM analysis showed high quality and atomically flat amorphous coatings on wafer silicon. Combined TEM and RBS analysis gave a coating density of 3.25 g cm-3. Raman spectroscopy was performed to probe for sp2/sp3 bonds in the coatings. The results indicate that low energy ion implantation with 6 kV produces hydrogenated amorphous carbon coatings with a sp3 content of about 20%. Results highlight the opportunity of developing room temperature DLC coatings with ion beam technology for industrial applications.

  15. Preparation of graphene on Cu foils by ion implantation with negative carbon clusters

    NASA Astrophysics Data System (ADS)

    Li, Hui; Shang, Yan-Xia; Zhang, Zao-Di; Wang, Ze-Song; Zhang, Rui; Fu, De-Jun

    2015-01-01

    We report on few-layer graphene synthesized on Cu foils by ion implantation using negative carbon cluster ions, followed by annealing at 950 °C in vacuum. Raman spectroscopy reveals IG/I2D values varying from 1.55 to 2.38 depending on energy and dose of the cluster ions, indicating formation of multilayer graphene. The measurements show that the samples with more graphene layers have fewer defects. This is interpreted by graphene growth seeded by the first layers formed via outward diffusion of C from the Cu foil, though nonlinear damage and smoothing effects also play a role. Cluster ion implantation overcomes the solubility limit of carbon in Cu, providing a technique for multilayer graphene synthesis. Project supported by the National Natural Science Foundation of China (Grant Nos. 11105100, 11205116, and 11375135) and the State Key Laboratory of Advanced Welding and Joining, Harbin Institute of Technology, China (Grant No. AWJ-M13-03).

  16. Interfacial shear strength of bioactive-coated carbon fiber reinforced polyetheretherketone after in vivo implantation.

    PubMed

    Nakahara, Ichiro; Takao, Masaki; Goto, Tomoyo; Ohtsuki, Chikara; Hibino, Shigeru; Sugano, Nobuhiko

    2012-10-01

    Despite the excellent osseointegration of carbon-fiber-reinforced polyetheretherketone (CFR/PEEK) with a surface hydroxyapatite (HA) coating, the bone-implant interfacial shear strength of HA-coated CFR/PEEK after osseointegration is unclear. We examined the interfacial shear strength of HA-coated CFR/PEEK implants after in vivo implantation in a rabbit femur-implant pull-out test model. HA coating was performed by a newly developed method. Uncoated CFR/PEEK, HA-coated blasted titanium alloy, and uncoated blasted titanium alloy were used as control implants. The implants were inserted into drilled femoral cortex, and pull-out tests were conducted after 6 and 12 weeks of implantation to determine maximum interfacial shear strength. The HA-coated CFR/PEEK (15.7  ± 4.5 MPa) and HA-coated titanium alloy (14.1  ±  6.0 MPa) exhibited significantly larger interfacial shear strengths than the uncoated CFR/PEEK (7.7 ± 1.8 MPa) and the uncoated titanium alloy (7.8  ±  2.1 MPa) at 6 weeks. At 12 weeks, only the uncoated CFR/PEEK (8.3  ±  3.0 MPa) exhibited a significantly smaller interfacial shear strength, as compared to the HA-coated CFR/PEEK (17.4  ±  3.6 MPa), HA-coated titanium alloy (14.2  ±  4.8 MPa), and uncoated titanium alloy (15.0  ±  2.6 MPa). Surface analysis of the removed implants revealed detachment of the HA layer in both the HA-coated CFR/PEEK and titanium alloy implants. The proposed novel HA coating method of CFR/PEEK significantly increased interfacial shear strength between bone and CFR/PEEK. The achieved interfacial shear strength of the HA-coated CFR/PEEK implant is of the same level as that of grit-blasted titanium alloy with HA. Copyright © 2012 Orthopaedic Research Society.

  17. Endothelial retention and phenotype on carbonized cardiovascular implant surfaces

    PubMed Central

    Frendl, Chris; Tucker, Scott; Khan, Nadeem; Esch, Mandy; Kanduru, Shrinidhi; Cao, Thong M.; García, Andrés J.; King, Michael R.; Butcher, Jonathan T.

    2014-01-01

    Heart valve disease is an increasing clinical burden for which there is no effective treatment outside of prosthetic replacement. Over the last 20 years, clinicians have increasingly preferred the use of biological prosthetics to mechanical valves despite their superior durability because of the lifelong anticoagulation therapy that is required. Mechanical valve surface engineering has largely focused on being as non-thrombogenic as possible, but despite decades of iteration has had insufficient impact on the anticoagulation burden. In this study, we systematically evaluate the potential for endothelialization of the pyrolytic carbon surface used in mechanical valves. We compared adsorbed adhesion ligand type (collagen I, fibronectin, laminin, and purified adhesion domain fragments GFOGER and FN7-10) and concentration on endothelial adhesion rates and adhesion strength on Medtronic-Hall prosthetic valve surfaces. Regardless of ligand type or concentration, endothelial adhesion strengthening was insufficient for their intended ultra-high shear stress environment. We then hypothesized that microfabricated trenches would reduce shear stress to tolerable levels while maintaining endothelial access to the flow stream, thereby promoting a confluent and anticoagulant endothelial monolayer. Computational fluid dynamics simulations predicted an empirical relationship of channel width, depth, and spacing that would maintain interior surface shear stress within tolerable levels. Endothelial cells seeded to confluence in these channels retained a confluent monolayer when exposed to 600 dynes/cm2 shear stress for 48 hours regardless of applied adhesive ligand. Furthermore, sheared EC expressed a mature anti-coagulant profile, including endothelial nitric oxide synthase (eNOS), VE-cadherin, and significantly downregulated plasminogen activator inhibitor-1 (PAI-1). As a final test, channeled pyrolytic carbon surfaces with confluent EC reduced human platelet adhesion 1000-fold

  18. Endothelial retention and phenotype on carbonized cardiovascular implant surfaces.

    PubMed

    Frendl, Christopher M; Tucker, Scott M; Khan, Nadeem A; Esch, Mandy B; Kanduru, Shrinidhi; Cao, Thong M; García, Andrés J; King, Michael R; Butcher, Jonathan T

    2014-09-01

    Heart valve disease is an increasing clinical burden for which there is no effective treatment outside of prosthetic replacement. Over the last 20 years, clinicians have increasingly preferred the use of biological prosthetics to mechanical valves despite their superior durability because of the lifelong anticoagulation therapy that is required. Mechanical valve surface engineering has largely focused on being as non-thrombogenic as possible, but despite decades of iteration has had insufficient impact on the anticoagulation burden. In this study, we systematically evaluate the potential for endothelialization of the pyrolytic carbon surface used in mechanical valves. We compared adsorbed adhesion ligand type (collagen I, fibronectin, laminin, and purified adhesion domain fragments GFOGER and FN7-10) and concentration on endothelial adhesion rates and adhesion strength on Medtronic-Hall prosthetic valve surfaces. Regardless of ligand type or concentration, endothelial adhesion strengthening was insufficient for their intended ultra-high shear stress environment. We then hypothesized that microfabricated trenches would reduce shear stress to tolerable levels while maintaining endothelial access to the flow stream, thereby promoting a confluent and anticoagulant endothelial monolayer. Computational fluid dynamics simulations predicted an empirical relationship of channel width, depth, and spacing that would maintain interior surface shear stress within tolerable levels. Endothelial cells seeded to confluence in these channels retained a confluent monolayer when exposed to 600 dyn/cm(2) shear stress for 48 h regardless of applied adhesive ligand. Furthermore, sheared EC expressed a mature anti-coagulant profile, including endothelial nitric oxide synthase (eNOS), VE-cadherin, and significantly downregulated plasminogen activator inhibitor-1 (PAI-1). As a final test, channeled pyrolytic carbon surfaces with confluent EC reduced human platelet adhesion 1000-fold over

  19. Design and evaluation of carbon nanofiber and silicon materials for neural implant applications

    NASA Astrophysics Data System (ADS)

    McKenzie, Janice L.

    Reduction of glial scar tissue around central nervous system implants is necessary for improved efficacy in chronic applications. Design of materials that possess tunable properties inspired by native biological tissue and elucidation of pertinent cellular interactions with these materials was the motivation for this study. Since nanoscale carbon fibers possess the fundamental dimensional similarities to biological tissue and have attractive material properties needed for neural biomaterial implants, this present study explored cytocompatibility of these materials as well as modifications to traditionally used silicon. On silicon materials, results indicated that nanoscale surface features reduced astrocyte functions, and could be used to guide neurite extension from PC12 cells. Similarly, it was determined that astrocyte functions (key cells in glial scar tissue formation) were reduced on smaller diameter carbon fibers (125 nm or less) while PC12 neurite extension was enhanced on smaller diameter carbon fibers (100 nm or less). Further studies implicated laminin adsorption as a key mechanism in enhancing astrocyte adhesion to larger diameter fibers and at the same time encouraging neurite extension on smaller diameter fibers. Polycarbonate urethane (PCU) was then used as a matrix material for the smaller diameter carbon fibers (100 and 60 nm). These composites proved very versatile since electrical and mechanical properties as well as cell functions and directionality could be influenced by changing bulk and surface composition and features of these matrices. When these composites were modified to be smooth at the micronscale and only rough at the nanoscale, P19 cells actually submerged philopodia, extensions, or whole cells bodies beneath the PCU in order to interact with the carbon nanofibers. These carbon nanofiber composites that have been formulated are a promising material to coat neural probes and thereby enhance functionality at the tissue interface. This

  20. [Carbon fiber reinforced polysulfone implants for tumor surgery of the spine].

    PubMed

    Burri, C; Claes, L; Mutschler, W; Wörsdörfer, O

    1989-12-01

    Anterior tumor removal, cord decompression and spinal stabilization gain in significance in surgical treatment of vertebral tumors. An implant system, consisting of a basket as vertebral body replacement, plates and screws, was developed using carbon fibre reinforced polysulfone. This system allows to perform individually shaped, stable and short-distance spine fusions from an anterior approach. Moreover its radiolucence facilitates postoperative care and irradiation. Operative technique and clinical experience are demonstrated in two patients.

  1. Friction and Wear Properties of As-deposited and Carbon Ion-implanted Diamond Films

    NASA Technical Reports Server (NTRS)

    Miyoshi, Kazuhisa

    1994-01-01

    Recent work on the friction and wear properties of as-deposited and carbon ion-implanted diamond films was reviewed. Diamond films were produced by the microwave plasma chemical vapor deposition (CVD) technique. Diamond films with various grain sizes and surface roughnesses were implanted with carbon ions at 60 ke V ion energy, resulting in a dose of 1.2310(exp 17) carbon ions/cm(exp 2). Various analytical techniques, including Raman spectroscopy, proton recoil analysis, Rutherford backscattering, transmission and scanning electron microscopy, x-ray photoelectron spectroscopy, and x-ray diffraction, were utilized to characterize the diamond films. Sliding friction experiments were conducted with a polished natural diamond pin in contact with diamond films in the three environments: humid air (40 percent relative humidity), dry nitrogen (less than 1 percent relative humidity), and ultrahigh vacuum (10(exp -7) Pa). The CVD diamond films indeed have friction and were properties similar to those of natural diamond in the three environments. The as-deposited, fine-grain diamond films can be effectively used as self-lubricating, wear-resistant coatings that have low coefficients of friction (0.02 to 0.04) and low wear rates (10(exp -7) to 10(exp -8)mm(exp 3)/N-m) in both humid air and dry nitrogen. However, they have high coefficients of friction (1.5 to 1.7) and a high wear rate (10(exp -4)mm(exp 3/N-m) in ultrahigh vacuum. The carbon ion implanation produced a thin surficial layer (less than 0.1 micron thick) of amorphous, nondiamond carbon on the diamond films. In humid air and dry nitrogen, the ion-implanted, fine- and coarse-grain diamond films have a low coefficient of friction (around 0.1) and a low wear rate (10(exp -7)mm(exp 3/N-m). Even in ultrahigh vacuum, the presence of the nondiamond carbon layer reduced the coefficient of friction of fine-grain diamond films to 0.1 or lower and the wear rate to 10(exp -6)mm(exp 3)/N-m. Thus, the carbon ion-implanted, fine

  2. Tissue-compliant neural implants from microfabricated carbon nanotube multilayer composite.

    PubMed

    Zhang, Huanan; Patel, Paras R; Xie, Zhixing; Swanson, Scott D; Wang, Xueding; Kotov, Nicholas A

    2013-09-24

    Current neural prosthetic devices (NPDs) induce chronic inflammation due to complex mechanical and biological reactions related, in part, to staggering discrepancies of mechanical properties with neural tissue. Relatively large size of the implants and traumas to blood-brain barrier contribute to inflammation reactions, as well. Mitigation of these problems and the realization of long-term brain interface require a new generation of NPDs fabricated from flexible materials compliant with the brain tissue. However, such materials will need to display hard-to-combine mechanical and electrical properties which are not available in the toolbox of classical neurotechnology. Moreover, these new materials will concomitantly demand different methods of (a) device micromanufacturing and (b) surgical implantation in brains because currently used processes take advantage of high stiffness of the devices. Carbon nanotubes (CNTs) serve as a promising foundation for such materials because of their record mechanical and electrical properties, but CNT-based tissue-compliant devices have not been realized yet. In this study, we formalize the mechanical requirements to tissue-compliant implants based on critical rupture strength of brain tissue and demonstrate that miniature CNT-based devices can satisfy these requirements. We fabricated them using MEMS-like technology and miniaturized them so that at least two dimensions of the electrodes would be comparable to brain tissue cells. The nanocomposite-based flexible neural electrodes were implanted into the rat motor cortex using a surgical procedure specifically designed for soft tissue-compliant implants. The post-surgery implant localization in the motor cortex was successfully visualized with magnetic resonance and photoacoustic imaging. In vivo functionality was demonstrated by successful registration of the low-frequency neural recording in the live brain of anesthetized rats. Investigation of inflammation processes around these

  3. The Structure of Sapphire Implanted with Carbon at Room Temperature and 1000 deg. C

    SciTech Connect

    Alves, E.; Marques, C.; Safran, G.; McHargue, Carl J.

    2009-03-10

    Carbon was implanted into sapphire at various temperatures as part of a study of the different defect structures produced by a series of light ions. Implantations were made with 150 keV ions to fluences of 1x10{sup 16} and 1x10{sup 17} ions/cm{sup 2} at room temperature (RT) and 1000 deg. C. The defect structures were characterized using Rutherford backscattering-channeling (RBS-C) and transmission electron microscopy (TEM). The RBS-C spectra indicated low residual disorder for RT implantation at 1x10{sup 16} C{sup +}/cm{sup 2}. The de-channeling approached the random value at 1x10{sup 17} C{sup +}/cm{sup 2} and the TEM examination revealed a buried amorphous layer containing embedded sapphire nanocrystals. Damaged layers containing planar defects generally aligned parallel to the surface surrounded this layer. The RBS-C spectra for the sample implanted at 1000 deg. C with 1x10{sup 17} C{sup +}/cm{sup 2} suggested a highly damaged but crystalline surface that was confirmed by TEM micrographs.

  4. Geometrically structured implants for cranial reconstruction made of biodegradable polyesters and calcium phosphate/calcium carbonate.

    PubMed

    Schiller, Carsten; Rasche, Christian; Wehmöller, Michael; Beckmann, Felix; Eufinger, Harald; Epple, Matthias; Weihe, Stephan

    2004-01-01

    The aim of this study was the development of a processing pathway for manufacturing of biodegradable skull implants with individual geometry. The implants on the basis of polylactide and calcium phosphate/calcium carbonate were prepared by a combination of hot pressing and gas foaming. On the inside, the implant consists of a macroporous and faster degradable material (poly(D,L-lactide)+CaCO3) to allow the ingrowth of bone cells. The pore size is in the range of 200-400 microm. On the outside, the implant consists of a compact and slower biodegradable material (poly(L-lactide) and calcium phosphate) to ensure mechanical stability and protection. To overcome problems like inflammatory reactions caused by acidic degradation products of polylactide, the polyester was combined with basic filling materials (calcium salts). The filler neutralises the lactic acid produced during polymer degradation and increases the bioactivity of the material. The stabilised pH was demonstrated by long-term in vitro pH studies. Over a time period of 250 d in demineralised water, the pH was in the physiological range. The in vitro biocompatibility was shown by cell cultures with human osteoblasts. A good proliferation of the cells was observed over the whole test period of 4 weeks.

  5. Optical properties of K9 glass waveguides fabricated by using carbon-ion implantation

    NASA Astrophysics Data System (ADS)

    Liu, Chun-Xiao; Wei, Wei; Fu, Li-Li; Zhu, Xu-Feng; Guo, Hai-Tao; Li, Wei-Nan; Lin, She-Bao

    2016-07-01

    K9 glass is a material with promising properties that make it attractive for optical devices. Ion implantation is a powerful technique to form waveguides with controllable depth and refractive index profile. In this work, optical planar waveguide structures were fabricated in K9 glasses by using 6.0-MeV C3+-ion implantation with a fluence of 1.0 × 1015 ions/cm2. The effective refractive indices of the guided modes were measured by using a prism-coupling system. The refractive index change in the ion-irradiated region was simulated by using the intensity calculation method. The modal intensity profile of the waveguide was calculated and measured by using the finite difference beam propagation method and the end-face coupling technique, respectively. The transmission spectra before and after the implantation showed that the main absorption band was not influenced by the low fluence dopants. The optical properties of the carbon-implanted K9 glass waveguides show promise for use as integrated photonic devices.

  6. The Use of Carbon-Fiber-Reinforced (CFR) PEEK Material in Orthopedic Implants: A Systematic Review

    PubMed Central

    Li, Chuan Silvia; Vannabouathong, Christopher; Sprague, Sheila; Bhandari, Mohit

    2015-01-01

    Carbon-fiber-reinforced polyetheretherketone (CFR-PEEK) has been successfully used in orthopedic implants. The aim of this systematic review is to investigate the properties, technical data, and safety of CFR-PEEK biomaterial and to evaluate its potential for new innovation in the design of articulating medical devices. A comprehensive search in PubMed and EMBASE was conducted to identify articles relevant to the outcomes of CFR-PEEK orthopedic implants. The search was also expanded by reviewing the reference sections of selected papers and references and benchmark reports provided by content experts. A total of 23 articles were included in this review. There is limited literature available assessing the performance of CFR-PEEK, specifically as an implant material for arthroplasty systems. Nevertheless, available studies strongly support CFR-PEEK as a promising and suitable material for orthopedic implants because of its biocompatibility, material characteristics, and mechanical durability. Future studies should continue to investigate CFR-PEEK’s potential benefits. PMID:25780341

  7. Adherent diamond like carbon coatings on metals via plasma source ion implantation

    SciTech Connect

    Walter, K.C.; Nastasi, M.; Munson, C.P.

    1996-12-01

    Various techniques are currently used to produce diamond-like carbon (DLC) coatings on various materials. Many of these techniques use metallic interlayers, such as Ti or Si, to improve the adhesion of a DLC coating to a ferrous substrate. An alternative processing route would be to use plasma source ion implantation (PSII) to create a carbon composition gradient in the surface of the ferrous material to serve as the interface for a DLC coating. The need for interlayer deposition is eliminated by using a such a graded interfaces PSII approach has been used to form adherent DLC coatings on magnesium, aluminum, silicon, titanium, chromium, brass, nickel, and tungsten. A PSII process tailored to create a graded interface allows deposition of adherent DLC coatings even on metals that exhibit a positive heat of formation with carbon, such as magnesium, iron, brass and nickel.

  8. Graphitic carbon in a nanostructured titanium oxycarbide thin film to improve implant osseointegration.

    PubMed

    Zanoni, R; Ioannidu, C A; Mazzola, L; Politi, L; Misiano, C; Longo, G; Falconieri, M; Scandurra, R

    2015-01-01

    A nanostructured coating layer on titanium implants, able to improve their integration into bones and to protect against the harsh conditions of body fluids, was obtained by Ion Plating Plasma Assisted, a method suitable for industrial applications. A titanium carbide target was attached under vacuum to a magnetron sputtering source powered with a direct current in the 500-1100 W range, and a 100 W radio frequency was applied to the sample holder. The samples produced at 900 W gave the best biological response in terms of overexpression of some genes of proteins involved in bone turnover. We report the characterization of a reference and of an implant sample, both obtained at 900 W. Different micro/nanoscopic techniques evidenced the morphology of the substrates, and X-ray Photoelectron Spectroscopy was used to disclose the surface composition. The layer is a 500 nm thick hard nanostructure, composed of 60% graphitic carbon clustered with 15% TiC and 25% Ti oxides.

  9. Irradiation effect of carbon negative-ion implantation on polytetrafluoroethylene for controlling cell-adhesion property

    NASA Astrophysics Data System (ADS)

    Sommani, Piyanuch; Tsuji, Hiroshi; Kojima, Hiroyuki; Sato, Hiroko; Gotoh, Yasuhito; Ishikawa, Junzo; Takaoka, Gikan H.

    2010-10-01

    We have investigated the irradiation effect of negative-ion implantation on the changes of physical surface property of polytetrafluoroethylene (PTFE) for controlling the adhesion property of stem cells. Carbon negative ions were implanted into PTFE sheets at fluences of 1 × 10 14-1 × 10 16 ions/cm 2 and energies of 5-20 keV. Wettability and atomic bonding state including the ion-induced functional groups on the modified surfaces were investigated by water contact angle measurement and XPS analysis, respectively. An initial value of water contact angles on PTFE decreased from 104° to 88° with an increase in ion influence to 1 × 10 16 ions/cm 2, corresponding to the peak shifting of XPS C1s spectra from 292.5 eV to 285 eV with long tail on the left peak-side. The change of peak position was due to decrease of C-F 2 bonds and increase of C-C bonds with the formation of hydrophilic oxygen functional groups of OH and C dbnd O bonds after the ion implantation. After culturing rat mesenchymal stem cells (MSC) for 4 days, the cell-adhesion properties on the C --patterned PTFE were observed by fluorescent microscopy with staining the cell nuclei and their actin filament (F-actin). The clear adhesion patterning of MSCs on the PTFE was obtained at energies of 5-10 keV and a fluence of 1 × 10 15 ions/cm 2. While the sparse patterns and the uncontrollable patterns were found at a low fluence of 3 × 10 14 ions/cm 2 and a high fluence of 3 × 10 15 ions/cm 2, respectively. As a result, we could improve the surface wettability of PTFE to control the cell-adhesion property by carbon negative-ion implantation.

  10. Coating of carbon fiber-reinforced polyetheretherketone implants with titanium to improve bone apposition.

    PubMed

    Devine, Declan M; Hahn, Joachim; Richards, R Geoffery; Gruner, Heiko; Wieling, Ronald; Pearce, Simon G

    2013-05-01

    Carbon fiber-reinforced polyetheretherketone (CF/PEEK) is a thermoplastic composite biomaterial exhibiting properties suitable for load-bearing orthopedic implants. However, the hydrophobic surface of CF/PEEK implants induces the deposition of a peri-implant fibrous tissue capsule preventing bone apposition. However, if bone apposition was improved, the use of CF/PEEK in orthopedics could be increased as it has many advantages compared with metallic implants. In this study, CF/PEEK screws were coated with titanium (Ti) using two different techniques, namely vacuum plasma spraying (VPS) and physical vapor deposition (PVD) with uncoated screws as controls. These coatings were characterized and implanted in a loaded sheep tibia model. In the characterization of the screw surfaces using microscopy techniques, the uncoated screws were seen to have an irregular surface. The PVD coating appeared smooth and consistent, whereas the VPS coating appeared to be a rough coating with some inhomogeneities, which did not cover the entire surface area. Nevertheless, in the ex vivo analysis the VPS-coated screws had a screw removal torque which was statistically greater than uncoated and PVD-coated screws (p ≤ 0.002 for both comparisons). Additionally, the VPS-coated screws had a statistically higher bone contact area than the uncoated screws (p = 0.006), whereas no statistical difference was detected between VPS and PVD coating types (p = 0.11). Thereby illustrating that Ti coating of CF/PEEK screws significantly improve bone apposition and removal torque compared with uncoated CF/PEEK screws. Copyright © 2012 Wiley Periodicals, Inc.

  11. Glassy correlations in nematic elastomers

    NASA Astrophysics Data System (ADS)

    Lu, Bing; Goldbart, Paul; Mao, Xiaoming

    2009-03-01

    We address the physical properties of an isotropic melt or solution of nematogenic polymers that is then cross-linked beyond the vulcanization point. To do this, we construct a replica Landau theory involving a coupled pair of order- parameter fields: one describing vulcanization, the other describing local nematic order. Thermal nematic fluctuations, present at the time of cross-linking, are trapped by cross- linking into the vulcanized network. The resulting glassy nematic fluctuations are analyzed in the Gaussian approximation in two regimes. When the localization length is shorter than the thermal nematic correlation length, the nematic correlations are well captured as glassy correlations. In the opposite regime, fluctuations in the positions of the localized polymers partially wash out the glassy nematic correlations.

  12. Biomimetic synthesis and characterization of cobalt nanoparticles using apoferritin, and investigation of direct electron transfer of Co(NPs)-ferritin at modified glassy carbon electrode to design a novel nanobiosensor.

    PubMed

    Kashanian, Soheila; Abasi Tarighat, Fereshteh; Rafipour, Ronak; Abbasi-Tarighat, Maryam

    2012-09-01

    Oxyhydroxy cobalt CoO(OH) nanoparticles (Co-NPs) were prepared in horse spleen apoferritin (HsAFr) cavity. Transmission electron microscopy revealed the particle size was 5.5-6 nm. Mineralization effect on HsAFr was investigated by fluorescence and far-UV circular dichroism (far-UV CD) spectroscopies. The far-UV CD experiments indicated an increase in the α-helical content after mineralization. Intrinsic fluorescence data showed that mineralization acts as a quencher of HsAFr. For the first time, direct electron transfer between Co(NPs)-HsAFr and a glassy carbon electrode in the thin film of dihexadecylphosphate (DHP) was investigated by cyclic voltammetry (CV) to design a biosensor. The anionic surfactant DHP was used to achieve direct electron-transfer between Co(NPs)-HsAFr molecules and the GC electrode surface. CV result showed clearly a pair of well-defined and quasi-reversible redox peaks arise from Co(NPs)-HsAFr embedded in DHP film. This novel biosensor can be used in medical and industrial fields to detect different analytes.

  13. Electrochemical synthesis of Ag nanoparticles supported on glassy carbon electrode by means of p-isopropyl calix[6]arene matrix and its application for electrocatalytic reduction of H 2O 2

    NASA Astrophysics Data System (ADS)

    Raoof, Jahan Bakhsh; Ojani, Reza; Hasheminejad, Ehteram; Rashid-Nadimi, Sahar

    2012-01-01

    The silver nanoparticles were prepared on the glassy carbon (GC) electrode, modified with p-iso propyl calix[6]arene, by preconcentration of silver ions in open circuit potential and followed by electrochemical reduction of silver ions. The stepwise fabrication process of Ag nanoparticles was characterized by scanning electron microscopy and electrochemical impedance spectroscopy. The prepared Ag nanoparticles were deposited with an average size of 70 nm and a homogeneous distribution on the surface of electrode. The observed results indicated that the presence of calixarene layer on the electrode surface can control the particle size and prevent the agglomeratione and electrochemical deposition is a promising technique for preparation of nanoparticles due to its easy-to-use procedure and low cost of implementation. Cyclic voltammetry experiments showed that Ag nanoparticles had a good catalytic ability for the reduction of hydrogen peroxide (H2O2). The effects of p-isopropyl calix[6]arene concentration, applied potential for reduction of Ag+, number of calixarene layers and pH value on the electrocatalytic ability of Ag nanoparticles were investigated. The present modified electrode exhibited a linear range from 5.0 × 10-5 to 6.5 × 10-3 M and a detection limit 2.7 × 10-5 M of H2O2 (S/N = 3) using amperometric method.

  14. Ion-exchange voltammetry of dopamine at Nafion-coated glassy carbon electrodes: quantitative features of ion-exchange partition and reassessment on the oxidation mechanism of dopamine in the presence of excess ascorbic acid.

    PubMed

    Rocha, Luciana S; Carapuça, Helena M

    2006-10-01

    The incorporation/exclusion features of dopamine (DA), ascorbic acid (AA) and uric acid (UA) are evaluated for Nafion (NA)-coated glassy carbon electrodes (GCE) of different thicknesses. The ion-exchange partition of DA(+) between the NA film and the sodium phosphate electrolyte is evaluated by determining the partition coefficient (k(D)) and the apparent diffusion coefficient (D(app)) in thick NA films which were 401 and 1.5 x 10(-9) cm(2) s(-1), respectively. The solution diffusion coefficient was found to be 6.0 x 10(-6) cm(2) s(-1). Also, the effect of NA loading and of the voltammetric timescale on DA voltammetry in the presence of excess AA is assessed, at physiologic like conditions. It is demonstrated that, although AA is excluded at the NA coating, a catalytic regeneration of DA, induced by AA, occurs at the interface NA film/electrolyte resulting from the diffusion of the o-quinone product of DA oxidation from the electrode surface to that interface. The interference of AA in the voltammetric signal of DA is eliminated using 18 microg mm(-2) NA films and v> or =0.5 V s(-1). Therefore, fast, selective and sensitive voltammetric analysis of DA at concentrations<100 microM in the presence of excess AA, e.g., 1 mM is achieved.

  15. Mixed polyelectrolyte coatings on glassy carbon electrodes: Ion-exchange, permselectivity properties and analytical application of poly-l-lysine-poly(sodium 4-styrenesulfonate)-coated mercury film electrodes for the detection of trace metals.

    PubMed

    Monterroso, Sandra C C; Carapuça, Helena M; Duarte, Armando C

    2006-02-28

    The present work describes the preparation, optimization and characterization of mixed polyelectrolyte coatings of poly-l-lysine (PLL) and poly(sodium 4-styrenesulfonate) (PSS) for the modification of thin mercury film electrodes (MFEs). The novel-modified electrodes were applied in the direct analysis of trace metals in estuarine waters by square-wave anodic stripping voltammetry (SWASV). The effects of the coating morphology and thickness and also of the monomeric molar ratio PLL/PSS on the cation-exchange ability of the PLL-PSS polyelectrolyte coatings onto glassy carbon (GC) were evaluated using target cationic species such as dopamine (DA) or lead cation. Further, the semi-permeability of the PLL-PSS-coated electrodes based both on electrostatic interactions and on molecular size leads to an improved anti-fouling ability against several tensioactive species. The analytical usefulness of the PLL-PSS-mixed polyelectrolyte coatings on thin mercury film electrodes is demonstrated via SWASV measurements of trace metals (lead, copper and cadmium at the low nanomolar level; accumulation time of 180s) in estuarine waters containing moderate levels of dissolved organic matter, resulting in a fast and direct methodology requiring no sample pretreatment.

  16. Direct Quantification of Cd2+ in the Presence of Cu2+ by a Combination of Anodic Stripping Voltammetry Using a Bi-Film-Modified Glassy Carbon Electrode and an Artificial Neural Network

    PubMed Central

    Zhao, Guo; Wang, Hui; Liu, Gang

    2017-01-01

    In this study, a novel method based on a Bi/glassy carbon electrode (Bi/GCE) for quantitatively and directly detecting Cd2+ in the presence of Cu2+ without further electrode modifications by combining square-wave anodic stripping voltammetry (SWASV) and a back-propagation artificial neural network (BP-ANN) has been proposed. The influence of the Cu2+ concentration on the stripping response to Cd2+ was studied. In addition, the effect of the ferrocyanide concentration on the SWASV detection of Cd2+ in the presence of Cu2+ was investigated. A BP-ANN with two inputs and one output was used to establish the nonlinear relationship between the concentration of Cd2+ and the stripping peak currents of Cu2+ and Cd2+. The factors affecting the SWASV detection of Cd2+ and the key parameters of the BP-ANN were optimized. Moreover, the direct calibration model (i.e., adding 0.1 mM ferrocyanide before detection), the BP-ANN model and other prediction models were compared to verify the prediction performance of these models in terms of their mean absolute errors (MAEs), root mean square errors (RMSEs) and correlation coefficients. The BP-ANN model exhibited higher prediction accuracy than the direct calibration model and the other prediction models. Finally, the proposed method was used to detect Cd2+ in soil samples with satisfactory results. PMID:28671628

  17. Generation of non-multilinear three-way voltammetric arrays by an electrochemically oxidized glassy carbon electrode as an efficient electronic device to achieving second-order advantage: challenges, and tailored applications.

    PubMed

    Jalalvand, Ali R; Gholivand, Mohammad-Bagher; Goicoechea, Hector C; Skov, Thomas

    2015-03-01

    For the first time, several second-order calibration models based on artificial neural network-residual bilinearization (ANN-RBL), unfolded-partial least squares-RBL (U-PLS/RBL), multidimensional-partial least squares-RBL (N-PLS/RBL), multivariate curve resolution-alternating least squares (MCR-ALS), and parallel factor analysis 2 (PARAFAC2) were used to exploiting second-order advantage to identify which technique offers the best predictions for the simultaneous quantification of norepinephrine (NE), paracetamol (AC), and uric acid (UA) in the presence of pteroylglutamic acid (FA) as an uncalibrated interference at an electrochemically oxidized glassy carbon electrode (OGCE). Three-way differential pulse voltammetric (DPV) arrays were obtained by recording the DPV signals at different pulse heights. The recorded three-way arrays were both non-bilinear and non-trilinear therefore, the observed shifts in the recorded DPV data were corrected using correlation optimised warping (COW) algorithm. All the algorithms achieved the second-order advantage and were in principle able to overcome the problem of the presence of unexpected interference. Comparison of the performance of the applied second-order chemometric algorithms confirmed the more superiority of U-PLS/RBL to resolve complex systems. The results of applying U-PLS/RBL for the simultaneous quantification of the studied analytes in human serum samples were also encouraging.

  18. Direct Quantification of Cd(2+) in the Presence of Cu(2+) by a Combination of Anodic Stripping Voltammetry Using a Bi-Film-Modified Glassy Carbon Electrode and an Artificial Neural Network.

    PubMed

    Zhao, Guo; Wang, Hui; Liu, Gang

    2017-07-03

    Abstract: In this study, a novel method based on a Bi/glassy carbon electrode (Bi/GCE) for quantitatively and directly detecting Cd(2+) in the presence of Cu(2+) without further electrode modifications by combining square-wave anodic stripping voltammetry (SWASV) and a back-propagation artificial neural network (BP-ANN) has been proposed. The influence of the Cu(2+) concentration on the stripping response to Cd(2+) was studied. In addition, the effect of the ferrocyanide concentration on the SWASV detection of Cd(2+) in the presence of Cu(2+) was investigated. A BP-ANN with two inputs and one output was used to establish the nonlinear relationship between the concentration of Cd(2+) and the stripping peak currents of Cu(2+) and Cd(2+). The factors affecting the SWASV detection of Cd(2+) and the key parameters of the BP-ANN were optimized. Moreover, the direct calibration model (i.e., adding 0.1 mM ferrocyanide before detection), the BP-ANN model and other prediction models were compared to verify the prediction performance of these models in terms of their mean absolute errors (MAEs), root mean square errors (RMSEs) and correlation coefficients. The BP-ANN model exhibited higher prediction accuracy than the direct calibration model and the other prediction models. Finally, the proposed method was used to detect Cd(2+) in soil samples with satisfactory results.

  19. Recrystallization of AlNx (x < 1) thin films induced by N implantation

    NASA Astrophysics Data System (ADS)

    Kobayashi, K.; Namba, S.; Fujihana, T.; Kobayashi, T.; Dai, Y.; Iwaki, M.

    1988-07-01

    The effect of ion implantation on recrystallization of films has been investigated using AlNx (x<1) films as targets. The 750 Å AlNx (x<1) films were deposited on Si(111), glassy carbon, and commercial glass by an activated reactive evaporation method in a nitrogen atmosphere. The 80 keV N+ implantations were carried out near room temperature with doses ranging from 5×1016 to 5×1017 N+ions/cm2 at 1×10-6 Torr. The x-ray diffraction patterns revealed that N implantation enhances a (002) orientation of AlN, growth of which depends on doses. The optical transmittance of the AlNx films is also improved by N implantation, depending on doses. N implantation into AlNx (x<1) even without any annealing is effective for recrystallization of the films, which leads to improvement of optical properties.

  20. Effects of carbon dioxide plasma immersion ion implantation on the electrochemical properties of AZ31 magnesium alloy in physiological environment

    NASA Astrophysics Data System (ADS)

    Xu, Ruizhen; Yang, Xiongbo; Zhang, Xuming; Wang, Mei; Li, Penghui; Zhao, Ying; Wu, Guosong; Chu, Paul K.

    2013-12-01

    Plasma immersion ion implantation (PIII) is conducted to improve the intrinsically poor corrosion properties of biodegradable AZ31 magnesium alloy in the physiological environment. Carbon dioxide is implanted into the samples and X-ray photoelectron spectroscopy and scanning electron microscopy are used to characterize the materials. The corrosion properties are systematically studied by potentiodynamic polarization tests in two simulated physiological environments, namely simulated body fluids and cell culture medium. The plasma-implanted materials exhibit a lower initial corrosion rate. Being a gaseous ion PIII technique, conformal ion implantation into an object with a complex shape such as an orthopedic implant can be easily accomplished and CO2 PIII is a potential method to improve the biological properties of magnesium and its alloys in clinical applications.

  1. The Effect of Carbon Dioxide and Nitrogen ion implantation of AISI 52100 Steel

    NASA Astrophysics Data System (ADS)

    Sari, Amir H.; Ghoranneviss, M.; Mardanian, M.; Hantehzadeh, M. R.; Hora, H.

    2003-06-01

    Ion implantation has been used to modify the mechanical properties of a wide range of metals and alloys using plasma techniques for ion sources and plasma surface treatment [1]. In this study AISI 52100 steel disks, containing 1.5 wt% Cr as the major alloying element, were implanted with nitrogen and carbon dioxide ions at the energy of 90 KeV, with dose in the range 1 × 1018 to 1 × 1019 N2+ ions cm-2, and 3 × 1018 to 1 × 1019 for co2+ ions cm-2. Ion beam current densities and sample temperature, during implantation were 3-6 μA/cm2 and 170°C, respectively. Experiments show, hardness of sample, increases 30-49% using N2+ ions, and 5-17% using co2+ ions. In order to explain the results, formation of beta-CrN and carbide pahses have been carried out using X-ray diffraction technique.

  2. Hydrogenated amorphous carbon coatings on implants drastically reduce biofilm formation and water permeation

    NASA Astrophysics Data System (ADS)

    Bernsmann, Falk; Laube, Norbert; Baldsiefen, Gerhard; Castellucci, Mattia

    2014-11-01

    Inflammations and crystalline bacterial biofilms (encrustations) remain a major complication in long-term artificial urinary tract drainage. To solve this problem we present urological implants with coatings made of amorphous hydrogenated carbon (a-C:H) that show excellent protection from encrustation in-vitro as well as in-vivo. Part of the success of a-C:H coatings is attributed to their ability to act as a diffusion barrier between an implant and the body, which prevents leaching of solvents from polymeric implants. To further enhance their barrier properties a-C:H coatings are combined with parylene coatings to develop diffusion-barrier multilayer coatings with a total thickness between 0.2 μm and 0.8 μm. The combination of the two types of coatings leads to a reduction of water diffusion by a factor of up to ten with respect to uncoated 25 μm thick polyimide sub-strates. The diffusion of water vapour from a controlled atmospheric pressure chamber through coated foils to a vacuum chamber is measured in a custom-built device.

  3. Low-cost carbon thick-film strain sensors for implantable applications

    NASA Astrophysics Data System (ADS)

    Gutierrez, Christian A.; Meng, Ellis

    2010-09-01

    The suitability of low-cost carbon thick-film strain sensors embedded within a biomedical grade silicone rubber (Silastic® MDX4-4210) for implantable applications is investigated. These sensors address the need for robust cost-effective implantable strain sensing technology for the closed loop operation of function-restoring neural prosthetic systems. Design, fabrication and characterization of the sensors are discussed in the context of the application to strain/fullness measurements of the urinary bladder as part of the neuroprosthetic treatment of lower urinary tract dysfunction. The fabrication process, utilizing off-the-shelf screen-printing materials, is convenient and cost effective while achieving resolutions down to 75 µm. This method can also be extended to produce multilayer embedded devices by superposition of different screen-printable materials. Uniaxial loading performance, temperature dependence and long-term soak testing are used to validate suitability for implantation while proof-of-concept operation (up to 40% strain) is demonstrated on a bench-top latex balloon bladder model.

  4. SiC precipitate formation during high dose carbon implantation into silicon

    SciTech Connect

    Lindner, J.K.N.; Volz, K.; Stritzker, B.

    1997-11-01

    The formation of SiC precipitates during the high-dose implantation of carbon ions into Si(100) is studied by means of TEM for implantation conditions, which are suitable for the ion beam synthesis of buried SiC layers in silicon. It is observed that in crystalline silicon nm-sized epitaxially oriented 3C-SiC precipitates are formed which are almost identical in size, nearly independent of the depth and dose (4--9 {times} 10{sup 17} C{sup +}/cm{sup 2}). With increasing dose, it is mainly the density of precipitates which increases. Amorphization of the silicon host lattice leads to depth intervals with a strongly decreased density of oriented crystalline SiC precipitates. The irradiation induced formation of larger randomly oriented SiC crystallites is observed to occur in amorphized regions after prolonged implantation. Both the irradiation induced destruction and formation of SiC precipitates contribute to the generation of a nearly box-shaped precipitate density distribution at doses near the stoichiometry dose.

  5. Tissue Response to, and Degradation Rate of, Photocrosslinked Trimethylene Carbonate-Based Elastomers Following Intramuscular Implantation

    PubMed Central

    Timbart, Laurianne; Tse, Man Yat; Pang, Stephen C.; Amsden, Brian G.

    2010-01-01

    Cylindrical elastomers were prepared through the UV-initiated crosslinking of terminally acrylated, 8,000 Da star-poly(trimethylene carbonate-co-ε-caprolactone) and star-poly(trimethylene carbonate-co-d,l-lactide). These elastomers were implanted intramuscularly into the hind legs of male Wistar rats to determine the influence of the comonomer on the weight loss, tissue response, and change in mechanical properties of the elastomer. The elastomers exhibited only a mild inflammatory response that subsided after the first week; the response was greater for the stiffer d,l-lactide-containing elastomers. The elastomers exhibited weight loss and sol content changes consistent with a bulk degradation mechanism. The d,l-lactide-containing elastomers displayed a nearly zero-order change in Young’s modulus and stress at break over the 30 week degradation time, while the ε-caprolactone-containing elastomers exhibited little change in modulus or stress at break.

  6. Glassy composition for hermetic seals

    DOEpatents

    Wilder, Jr., James A.

    1980-01-01

    The invention relates to a glassy composition adaptable for sealing to aluminum-based alloys to form a hermetically-sealed insulator body. The composition may either be employed as a glass or, after devitrifying heat treatment, as a glass-ceramic.

  7. Characterization and nanomechanical properties of novel dental implant coatings containing copper decorated-carbon nanotubes.

    PubMed

    Sasani, N; Vahdati Khaki, J; Mojtaba Zebarjad, S

    2014-09-01

    Fluorapatite-titania coated Ti-based implants are promising for using in dental surgery for restoring teeth. One of the challenges in implantology is to achieve a bioactive coating with appropriate mechanical properties. In this research, simple sol-gel method was developed for synthesis of fluorapatite-titania-carbon nanotube decorated with antibacterial agent. Triethyl phosphate [PO4(C2H5)3], calcium nitrate [Ca(NO3)2] and ammonium fluoride (NH4F) were used as precursors under an ethanol-water based solution for fluorapatite (FA) production. Titanium isopropoxide and isopropanol were used as starting materials for making TiO2 sol-gels. Also, Copper acetate [Cu(C2H3O2)2·H2O] was used as precursor for decoration of multi walled carbon nanotubes (MWCNTs) with wet chemical method. The decorated MWCNTs (CNT(Cu)) were evaluated by transmission electron microscopy (TEM). The phase identification of the FA-TiO2-CNT(Cu) coating was carried out by XRD analysis. Morphology of coated samples was investigated by SEM observations. The surface elastic modulus and hardness of coatings were studied using nanoindentation technique. The results indicate that novel dental implant coating containing FA, TiO2 and copper decorated MWCNTs have proper morphological features. The results of nanoindentation test show that incorporation of CNT(Cu) in FA-TiO2 matrix can improve the nanomechanical properties of composite coating.

  8. Fabrication of β-cyclodextrin-coated poly (diallyldimethylammonium chloride)-functionalized graphene composite film modified glassy carbon-rotating disk electrode and its application for simultaneous electrochemical determination colorants of sunset yellow and tartrazine.

    PubMed

    Ye, Xiaoliang; Du, Yongling; Lu, Daban; Wang, Chunming

    2013-05-24

    We proposed a green and facile approach for the synthesis of β-cyclodextrin-coated poly(diallyldimethylammonium chloride)-functionalized graphene composite film (β-CD-PDDA-Gr) by using L-ascorbic acid (L-AA) as the reducing agent at room temperature. The β-CD-PDDA-Gr composite film modified glassy carbon-rotating disk electrode (GC-RDE) was then developed for the sensitive simultaneous determination of two synthetic food colorants: sunset yellow (SY) and tartrazine (TT). By cyclic voltammetry (CV), the peak currents of SY and TT increased obviously on the developed electrochemical sensor. The kinetic parameters, such as diffusion coefficient D and standard heterogeneous rate constant kb, were estimated by linear sweep voltammetry (LSV). Under the optimal conditions, the differential pulse voltammetry (DPV) signals of SY and TT on the β-CD-PDDA-Gr modified GC-RDE were significantly enhanced. The enhanced anodic peak currents represented the excellent analytical performance of simultaneous detection of SY and TT in the range of 5.0×10(-8) to 2.0×10(-5) mol L(-1), with a low limit of detection (LOD) of 1.25×10(-8) mol L(-1) for SY and 1.43×10(-8) mol L(-1) for TT (SN(-1)=3). This proposed method displayed outstanding selectivity, good stability and acceptable repeatability and reproducibility, and also has been used to simultaneously determine SY and TT in some commercial soft drinks with satisfactory results. The obtained results were compared to HPLC of analysis for those two colorants and no significant differences were found. By the treatment of the experimental data, the electrochemical reaction mechanisms of SY and TT both involved a one-electron-one-proton-transfer process.

  9. Highly sensitive label free electrochemical detection of VGEF165 tumor marker based on "signal off" and "signal on" strategies using an anti-VEGF165 aptamer immobilized BSA-gold nanoclusters/ionic liquid/glassy carbon electrode.

    PubMed

    Shamsipur, Mojtaba; Farzin, Leila; Amouzadeh Tabrizi, Mahmoud; Molaabasi, Fatemeh

    2015-12-15

    In this work, a label free electrochemical aptasensor for the detection of ultra-traces of vascular endothelial growth factor (VEGF165) based on "signal off" and "signal on" mechanisms of response was developed. The BSA-gold nanoclusters/ionic liquid (BSA-AuNCs/IL) was used as a suitable nanocomposite platform for immobilization of the aptamer on a glassy carbon electrode. In "signal off" mechanism, the interaction of VEGF165 with its anti-VEGF165 aptamers, resulted in desorption of methylene blue (MB) probe from aptamer and its release into solution. Consequently, the decrease in current intensity of the differential pulse voltammogram of adsorbed MB was monitored and found to be linearly proportional with increasing concentration of VEGF165 in sample solution in the range of 1-120 pM with a limit of detection of 0.32p M. While, in "signal on" mechanism, the interaction of immobilized anti-VEGF165 aptamers on the electrode surface with VEGF165, led to more mass-transfer limiting of the [Fe(CN)6](3-/4-) probe to the electrode surface. Therefore, the charge transfer resistance (Rct) of the probe was increased linearly with increasing concentration of VEGF165 in the range of 2.5-250 pM with a limit of detection of 0.48 pM. The experimental results demonstrated that both of these mechanisms are suitable for determination of low levels of the VEGF165 tumor marker in serum samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  10. Anodic Oxidation and Amperometric Sensing of Hydrazine at a Glassy Carbon Electrode Modified with Cobalt (II) Phthalocyanine–cobalt (II) Tetraphenylporphyrin (CoPc-(CoTPP)4) Supramolecular Complex

    PubMed Central

    Ozoemena, Kenneth I.

    2006-01-01

    This paper describes the electrocatalytic behaviour of a glassy carbon electrode (GCE) modified with cobalt(II)phthalocyanine (CoPc) complex peripherally tetrasubstituted with cobalt(II)tetraphenylporphyrin (CoTPP) complexes via ether linkages (i.e., CoPc-(CoTPP)4). The features of the immobilised pentamer were interrogated with cyclic voltammetry and electrochemical impedance spectroscopy (EIS) using [Fe(CN)6]3-/4- as redox probe revealed enhanced electron transfer properties with kapp ≈ 18 × 10-6 cms-1 compared to that of the bare GCE (4.7 × 10-6 cms-1). The viability of this supramolecular complex as a redox mediator for the anodic oxidation and sensitive amperometric determination of hydrazine in alkaline conditions is described. The electrocatalytic oxidation of hydrazine by GCE-CoPc-(CoTPP)4 was characterised with satisfactory catalytic current response with low non-Faradaic current (ca. 30 times lower than the bare GCE) and at much lower oxidation potential (ca. 300 mV lower than the bare GCE). A mechanism for the studied electrocatalytic reaction was proposed based on the spectrophotometric evidence that revealed the major involvement of the Co(III)/Co(II) redox couple of the central CoPc species rather than the CoTPP component of the pentamer. Rate constant for the anodic oxidation of hydrazine was estimated from chronoamperometry as ∼ 3×103 M-1s-1. The proposed amperometric sensor displayed excellent charateristics towards the determination of hydrazine in 0.2 M NaOH; such as low overpotentials (+100 mV vs Ag|AgCl), very fast amperometric response time (1 s), linear concentration range of up to 230 μM, with micromolar detection limit, high sensitivity and stability.

  11. Development of silicon carbide substrates by carbonization and ion implantation of single-crystalline substrates

    NASA Astrophysics Data System (ADS)

    Morales Sanchez, Francisco Miguel

    Mechanisms of formation involved in both thin films and crystalline precipitates of silicon carbide (SiC) are studied in this Ph. D. thesis. SiC is fabricated starting from single-crystalline silicon (Si) substrates by carbonization or by ion implantation. The characterization of these structures allows to gather data and better physical and chemical understanding of these systems. The main objectives are (i) the fabrication and characterization of SiC and other interesting crystalline phases obtained from Si wafers and (ii) to demonstrate that these products are a viable way for using them as templates, compliant, seed or buffer layers in SiC or III-N overgrowth by epitaxial growth techniques. These approaches let the consecution of a crystalline quality enough to the development of devices. Indeed, their use allow a significant reduction of the high defect density present in III-N or SiC alloys compared to their quality when directly grown on Si. Therefore, long life are foreseen for electronic devices that could use these substrates. This is the limit needed for the beginning of their industrial production and commercialization. Samples studied in this work are framed inside three groups: (1) Silicon Carbide and other phases (Silicon Nitride (Si3N4) and carbon nitride (C3N4)) synthesized by Silicon ion implantation, (2) Silicon Carbide synthesized by Si carbonisation and (3) Silicon Carbide and Gallium Nitride heteroepitaxial growth on carbonized Si. All these structures are fabricated by techniques derived from classic (i) Ion Beam Induced Crystallization (IBIC), (ii) Chemical Vapour Deposition (CVD) or (iii) Molecular Beam Epitaxy (MBE). Structural characterizations are carried out mainly by (i) Scanning Electron Microscopy (SEM), (ii) Transmission Electron Microscopy (TEM), (iii) Fourier Transform Infra Red Spectrometry (FTIR) and other techniques.

  12. Immobilization of DNA at Glassy Ccarbon Electrodes: A Critical Study of Adsorbed Layer

    PubMed Central

    Pedano, M. L.; Rivas, G. A.

    2005-01-01

    In this work we present a critical study of the nucleic acid layer immobilized at glassy carbon electrodes. Different studies were performed in order to assess the nature of the interaction between DNA and the electrode surface. The adsorption and electrooxidation of DNA demonstrated to be highly dependent on the surface and nature of the glassy carbon electrode. The DNA layer immobilized at a freshly polished glassy carbon electrode was very stable even after applying highly negative potentials. The electron transfer of potassium ferricyanide, catechol and dopamine at glassy carbon surfaces modified with thin (obtained by adsorption under controlled potential conditions) and thick (obtained by casting the glassy carbon surface with highly concentrated DNA solutions) DNA layers was slower than that at the bare glassy carbon electrode, although this effect was dependent on the thickness of the layer and was not charge selective. Raman experiments showed an important decrease of the vibrational modes assigned to the nucleobases residues, suggesting a strong interaction of these residues with the electrode surface. The hybridization of oligo(dG)21 and oligo(dC)21 was evaluated from the guanine oxidation signal and the reduction of the redox indicator Co(phen)33+. In both cases the chronopotentiometric response indicated that the compromise of the bases in the interaction of DNA with the electrode surface is too strong, preventing further hybridization. In summary, glassy carbon is a useful electrode material to detect DNA in a direct and very sensitive way, but not to be used for the preparation of biorecognition layers by direct adsorption of the probe sequence on the electrode surface for detecting the hybridization event.

  13. Apoferritin-templated biosynthesis of manganese nanoparticles and investigation of direct electron transfer of MnNPs-HsAFr at modified glassy carbon electrode.

    PubMed

    Rafipour, Ronak; Kashanian, Soheila; Hashemi, Sadegh; Omidfar, Kobra; Ezzati Nazhad Dolatabadi, Jafar

    2017-01-01

    Manganese nanoparticles (MnNPs) were created within horse spleen apoferritin (HsAFr) cavity nanotemplates. Transmission electron microscopy revealed the particle size to be 6 nm. Intrinsic fluorescence data showed that the mineralization acted as a quencher of the HsAFr fluorescence, and extrinsic fluorescence data revealed that the hydrophobic binding site at the surface of HsAFr was not changed. Finally, the MnNP-HsAFr was immobilized onto multiwalled carbon nanotubes entrapped into chitosan (CS) matrices by through sequential 1-ethyl-3-(3-dimethylaminopropyl) carbodiimide-N-hydroxysuccinimide and glutaraldehyde coupling. The MnNPs-HsAFr immobilized on CNT-CS/GC electrode was characterized by cyclic voltammetry. This charge transfer coefficient (α) and the exchange current (i0 ) of MnNPs-HsAFr immobilized on modified electrode in 0.1 M phosphate solution (pH 7.5) were found to be 0.57 and 0.48 μA, respectively. © 2015 International Union of Biochemistry and Molecular Biology, Inc.

  14. Thermal expansion of glassy polymers.

    PubMed

    Davy, K W; Braden, M

    1992-01-01

    The thermal expansion of a number of glassy polymers of interest in dentistry has been studied using a quartz dilatometer. In some cases, the expansion was linear and therefore the coefficient of thermal expansion readily determined. Other polymers exhibited non-linear behaviour and values appropriate to different temperature ranges are quoted. The linear coefficient of thermal expansion was, to a first approximation, a function of both the molar volume and van der Waal's volume of the repeating unit.

  15. Failure of a carbon fiber-reinforced polymer implant used for transforaminal lumbar interbody fusion.

    PubMed

    Sardar, Zeeshan; Jarzem, Peter

    2013-12-01

    Lumbar interbody fusion is a common procedure owing to the high prevalence of degenerative spinal disorders. During such procedures, carbon fiber-reinforced polymer (CFRP) cages are frequently utilized to fill the void created between adjacent vertebral bodies, to provide mechanical stability, and to carry graft material. Failure of such implants can lead to significant morbidity. We discuss the possible causes leading to the failure of a CFRP cage in a patient with rheumatoid arthritis. Review of a 49-year-old woman who underwent revision anterior lumbar interbody fusion 2 years after posterior instrumentation and transforaminal lumbar interbody fusion at L4-L5 and L5-S1. The patient developed pseudarthrosis at the two previously fused levels with failure of the posterior instrumentation. Revision surgery reveled failure with fragmentation of the CFRP cage at the L5-S1 level. CFRP implants can break if mechanical instability or nonunion occurs in the spinal segments, thus emphasizing the need for optimizing medical management and meticulous surgical technique in achieving stability.

  16. Failure of a Carbon Fiber–Reinforced Polymer Implant Used for Transforaminal Lumbar Interbody Fusion

    PubMed Central

    Sardar, Zeeshan; Jarzem, Peter

    2013-01-01

    Lumbar interbody fusion is a common procedure owing to the high prevalence of degenerative spinal disorders. During such procedures, carbon fiber–reinforced polymer (CFRP) cages are frequently utilized to fill the void created between adjacent vertebral bodies, to provide mechanical stability, and to carry graft material. Failure of such implants can lead to significant morbidity. We discuss the possible causes leading to the failure of a CFRP cage in a patient with rheumatoid arthritis. Review of a 49-year-old woman who underwent revision anterior lumbar interbody fusion 2 years after posterior instrumentation and transforaminal lumbar interbody fusion at L4–L5 and L5–S1. The patient developed pseudarthrosis at the two previously fused levels with failure of the posterior instrumentation. Revision surgery reveled failure with fragmentation of the CFRP cage at the L5–S1 level. CFRP implants can break if mechanical instability or nonunion occurs in the spinal segments, thus emphasizing the need for optimizing medical management and meticulous surgical technique in achieving stability. PMID:24436878

  17. In-vivo degradation of poly(carbonate-urethane) based spine implants

    PubMed Central

    Cipriani, E.; Bracco, P.; Kurtz, S.M.; Costa, L.; Zanetti, M.

    2013-01-01

    Fourteen explanted Dynesys® spinal devices were analyzed for biostability and compared with a reference, never implanted, control. Both poly(carbonate-urethane) (PCU) spacers and polyethylene-terephthalate (PET) cords were analyzed. The effect of implantation was evaluated through the observation of physical alterations of the device surfaces, evaluation of the chemical degradation and fluids absorption on the devices and examination of the morphological and mechanical features. PCU spacers exhibited a variety of surface damage mechanisms, the most significant being abrasion and localized, microscopic surface cracks. Evidence of oxidation and chain scission were detected on PCU spacers ATR–FTIR. ATR–FTIR, DSC and hardness measurements also showed a slight heterogeneity in the composition of PCU. The extraction carried out on the PCU spacers revealed the presence of extractable polycarbonate segments. One spacer and all PET cords visually exhibited the presence of adherent biological material (proteins), confirmed by the ATR–FTIR results. GC/MS analyses of the extracts from PET cords revealed the presence of biological fluids residues, mainly cholesterol derivatives and fatty acids, probably trapped into the fiber network. No further chemical alterations were observed on the PET cords. Although the observed physical and chemical damage can be considered superficial, greater attention must be paid to the chemical degradation mechanisms of PCU and to the effect of byproducts on the body. PMID:24043907

  18. In-vivo degradation of poly(carbonate-urethane) based spine implants.

    PubMed

    Cipriani, E; Bracco, P; Kurtz, S M; Costa, L; Zanetti, M

    2013-06-01

    Fourteen explanted Dynesys® spinal devices were analyzed for biostability and compared with a reference, never implanted, control. Both poly(carbonate-urethane) (PCU) spacers and polyethylene-terephthalate (PET) cords were analyzed. The effect of implantation was evaluated through the observation of physical alterations of the device surfaces, evaluation of the chemical degradation and fluids absorption on the devices and examination of the morphological and mechanical features. PCU spacers exhibited a variety of surface damage mechanisms, the most significant being abrasion and localized, microscopic surface cracks. Evidence of oxidation and chain scission were detected on PCU spacers ATR-FTIR. ATR-FTIR, DSC and hardness measurements also showed a slight heterogeneity in the composition of PCU. The extraction carried out on the PCU spacers revealed the presence of extractable polycarbonate segments. One spacer and all PET cords visually exhibited the presence of adherent biological material (proteins), confirmed by the ATR-FTIR results. GC/MS analyses of the extracts from PET cords revealed the presence of biological fluids residues, mainly cholesterol derivatives and fatty acids, probably trapped into the fiber network. No further chemical alterations were observed on the PET cords. Although the observed physical and chemical damage can be considered superficial, greater attention must be paid to the chemical degradation mechanisms of PCU and to the effect of byproducts on the body.

  19. Understanding heterogeneity in Genesis diamond-like carbon film using SIMS analysis of implants

    DOE PAGES

    Jurewicz, Amy J. G.; Burnett, Don S.; Rieck, Karen D.; ...

    2017-07-05

    An amorphous diamond-like carbon film deposited on silicon made at Sandia National Laboratory by pulsed laser deposition was one of several solar wind (SW) collectors used by the Genesis Mission (NASA Discovery Class Mission #5). The film was ~1 μm thick, amorphous, anhydrous, and had a high ratio of sp3–sp2 bonds (>50%). For 27 months of exposure to space at the first We passively irradiated lagrange point, the collectors, with SW (H fluence ~2 × 1016 ions cm-2; He fluence ~8 × 1014 ions cm-2). The radiation damage caused by the implanted H ions peaked at 12–14 nm below themore » surface of the film and that of He about 20–23 nm. To enable quantitative measurement of the SW fluences by secondary ion mass spectroscopy, minor isotopes of Mg (25Mg and 26Mg) were commercially implanted into flight-spare collectors at 75 keV and a fluence of 1 × 1014 ions cm-2. Furthermore, the shapes of analytical depth profiles, the rate at which the profiles were sputtered by a given beam current, and the intensity of ion yields are used to characterize the structure of the material in small areas (~200 × 200 ± 50 μm). Data were consistent with the hypothesis that minor structural changes in the film were induced by SW exposure.« less

  20. Novel bulk carbon nanotube materials for implant by spark plasma sintering.

    PubMed

    Wang, Wei; Omori, Mamoru; Watari, Fumio; Yokoyama, Atsuro

    2005-12-01

    Novel, bulk multiwall carbon nanotubes (MWCNTs) sintered with polycarbosilane (PCS) as a binder agent were fabricated by spark plasma sintering (SPS), and their microstructure and properties were investigated. Sintering was done with 20-60 MPa pressure at 1200 degrees C. SEM and TEM observations showed that the nanosized tube microstructure was preserved even after sintering, and tubes adhered to each other with the nanosized nodules of SiC pyrolyzed form PCS as revealed by X-ray diffraction. Bulk density and Vickers hardness were found to increase, whereas the specific surface area decreased, as PCS content and sintering pressure increased. Through animal experiments, the inflammatory reaction of CNTs/PCS material was found to be slightly increased with increasing PCS content. In conclusion, sintered CNTs had physical and mechanical properties close to bone, and their good biocompatibility based on tissue response served to pave their way as a suitable implant material in the future.

  1. Osseointegration is improved by coating titanium implants with a nanostructured thin film with titanium carbide and titanium oxides clustered around graphitic carbon.

    PubMed

    Veronesi, Francesca; Giavaresi, Gianluca; Fini, Milena; Longo, Giovanni; Ioannidu, Caterina Alexandra; Scotto d'Abusco, Anna; Superti, Fabiana; Panzini, Gianluca; Misiano, Carlo; Palattella, Alberto; Selleri, Paolo; Di Girolamo, Nicola; Garbarino, Viola; Politi, Laura; Scandurra, Roberto

    2017-01-01

    Titanium implants coated with a 500nm nanostructured layer, deposited by the Ion Plating Plasma Assisted (IPPA) technology, composed of 60% graphitic carbon, 25% titanium oxides and 15% titanium carbide were implanted into rabbit femurs whilst into the controlateral femurs uncoated titanium implants were inserted as control. At four time points the animals were injected with calcein green, xylenol orange, oxytetracycline and alizarin. After 2, 4 and 8weeks femurs were removed and processed for histology and static and dynamic histomorphometry for undecalcified bone processing into methylmethacrylate, sectioned, thinned, polished and stained with Toluidine blue and Fast green. The overall bone-implant contacts rate (percentage of bone-implant contacts/weeks) of the TiC coated implant was 1.6 fold than that of the uncoated titanium implant. The histomorphometric analyses confirmed the histological evaluations. More precisely, higher Mineral Apposition Rate (MAR, μm/day) (p<0.005) and Bone Formation Rate (BFR, μm(2)/μm/day) (p<0.0005) as well as Bone Implant Contact (Bic) and Bone Ingrowth values (p<0.0005) were observed for the TiC coated implants compared to uncoated implants. In conclusion the hard nanostructured TiC layer protects the bulk titanium implant against the harsh conditions of biological tissues and in the same time, stimulating adhesion, proliferation and activity of osteoblasts, induces a better bone-implant contacts of the implant compared to the uncoated titanium implant.

  2. Effects of thermal annealing on the structural and optical properties of carbon-implanted SiO2.

    PubMed

    Poudel, P R; Paramo, J A; Poudel, P P; Diercks, D R; Strzhemechny, Y M; Rout, B; McDaniel, F D

    2012-03-01

    Amorphous carbon (a-C) nanoclusters were synthesized by the implantation of carbon ions (C-) into thermally grown silicon dioxide film (-500 nm thick) on a Si (100) wafer and processed by high temperature thermal annealing. The carbon ions were implanted with an energy of 70 keV at a fluence of 5 x 10(17) atoms/cm2. The implanted samples were annealed at 1100 degrees C for different time periods in a gas mixture of 96% Ar+4% H2. Raman spectroscopy, X-ray photoelectron spectroscopy (XPS) and High Resolution Transmission Electron Microscopy (HRTEM) were used to study the structural properties of both the as-implanted and annealed samples. HRTEM reveals the formation of nanostructures in the annealed samples. The Raman spectroscopy also confirms the formation of carbon nano-clusters in the samples annealed for 10 min, 30 min, 60 min and 90 min. No Raman features originating from the carbon-clusters are observed for the sample annealed further to 120 min, indicating a complete loss of implanted carbon from the SiO2 layer. The loss of the implanted carbon in the 120 min annealed sample from the SiO2 layer was also observed in the XPS depth profile measurements. Room temperature photoluminescence (PL) spectroscopy revealed visible emissions from the samples pointing to carbon ion induced defects as the origin of a broad 2.0-2.4 eV band, and the intrinsic defects in SiO2 as the possible origin of the -2.9 eV bands. In low temperature photoluminescence spectra, two sharp and intense photoluminescence lines at -3.31 eV and -3.34 eV appear for the samples annealed for 90 min and 120 min, whereas no such bands are observed in the samples annealed for 10 min, 30 min, and 60 min. The Si nano-clusters forming at the Si-SiO2 interface could be the origin of these intense peaks.

  3. Coating dental implant abutment screws with diamondlike carbon doped with diamond nanoparticles: the effect on maintaining torque after mechanical cycling.

    PubMed

    Lepesqueur, Laura Soares; de Figueiredo, Viviane Maria Gonçalves; Ferreira, Leandro Lameirão; Sobrinho, Argemiro Soares da Silva; Massi, Marcos; Bottino, Marco Antônio; Nogueira Junior, Lafayette

    2015-01-01

    To determine the effect of maintaining torque after mechanical cycling of abutment screws that are coated with diamondlike carbon and coated with diamondlike carbon doped with diamond nanoparticles, with external and internal hex connections. Sixty implants were divided into six groups according to the type of connection (external or internal hex) and the type of abutment screw (uncoated, coated with diamondlike carbon, and coated with diamondlike carbon doped with diamond nanoparticles). The implants were inserted into polyurethane resin and crowns of nickel chrome were cemented on the implants. The crowns had a hole for access to the screw. The initial torque and the torque after mechanical cycling were measured. The torque values maintained (in percentages) were evaluated. Statistical analysis was performed using one-way analysis of variance and the Tukey test, with a significance level of 5%. The largest torque value was maintained in uncoated screws with external hex connections, a finding that was statistically significant (P = .0001). No statistically significant differences were seen between the groups with and without coating in maintaining torque for screws with internal hex connections (P = .5476). After mechanical cycling, the diamondlike carbon with and without diamond doping on the abutment screws showed no improvement in maintaining torque in external and internal hex connections.

  4. Silver nanoparticle-enriched diamond-like carbon implant modification as a mammalian cell compatible surface with antimicrobial properties.

    PubMed

    Gorzelanny, Christian; Kmeth, Ralf; Obermeier, Andreas; Bauer, Alexander T; Halter, Natalia; Kümpel, Katharina; Schneider, Matthias F; Wixforth, Achim; Gollwitzer, Hans; Burgkart, Rainer; Stritzker, Bernd; Schneider, Stefan W

    2016-03-09

    The implant-bone interface is the scene of competition between microorganisms and distinct types of tissue cells. In the past, various strategies have been followed to support bony integration and to prevent bacterial implant-associated infections. In the present study we investigated the biological properties of diamond-like carbon (DLC) surfaces containing silver nanoparticles. DLC is a promising material for the modification of medical implants providing high mechanical and chemical stability and a high degree of biocompatibility. DLC surface modifications with varying silver concentrations were generated on medical-grade titanium discs, using plasma immersion ion implantation-induced densification of silver nanoparticle-containing polyvinylpyrrolidone polymer solutions. Immersion of implants in aqueous liquids resulted in a rapid silver release reducing the growth of surface-bound and planktonic Staphylococcus aureus and Staphylococcus epidermidis. Due to the fast and transient release of silver ions from the modified implants, the surfaces became biocompatible, ensuring growth of mammalian cells. Human endothelial cells retained their cellular differentiation as indicated by the intracellular formation of Weibel-Palade bodies and a high responsiveness towards histamine. Our findings indicate that the integration of silver nanoparticles into DLC prevents bacterial colonization due to a fast initial release of silver ions, facilitating the growth of silver susceptible mammalian cells subsequently.

  5. Silver nanoparticle-enriched diamond-like carbon implant modification as a mammalian cell compatible surface with antimicrobial properties

    PubMed Central

    Gorzelanny, Christian; Kmeth, Ralf; Obermeier, Andreas; Bauer, Alexander T.; Halter, Natalia; Kümpel, Katharina; Schneider, Matthias F.; Wixforth, Achim; Gollwitzer, Hans; Burgkart, Rainer; Stritzker, Bernd; Schneider, Stefan W.

    2016-01-01

    The implant-bone interface is the scene of competition between microorganisms and distinct types of tissue cells. In the past, various strategies have been followed to support bony integration and to prevent bacterial implant-associated infections. In the present study we investigated the biological properties of diamond-like carbon (DLC) surfaces containing silver nanoparticles. DLC is a promising material for the modification of medical implants providing high mechanical and chemical stability and a high degree of biocompatibility. DLC surface modifications with varying silver concentrations were generated on medical-grade titanium discs, using plasma immersion ion implantation-induced densification of silver nanoparticle-containing polyvinylpyrrolidone polymer solutions. Immersion of implants in aqueous liquids resulted in a rapid silver release reducing the growth of surface-bound and planktonic Staphylococcus aureus and Staphylococcus epidermidis. Due to the fast and transient release of silver ions from the modified implants, the surfaces became biocompatible, ensuring growth of mammalian cells. Human endothelial cells retained their cellular differentiation as indicated by the intracellular formation of Weibel-Palade bodies and a high responsiveness towards histamine. Our findings indicate that the integration of silver nanoparticles into DLC prevents bacterial colonization due to a fast initial release of silver ions, facilitating the growth of silver susceptible mammalian cells subsequently. PMID:26955791

  6. Silver nanoparticle-enriched diamond-like carbon implant modification as a mammalian cell compatible surface with antimicrobial properties

    NASA Astrophysics Data System (ADS)

    Gorzelanny, Christian; Kmeth, Ralf; Obermeier, Andreas; Bauer, Alexander T.; Halter, Natalia; Kümpel, Katharina; Schneider, Matthias F.; Wixforth, Achim; Gollwitzer, Hans; Burgkart, Rainer; Stritzker, Bernd; Schneider, Stefan W.

    2016-03-01

    The implant-bone interface is the scene of competition between microorganisms and distinct types of tissue cells. In the past, various strategies have been followed to support bony integration and to prevent bacterial implant-associated infections. In the present study we investigated the biological properties of diamond-like carbon (DLC) surfaces containing silver nanoparticles. DLC is a promising material for the modification of medical implants providing high mechanical and chemical stability and a high degree of biocompatibility. DLC surface modifications with varying silver concentrations were generated on medical-grade titanium discs, using plasma immersion ion implantation-induced densification of silver nanoparticle-containing polyvinylpyrrolidone polymer solutions. Immersion of implants in aqueous liquids resulted in a rapid silver release reducing the growth of surface-bound and planktonic Staphylococcus aureus and Staphylococcus epidermidis. Due to the fast and transient release of silver ions from the modified implants, the surfaces became biocompatible, ensuring growth of mammalian cells. Human endothelial cells retained their cellular differentiation as indicated by the intracellular formation of Weibel-Palade bodies and a high responsiveness towards histamine. Our findings indicate that the integration of silver nanoparticles into DLC prevents bacterial colonization due to a fast initial release of silver ions, facilitating the growth of silver susceptible mammalian cells subsequently.

  7. Improvement in wear performance of surgical Ti-6Al-4V alloy by ion implantation of nitrogen or carbon

    SciTech Connect

    Williams, J.M.; Buchanan, R.A.; Rigney, E.D. Jr.

    1985-06-01

    The effects of ion implantations of either nitrogen or carbon on the corrosive-wear performance of surgical Ti-6A1-4V alloy were investigated. In vitro tests made use of an apparatus which could produce certain chemical and mechanical aspects of a sliding interface such as that which occurs between alloy and polyethylene components of an artificial hip (or knee) joint. Cylindrical samples of the Ti alloy were rotated between loaded, conforming pads made of ultrahigh molecular weight polyethylene (UHMWPE) while these test components were immersed either in a saline solution or a saline solution with bovine serum added. During the tests open-circuit corrosion currents for the alloy were measured by the Tafel extrapolation technique. Profilometry studies were done before and after the tests. Alloy samples implanted with either nitrogen or carbon remained as-new for all test conditions. Unimplanted control samples were severely scored. Corrosion currents as measured under the mechanical action were reduced by a factor of approximately one hundred by the ion implantation treatments. It is concluded that nitrogen or carbon ion implantation produces a marked improvement in the corrosive wear performance of the alloy in these tests. It is inferred that abrasive wear is the dominant mechanism of material removal. In addition, apparently owing to reduction of wear debris in the sliding interface, ion treatment of the alloy greatly improves wear performance of the mating UHMWPE component. 11 refs., 11 figs., 2 tabs.

  8. In situ high-temperature X-ray diffraction characterization of yttrium-implanted extra low-carbon steel

    SciTech Connect

    Caudron, E.; Buscail, H.; Perrier, S.

    1999-11-01

    Yttrium-implanted and unimplanted extra low-carbon steel samples were analyzed at T = 700 C and under an oxygen partial pressure P{sub O2} = 0.041Pa for 24 h to show the yttrium implantation effect on extra low-carbon steel high-temperature corrosion resistance. Sample oxidation weight gains were studied by thermogravimetry, and structural analyses were performed using in situ high-temperature X-ray diffraction with the same experimental conditions. The aim of this paper is to show the initial nucleation stage of the main compounds induced by oxidation at high temperatures according to the initial sample treatment (yttrium-implanted or unimplanted). The results obtained by in situ high-temperature X-ray diffraction will be compared to those by thermogravimetry to show the existing correlation between weight gain curves and structural studies. Results allow one to understand the improved corrosion resistance of yttrium-implanted extra low-carbon steel at high temperatures.

  9. Biological and functional evaluation of a novel pyrolytic carbon implant for the treatment of focal osteochondral defects in the medial femoral condyle: assessment in a canine model.

    PubMed

    Salkeld, Samantha L; Patron, Laura P; Lien, Joan C; Cook, Stephen D; Jones, Deryk G

    2016-12-01

    Osteochondral defects continue to be a clinical treatment challenge, and when left untreated, may cause pain and functional impairment. Pyrolytic carbon is a unique isotropic biomaterial used in heart valve and small joint replacements due to its excellent wear properties and biocompatibility with bone and articular cartilage. Therefore, a proposed solution is to utilize a focal pyrolytic carbon hemiarthroplasty implant as an alternative resurfacing treatment strategy for isolated cartilage lesions. A canine model (n = 9) was used to evaluate the in vivo histologic response and function of a pyrolytic carbon implant replacing a full-thickness osteochondral defect in the medial femoral condyle (MFC) of the knee. The gross appearance and histologic results were compared to an identical cobalt-chromium (Co-Cr) alloy implant placed in a defect in the contralateral MFC and evaluated up to 52 weeks. Extensive bone incorporation to the stem portion was observed for both implant types. The total mean histologic score for the cartilage of the MFC surrounding the pyrolytic carbon implants was significantly improved compared to that of the Co-Cr alloy implants at all evaluation periods (p < 0.05). Histologic grading and gross observations at 52 weeks for pyrolytic carbon implants were similar to those of Co-Cr alloy implants at 24 weeks. At 24 weeks, the mean total histologic score for Co-Cr alloy implants was 11.6 ± 0.7 (0-16 range point; 16 = normal appearance), while at 52 weeks, the mean total score for the pyrolytic carbon implants was 11.7 ± 1.3. Mean total histologic score of opposing medial tibia cartilage for the pyrolytic carbon implants was superior to that of the Co-Cr alloy group at all evaluation periods and significantly improved over the Co-Cr alloy implant group at 24 weeks (p = 0.001) and 52 weeks (p < 0.001). Use of a pyrolytic carbon implant for reconstruction of a focal cartilage defect demonstrated effective implant

  10. Glassy features of crystal plasticity

    NASA Astrophysics Data System (ADS)

    Lehtinen, Arttu; Costantini, Giulio; Alava, Mikko J.; Zapperi, Stefano; Laurson, Lasse

    2016-08-01

    Crystal plasticity occurs by deformation bursts due to the avalanchelike motion of dislocations. Here we perform extensive numerical simulations of a three-dimensional dislocation dynamics model under quasistatic stress-controlled loading. Our results show that avalanches are power-law distributed and display peculiar stress and sample size dependence: The average avalanche size grows exponentially with the applied stress, and the amount of slip increases with the system size. These results suggest that intermittent deformation processes in crystalline materials exhibit an extended critical-like phase in analogy to glassy systems instead of originating from a nonequilibrium phase transition critical point.

  11. In vivo implant fixation of carbon fiber-reinforced PEEK hip prostheses in an ovine model.

    PubMed

    Nakahara, Ichiro; Takao, Masaki; Bandoh, Shunichi; Bertollo, Nicky; Walsh, William R; Sugano, Nobuhiko

    2013-03-01

    Carbon fiber-reinforced polyetheretherketone (CFR/PEEK) is theoretically suitable as a material for use in hip prostheses, offering excellent biocompatibility, mechanical properties, and the absence of metal ions. To evaluate in vivo fixation methods of CFR/PEEK hip prostheses in bone, we examined radiographic and histological results for cementless or cemented CFR/PEEK hip prostheses in an ovine model with implantation up to 52 weeks. CFR/PEEK cups and stems with rough-textured surfaces plus hydroxyapatite (HA) coatings for cementless fixation and CFR/PEEK cups and stems without HA coating for cement fixation were manufactured based on ovine computed tomography (CT) data. Unilateral total hip arthroplasty was performed using cementless or cemented CFR/PEEK hip prostheses. Five cementless cups and stems and six cemented cups and stems were evaluated. On the femoral side, all cementless stems demonstrated bony ongrowth fixation and all cemented stems demonstrated stable fixation without any gaps at both the bone-cement and cement-stem interfaces. All cementless cases and four of the six cemented cases showed minimal stress shielding. On the acetabular side, two of the five cementless cups demonstrated bony ongrowth fixation. Our results suggest that both cementless and cemented CFR/PEEK stems work well for fixation. Cup fixation may be difficult for both cementless and cemented types in this ovine model, but bone ongrowth fixation on the cup was first seen in two cementless cases. Cementless fixation can be achieved using HA-coated CFR/PEEK implants, even under load-bearing conditions.

  12. Characteristics and analysis of 4H-SiC PiN diodes with a carbon-implanted drift layer

    NASA Astrophysics Data System (ADS)

    Jiangmei, Feng; Huajun, Shen; Xiaohua, Ma; Yun, Bai; Jia, Wu; Chengzhan, Li; Kean, Liu; Xinyu, Liu

    2016-04-01

    The characteristics of 4H-SiC PiN diodes with a carbon-implanted drift layer was investigated and the reason of characteristics improvement was analyzed. The forward voltage drops of the diodes with carbon-implanted drift layer were around 3.3 V, which is lower than that of devices without carbon implantation, the specific-on resistance was decreased from 9.35 to 4.38 mΩ·cm2 at 100 A/cm2, and the reverse leakage current was also decreased. The influence of carbon incorporation in the SiC crystalline grids was studied by using deep-level transient spectroscopy (DLTS). The DLTS spectra revealed that the Z 1/2 traps, which were regarded as the main lifetime limiting defects, were dramatically reduced. It is proposed that the reduction of Z 1/2 traps can achieve longer carrier lifetime in the drift layer, which is beneficial to the performance of bipolar devices. Project supported by the Opening Project of Key Laboratory of Microelectronics Devices & Integrated Technology, Institute of Microelectronics, Chinese Academy of Sciences.

  13. Structural and electrical properties of oxygen complexes in Cz and FZ silicon crystals implanted with carbon ions

    NASA Astrophysics Data System (ADS)

    Romanyuk, Boris; Melnik, Victor; Popov, Valentin; Babich, Vilik; Kladko, Vasyl; Gudymenko, Olexandr; Ilchenko, Volodimir; Vasyliev, Iegor; Goriachko, Andrii

    2014-12-01

    We present a comparative study of thermal donor (TD) center formation mechanisms as a result of carbon ion implantation into float zone (FZ-Si) and Czochralski (Cz-Si) silicon crystals. The kinetics of the TD center formation and transformation of their structure during annealing have been investigated. Also, the TD center formation takes place after additional oxygen implantation into FZ/Cz-Si, and an important role of recoil oxygen atoms (from the screen oxide) has been demonstrated for the FZ-Si case. Their concentration in the Si surface layer depends on the implantation dose and the screen oxide thickness, reaching up to values 1018 to 1019 cm-3, which is comparable with the oxygen concentration in Cz-Si. These oxygen atoms can lead to additional thermal donor centers generation, especially in the FZ-Si.

  14. Ending Aging in Super Glassy Polymer Membranes

    SciTech Connect

    Lau, CH; Nguyen, PT; Hill, MR; Thornton, AW; Konstas, K; Doherty, CM; Mulder, RJ; Bourgeois, L; Liu, ACY; Sprouster, DJ; Sullivan, JP; Bastow, TJ; Hill, AJ; Gin, DL; Noble, RD

    2014-04-16

    Aging in super glassy polymers such as poly(trimethylsilylpropyne) (PTMSP), poly(4-methyl-2-pentyne) (PMP), and polymers with intrinsic microporosity (PIM-1) reduces gas permeabilities and limits their application as gas-separation membranes. While super glassy polymers are initially very porous, and ultra-permeable, they quickly pack into a denser phase becoming less porous and permeable. This age-old problem has been solved by adding an ultraporous additive that maintains the low density, porous, initial stage of super glassy polymers through absorbing a portion of the polymer chains within its pores thereby holding the chains in their open position. This result is the first time that aging in super glassy polymers is inhibited whilst maintaining enhanced CO2 permeability for one year and improving CO2/N-2 selectivity. This approach could allow super glassy polymers to be revisited for commercial application in gas separations.

  15. Study of the effects of E × B fields as mechanism to carbon-nitrogen plasma immersion ion implantation on stainless steel samples

    NASA Astrophysics Data System (ADS)

    Pillaca, E. J. D. M.; Ueda, M.; Oliveira, R. M.; Pichon, L.

    2014-08-01

    Effects of E × B fields as mechanism to carbon-nitrogen plasma immersion ion implantation (PIII) have been investigated. This magnetic configuration when used in PIII allows obtaining high nitrogen plasma density close to the ion implantation region. Consequently, high ions dose on the target is possible to be achieved compared with standard PIII. In this scenario, nitrogen and carbon ions were implanted simultaneously on stainless steel, as measured by GDOES and detected by X-ray diffraction. Carbon-tape disposed on the sample-holder was sputtered by intense bombardment of nitrogen ions, being the source of carbon atoms in this experiment. The implantation of both N and C caused changes on sample morphology and improvement of the tribological properties of the stainless steel.

  16. The generation, detection and measurement of laser-induced carbon plasma ions and their implantation effects on brass substrate

    NASA Astrophysics Data System (ADS)

    Ahmad, Shahbaz; Bashir, Shazia; Shahid Rafique, M.; Yousaf, Daniel; Ahmad, Riaz

    2016-05-01

    The generation, detection and measurement of laser-induced carbon plasma ions and their implantation effects on brass substrate have been investigated. Thomson parabola technique was employed to measure the energy and flux of carbon ions. The magnetic field of strength 80 mT was applied on the graphite plasma plume to provide an appropriate trajectory to the generated ions. The energy of carbon ions is 678 KeV for laser fluence of 5.1 J/cm2 which was kept constant for all exposures. The flux of ions varies from 32 × 1011 to 72 × 1014 ions/cm2 for varying numbers of laser pulses from 3000 to 12,000. In order to explore the ion irradiation effects on brass, four brass substrates were irradiated by carbon ions of different flux. Scanning electron microscope (SEM) and X-ray diffractometer (XRD) are used to analyze the surface morphology and crystallographic structure of ion-implanted brass, respectively. SEM analysis reveals the formation and growth of nano-/micro-sized cavities, pores and pits for the various ion flux for varying numbers of laser pulses from 3000 to 12,000. By increasing ion flux by increasing the number of pulses up to 9000 shots, the dendritic structures initiate to grow along with cavities and pores. At the maximum ion flux for 12,000 shots, the unequiaxed dendritic structures become distinct and the distance between the dendrites is decreased, whereas cavities, pores and pits are completely finished. The XRD analysis reveals that a new phase of ZnC (0012) is formed in the brass substrate after ion implantation. Universal tensile testing machine and Vickers microhardness tester are used to explore the yield stress, ultimate tensile strength and microhardness of ion-implanted brass substrate. The mechanical properties monotonically increase by increasing the ion flux. Variations in mechanical properties are correlated with surface and structural modifications of brass.

  17. Influence of 400 keV carbon ion implantation on structural, optical and electrical properties of PMMA

    NASA Astrophysics Data System (ADS)

    Arif, Shafaq; Rafique, M. Shahid; Saleemi, Farhat; Sagheer, Riffat; Naab, Fabian; Toader, Ovidiu; Mahmood, Arshad; Rashid, Rashad; Mahmood, Mazhar

    2015-09-01

    Ion implantation is a useful technique to modify surface properties of polymers without altering their bulk properties. The objective of this work is to explore the 400 keV C+ ion implantation effects on PMMA at different fluences ranging from 5 × 1013 to 5 × 1015 ions/cm2. The surface topographical examination of irradiated samples has been performed using Atomic Force Microscope (AFM). The structural and chemical modifications in implanted PMMA are examined by Raman and Fourier Infrared Spectroscopy (FTIR) respectively. The effects of carbon ion implantation on optical properties of PMMA are investigated by UV-Visible spectroscopy. The modifications in electrical conductivity have been measured using a four point probe technique. AFM images reveal a decrease in surface roughness of PMMA with an increase in ion fluence from 5 × 1014 to 5 × 1015 ions/cm2. The existence of amorphization and sp2-carbon clusterization has been confirmed by Raman and FTIR spectroscopic analysis. The UV-Visible data shows a prominent red shift in absorption edge as a function of ion fluence. This shift displays a continuous reduction in optical band gap (from 3.13 to 0.66 eV) due to formation of carbon clusters. Moreover, size of carbon clusters and photoconductivity are found to increase with increasing ion fluence. The ion-induced carbonaceous clusters are believed to be responsible for an increase in electrical conductivity of PMMA from (2.14 ± 0.06) × 10-10 (Ω-cm)-1 (pristine) to (0.32 ± 0.01) × 10-5 (Ω-cm)-1 (irradiated sample).

  18. Collision cascades enhanced hydrogen redistribution in cobalt implanted hydrogenated diamond-like carbon films

    NASA Astrophysics Data System (ADS)

    Gupta, P.; Becker, H.-W.; Williams, G. V. M.; Hübner, R.; Heinig, K.-H.; Markwitz, A.

    2017-03-01

    Hydrogenated diamond-like carbon films produced by C3H6 deposition at 5 kV and implanted at room temperature with 30 keV Co atoms to 12 at.% show not only a bimodal distribution of Co atoms but also a massive redistribution of hydrogen in the films. Resonant nuclear reaction analysis was used to measure the hydrogen depth profiles (15N-method). Depletion of hydrogen near the surface was measured to be as low as 7 at.% followed by hydrogen accumulation from 27 to 35 at.%. A model is proposed considering the thermal energy deposited by collision cascade for thermal insulators. In this model, sufficient energy is provided for dissociated hydrogen to diffuse out of the sample from the surface and diffuse into the sample towards the interface which is however limited by the range of the incoming Co ions. At a hydrogen concentration of ∼35 at.%, the concentration gradient of the mobile unbounded hydrogen atoms is neutralised effectively stopping diffusion towards the interface. The results point towards new routes of controlling the composition and distribution of elements at the nanoscale within a base matrix without using any heat treatment methods. Exploring these opportunities can lead to a new horizon of materials and device engineering needed for enabling advanced technologies and applications.

  19. Diamond-like carbon coatings with zirconium-containing interlayers for orthopedic implants.

    PubMed

    Choudhury, Dipankar; Lackner, Juergen; Fleming, Robert A; Goss, Josh; Chen, Jingyi; Zou, Min

    2017-04-01

    Six types of diamond-like carbon (DLC) coatings with zirconium (Zr)-containing interlayers on titanium alloy (Ti-6Al-4V) were investigated for improving the biotribological performance of orthopedic implants. The coatings consist of three layers: above the substrate a layer stack of 32 alternating Zr and ZrN sublayers (Zr:ZrN), followed by a layer comprised of Zr and DLC (Zr:DLC), and finally a N-doped DLC layer. The Zr:ZrN layer is designed for increasing load carrying capacity and corrosion resistance; the Zr:DLC layer is for gradual transition of stress, thus enhancing layer adhesion; and the N-doped DLC layer is for decreasing friction, squeaking noises and wear. Biotribological experiments were performed in simulated body fluid employing a ball-on-disc contact with a Si3N4 ball and a rotational oscillating motion to mimic hip motion in terms of gait angle, dynamic contact pressures, speed and body temperature. The results showed that the Zr:DLC layer has a substantial influence on eliminating delamination of the DLC from the substrates. The DLC/Si3N4 pairs significantly reduced friction coefficient, squeaking noise and wear of both the Si3N4 balls and the discs compared to those of the Ti-6Al-4V/Si3N4 pair after testing for a duration that is equivalent to one year of hip motion in vivo. Copyright © 2017 Elsevier Ltd. All rights reserved.

  20. Search for Superconductivity in Carbon Nanotubes Doped by Boron Ion Implantation

    NASA Astrophysics Data System (ADS)

    Cornell, Nicholas; Kutsenov, Alex; Howard, Austin; Mayo, Nathaniel; Galstayan, Eduard; Chu, Wei Kan; Freyhardt, Herbert; Zakhidov, Anvar; Wang, Xuemei; University of Texas at Dallas Team; University of Houston Team

    2011-03-01

    The boron doping of single wall carbon nanotubes(CNT) by laser ablation synthesis has been reported to create superconducting B-CNTs with Tc's ranging from 12-19 Kelvin, depending on CNT inter-tube connection strength. We attempt to create boron doped multiwall CNT by ion implantation doping. Ion doping of boron(B) was performed at 60keV and 20keV, and low temperature transport combined with SQUID and ESR/LFMA was used in searching for SC. We have found that R(T) strongly depends on the metallic contact geometry. With thin film contacts on CNT sheets the R(T) shows no SC signatures, while when an Ag or Au paste penetrates the highly porous network of B doped multiwall CNT then R(T) drops and curvature changes are observed resembling SC transitions with Tc depending on B concentration and metallic electrode distances. We discuss these results in terms of possible SC in hybride ``metal-CNT'' system in which metal was predicted to supress phase fluctuation in one dimensional CNT network.

  1. Carbon nanotubes implanted manganese-based MOFs for simultaneous detection of biomolecules in body fluids.

    PubMed

    Wang, Min-Qiang; Ye, Cui; Bao, Shu-Juan; Zhang, Yan; Yu, Ya-Nan; Xu, Mao-wen

    2016-02-21

    Metal-organic frameworks (MOFs) have recently attracted much interest in electrochemical fields due to their controlled porosity, large internal surface area, and countless structural topologies. However, the direct application of single component MOFs is limited since they also exhibit poor electronic conductivity, low mechanical stability, and inferior electrocatalytic ability. To overcome these problems, we implanted multi-walled carbon nanotubes (MWCNTs) into manganese-based metal-organic frameworks (Mn-BDC) using a one-step solvothermal method and found that the introduction of MWCNTs can initiate the splitting of bulky Mn-BDC into thin layers. This splitting is highly significant in that it enhances the electronic conductivity and electrocatalytic ability of Mn-BDC. The constructed Mn-BDC@MWCNT composites were utilized as an electrode modifying material in the fabrication of an electrochemical sensor and then were used successfully for the determination of biomolecules in human body fluid. The sensor displayed successful detection performance with wide linear detection ranges (0.1-1150, 0.01-500, and 0.02-1100 μM for AA, DA and UA, respectively) and low limits of detection (0.01, 0.002, and 0.005 μM for AA, DA and UA, respectively); thus, this preliminary study presents an electrochemical biosensor constructed with a novel electrode modifying material that exhibits superior potential for the practical detection of AA, DA and UA in urine samples.

  2. Percutaneous and skeletal biocarbon implants

    NASA Technical Reports Server (NTRS)

    Mooney, V.

    1977-01-01

    Review of carbon implants developed by NASA discussed four different types of implants and subsequent improvements. Improvements could be of specific interest to rehabilitation centers and similar organizations.

  3. Percutaneous and skeletal biocarbon implants

    NASA Technical Reports Server (NTRS)

    Mooney, V.

    1977-01-01

    Review of carbon implants developed by NASA discussed four different types of implants and subsequent improvements. Improvements could be of specific interest to rehabilitation centers and similar organizations.

  4. Cooperative strings and glassy interfaces

    PubMed Central

    Salez, Thomas; Salez, Justin; Dalnoki-Veress, Kari; Raphaël, Elie; Forrest, James A.

    2015-01-01

    We introduce a minimal theory of glass formation based on the ideas of molecular crowding and resultant string-like cooperative rearrangement, and address the effects of free interfaces. In the bulk case, we obtain a scaling expression for the number of particles taking part in cooperative strings, and we recover the Adam–Gibbs description of glassy dynamics. Then, by including thermal dilatation, the Vogel–Fulcher–Tammann relation is derived. Moreover, the random and string-like characters of the cooperative rearrangement allow us to predict a temperature-dependent expression for the cooperative length ξ of bulk relaxation. Finally, we explore the influence of sample boundaries when the system size becomes comparable to ξ. The theory is in agreement with measurements of the glass-transition temperature of thin polymer films, and allows quantification of the temperature-dependent thickness hm of the interfacial mobile layer. PMID:26100908

  5. Cooperative strings and glassy interfaces.

    PubMed

    Salez, Thomas; Salez, Justin; Dalnoki-Veress, Kari; Raphaël, Elie; Forrest, James A

    2015-07-07

    We introduce a minimal theory of glass formation based on the ideas of molecular crowding and resultant string-like cooperative rearrangement, and address the effects of free interfaces. In the bulk case, we obtain a scaling expression for the number of particles taking part in cooperative strings, and we recover the Adam-Gibbs description of glassy dynamics. Then, by including thermal dilatation, the Vogel-Fulcher-Tammann relation is derived. Moreover, the random and string-like characters of the cooperative rearrangement allow us to predict a temperature-dependent expression for the cooperative length ξ of bulk relaxation. Finally, we explore the influence of sample boundaries when the system size becomes comparable to ξ. The theory is in agreement with measurements of the glass-transition temperature of thin polymer films, and allows quantification of the temperature-dependent thickness hm of the interfacial mobile layer.

  6. Effects of incident energy and angle on carbon cluster ions implantation on silicon substrate: a molecular dynamics study

    NASA Astrophysics Data System (ADS)

    Wei, Ye; Sang, Shengbo; Zhou, Bing; Deng, Xiao; Chai, Jing; Ji, Jianlong; Ge, Yang; Huo, Yuanliang; Zhang, Wendong

    2017-09-01

    Carbon cluster ion implantation is an important technique in fabricating functional devices at micro/nanoscale. In this work, a numerical model is constructed for implantation and implemented with a cutting-edge molecular dynamics method. A series of simulations with varying incident energies and incident angles is performed for incidence on silicon substrate and correlated effects are compared in detail. Meanwhile, the behavior of the cluster during implantation is also examined under elevated temperatures. By mapping the nanoscopic morphology with variable parameters, numerical formalism is proposed to explain the different impacts on phrase transition and surface pattern formation. Particularly, implantation efficiency (IE) is computed and further used to evaluate the performance of the overall process. The calculated results could be properly adopted as the theoretical basis for designing nano-structures and adjusting devices’ properties. Project supported by the National Natural Science Foundation of China (Nos. 51622507, 61471255, 61474079, 61403273, 51502193, 51205273), the Natural Science Foundation of Shanxi (Nos. 201601D021057, 201603D421035), the Youth Foundation Project of Shanxi Province (Nos. 2015021097), the Doctoral Fund of MOE of China (No. 20131402110013), the National High Technology Research and Development Program of China (No. 2015AA042601), and the Specialized Project in Public Welfare from The Ministry of Water Resources of China (Nos. 1261530110110).

  7. Optical properties of planar waveguides on ZnWO₄ formed by carbon and helium ion implantation and effects of annealing.

    PubMed

    Zhao, Jin-Hua; Liu, Tao; Guo, Sha-Sha; Guan, Jing; Wang, Xue-Lin

    2010-08-30

    We report on the optical properties of ZnWO(4) planar waveguides created by ion implantation, and the effect annealing has on these structures. Planar optical waveguides in ZnWO(4) crystals are fabricated by 5.0 MeV carbon ion implantation with a fluence of 1 × 10(15) ions/cm(2) or 500 keV helium ion implantation with the a fluence of 1 × 10(16) ions/cm(2). The thermal stability was investigated by 60 minute annealing cycles at different temperatures ranging from 260°C to 550°C in air. The guided modes were measured by a model 2010 prism coupler at wavelengths of 633 nm and 1539 nm. The reflectivity calculation method (RCM) was applied to simulate the refractive index profile in these waveguides. The near-field light intensity profiles were measured using the end-face coupling method. The absorption spectra show that the implantation processes have almost no influence on the visible band absorption.

  8. Effects of carbon and nitrogen plasma immersion ion implantation on in vitro and in vivo biocompatibility of titanium alloy.

    PubMed

    Zhao, Ying; Wong, Sze Man; Wong, Hoi Man; Wu, Shuilin; Hu, Tao; Yeung, Kelvin W K; Chu, Paul K

    2013-02-01

    Growth of bony tissues on titanium biomedical implants can be time-consuming, thereby prolonging recovery and hospitalization after surgery and a method to improve and expedite tissue-implant integration and healing is thus of scientific and clinical interests. In this work, nitrogen and carbon plasma immersion ion implantation (N-PIII and C-PIII) is conducted to modify Ti-6Al-4V to produce a graded surface layer composed of TiN and TiC, respectively. Both PIII processes do not significantly alter the surface hydrophilicity but increase the surface roughness and corrosion resistance. In vitro studies disclose improved cell adhesion and proliferation of MC3T3-E1 preosteoblasts and L929 fibroblasts after PIII. Micro-CT evaluation conducted 1 to 12 weeks after surgery reveals larger average bone volumes and less bone resorption on the N-PIII and C-PIII titanium alloy pins than the unimplanted one at every time point. The enhancements observed from both the in vitro and in vivo studies can be attributed to the good cytocompatibility, roughness, and corrosion resistance of the TiN and TiC structures which stimulate the response of preosteoblasts and fibroblasts and induce early bone formation. Comparing the two PIII processes, N-PIII is more effective and our results suggest a simple and practical means to improve the surface biocompatibility of medical-grade titanium alloy implants.

  9. Mechanical and physical properties of carbon-graphite fiber-reinforced polymers intended for implant suprastructures.

    PubMed

    Segerström, Susanna; Ruyter, I Eystein

    2007-09-01

    Mechanical properties and quality of fiber/matrix adhesion of poly(methyl methacrylate) (PMMA)-based materials, reinforced with carbon-graphite (CG) fibers that are able to remain in a plastic state until polymerization, were examined. Tubes of cleaned braided CG fibers were treated with a sizing resin. Two resin mixtures, resin A and resin B, stable in the fluid state and containing different cross-linking agents, were reinforced with CG fiber loadings of 24, 36, and 47 wt% (20, 29, and 38 vol.%). In addition, resin B was reinforced with 58 wt% (47 vol.%). After heat-polymerization, flexural strength and modulus were evaluated, both dry and after water storage. Coefficient of thermal expansion, longitudinally and in the transverse direction of the specimens, was determined. Adhesion between fibers and matrix was evaluated with scanning electron microscopy (SEM). Flexural properties and linear coefficient of thermal expansion were similar for both fiber composites. With increased fiber loading, flexural properties increased. For 47 wt% fibers in polymer A the flexural strength was 547.7 (28.12) MPa and for polymer B 563.3 (89.24) MPa when water saturated. Linear coefficient of thermal expansion was for 47 wt% CG fiber-reinforced polymers; -2.5 x 10(-6) degrees C-1 longitudinally and 62.4 x 10(-6) degrees C-1 in the transverse direction of the specimens. SEM revealed good adhesion between fibers and matrix. More porosity was observed with fiber loading of 58 wt%. The fiber treatment and the developed resin matrices resulted in good adhesion between CG fibers and matrix. The properties observed indicate a potential for implant-retained prostheses.

  10. Temperature dependent properties of silicon containing diamondlike carbon films prepared by plasma source ion implantation

    NASA Astrophysics Data System (ADS)

    Hatada, R.; Flege, S.; Baba, K.; Ensinger, W.; Kleebe, H.-J.; Sethmann, I.; Lauterbach, S.

    2010-04-01

    Silicon containing diamondlike carbon (Si-DLC) films were prepared on silicon wafer substrates by a plasma source ion implantation method with negative pulses superposed on a negative dc voltage. A mixture of acetylene and tetramethylsilane gas was introduced into the discharge chamber as working gases for plasma formation. Ions produced in the plasma are accelerated toward a substrate holder because of the negative voltage applied directly to it. After deposition, the films were annealed for 0.5 h in ambient air at temperatures up to 923 K in order to evaluate the thermal stability of the Si-DLC films. The films were analyzed by x-ray photoelectron spectroscopy (XPS), high resolution transmission electron microscopy, and Raman spectroscopy. The surface morphology of the films and the film thickness were observed by atomic force microscopy and scanning electron microscopy. The mechanical and tribological properties were investigated by an indentation method and a ball-on-disk test. The results show the silicon containing DLC films were amorphous and the surface roughness of the Si containing DLC films was very smooth and no special structure was observed. Integrated intensity ratios ID/IG of Raman spectroscopy of the Si containing DLC films decreased with Si content. The Raman spectra showed that the structure of the Si-free DLC film changed to a graphitelike structure with increasing annealing temperature, whereas that of the 24 at. % Si containing DLC films did not change at the maximum temperature used in this study. A very low friction coefficient was obtained for the 13 at. % Si containing DLC film. The surface roughness and the hardness of the films changed with increasing annealing temperature. The formation of Si oxide in a near surface layer was confirmed by XPS and it prevents further oxidation of the inside of the film. Heat resistivity of DLC films can be improved by Si addition into the DLC films.

  11. Application of Laser-Induced Bone Therapy by Carbon Dioxide Laser Irradiation in Implant Therapy

    PubMed Central

    Naka, Takahiro; Yokose, Satoshi

    2012-01-01

    This study evaluated the application of laser-induced bone therapy (LIBT) to reduce implant healing time in rat tibia. Twenty 10-week-old female Sprague-Dawlay rats were used. The rats received laser irradiation (laser group) or sham operation (control group) on either side of the tibia. Five days after invasion, titanium implants were inserted in proximal tibia. Five, 10, and 20 days after implant placement, tibiae were collected. After taking micro-CT and performing a torque test, the tibiae were decalcified and 8-μm-thick sections were prepared. Specimens were stained with hematoxylin and eosin. Results. Micro-CT images, removal torque values, and histomorphometric analysis data demonstrated a significantly accelerated bone formation in the laser group earlier in the healing process. Conclusion. The use of laser irradiation was effective in promoting bone formation and acquiring osseointegration of titanium implants inserted in rat tibia. LIBT may be suitable for use in implant therapy. PMID:22505900

  12. Suppression of the uranium-hydrogen reaction using high-dose carbon implantation

    SciTech Connect

    Musket, R.G.

    1987-04-17

    We have previously reported the delay and reduction of the hydriding of uranium by implantation of oxygen. The reduced hydriding was attributed to the presence of the uranium oxide layer created near room temperature. In this paper we present results for the layers formed by implantation of 80 keV C/sup +/ to a dose of 8E17 C/cm/sup 2/. The carbide layers formed were characterized by Auger electron spectroscopy, Rutherford backscattering, and glancing angle x-ray diffraction. Hydriding properties of both non-implanted and implanted uranium were measured for 76 Torr hydrogen at 130/sup 0/C. The implanted specimens had significantly longer incubation times for the start of the reaction after exposure to hydrogen and less area participating in the reaction.

  13. Bone formation in a carbonate-substituted hydroxyapatite implant is inhibited by zoledronate: the importance of bioresorption to osteoconduction.

    PubMed

    Spence, G; Phillips, S; Campion, C; Brooks, R; Rushton, N

    2008-12-01

    Carbonate-substituted hydroxyapatite (CHA) is more osteoconductive and more resorbable than hydroxyapatite (HA), but the underlying mode of its action is unclear. We hypothesised that increased resorption of the ceramic by osteoclasts might subsequently upregulate osteoblasts by a coupling mechanism, and sought to test this in a large animal model. Defects were created in both the lateral femoral condyles of 12 adult sheep. Six were implanted with CHA granules bilaterally, and six with HA. Six of the animals in each group received the bisphosphonate zoledronate (0.05 mg/kg), which inhibits the function of osteoclasts, intra-operatively. After six weeks bony ingrowth was greater in the CHA implants than in HA, but not in the animals given zoledronate. Functional osteoclasts are necessary for the enhanced osteoconduction seen in CHA compared with HA.

  14. Biofunctionalization of carbon nanotubes/chitosan hybrids on Ti implants by atom layer deposited ZnO nanostructures

    NASA Astrophysics Data System (ADS)

    Zhu, Yizhou; Liu, Xiangmei; Yeung, Kelvin W. K.; Chu, Paul K.; Wu, Shuilin

    2017-04-01

    One-dimensional (1D) nanostructures of ZnO using atomic layer deposition (ALD) on chitosan (CS) modified carbon nanotubes (CNTs) were first introduced onto the surfaces of biomedical implants. When the content of ZnO is not sufficient, CNTs can strengthen the antibacterial activity against E. coli and S. aureus by 8% and 39%, respectively. CS can improve the cytocompatibility of CNTs and ZnO. The amount of Zn content can be controlled by changing the cycling numbers of ALD processes. This hybrid coating can not only endow medical implants with high self-antibacterial efficacy against Escherichia coli (E. coli) and Staphylococcus aureus (S. aureus) of over 73% and 98%, respectively, but also regulate the proliferation and osteogenic differentiation of osteoblasts by controlling the amount of ZnO.

  15. Molecular mobility in glassy dispersions.

    PubMed

    Mehta, Mehak; McKenna, Gregory B; Suryanarayanan, Raj

    2016-05-28

    Dielectric spectroscopy was used to characterize the structural relaxation in pharmaceutical dispersions containing nifedipine (NIF) and either poly(vinyl) pyrrolidone (PVP) or hydroxypropyl methylcellulose acetate succinate (HPMCAS). The shape of the dielectric response (permittivity versus log time) curve was observed to be independent of temperature. Thus, for the pure NIF as well as the dispersions, the validity of the time-temperature superposition principle was established. Furthermore, though the shape of the full dielectric response varied with polymer concentration, the regime related to the α- or structural relaxation was found to superimpose for the dispersions, though not with the response of the NIF itself. Hence, there is a limited time-temperature-concentration superposition for these systems as well. Therefore, in this polymer concentration range, calculation of long relaxation times in these glass-forming systems becomes possible. We found that strong drug-polymer hydrogen bonding interactions improved the physical stability (i.e., delayed crystallization) by reducing the molecular mobility. The strength of hydrogen bonding, structural relaxation time, and crystallization followed the order: NIF-PV P>NIF-HPMCAS>NIF. With an increase in polymer concentration, the relaxation times were longer indicating a decrease in molecular mobility. The temperature dependence of relaxation time, in other words fragility, was independent of polymer concentration. This is the first application of the superposition principle to characterize structural relaxation in glassy pharmaceutical dispersions.

  16. Molecular mobility in glassy dispersions

    SciTech Connect

    Mehta, Mehak; McKenna, Gregory B.; Suryanarayanan, Raj

    2016-05-27

    Dielectric spectroscopy was used to characterize the structural relaxation in pharmaceutical dispersions containing nifedipine (NIF) and either poly(vinyl) pyrrolidone (PVP) or hydroxypropyl methylcellulose acetate succinate (HPMCAS). The shape of the dielectric response (permittivity versus log time) curve was observed to be independent of temperature. Thus, for the pure NIF as well as the dispersions, the validity of the time-temperature superposition principle was established. Furthermore, though the shape of the full dielectric response varied with polymer concentration, the regime related to the α- or structural relaxation was found to superimpose for the dispersions, though not with the response of the NIF itself. Hence, there is a limited time-temperature-concentration superposition for these systems as well. Therefore, in this polymer concentration range, calculation of long relaxation times in these glass-forming systems becomes possible. We found that strong drug-polymer hydrogen bonding interactions improved the physical stability (i.e., delayed crystallization) by reducing the molecular mobility. The strength of hydrogen bonding, structural relaxation time, and crystallization followed the order: NIF$-$PV P>NIF$-$HPMCAS>NIF. With an increase in polymer concentration, the relaxation times were longer indicating a decrease in molecular mobility. The temperature dependence of relaxation time, in other words fragility, was independent of polymer concentration. This is the first application of the superposition principle to characterize structural relaxation in glassy pharmaceutical dispersions.

  17. Molecular mobility in glassy dispersions

    NASA Astrophysics Data System (ADS)

    Mehta, Mehak; McKenna, Gregory B.; Suryanarayanan, Raj

    2016-05-01

    Dielectric spectroscopy was used to characterize the structural relaxation in pharmaceutical dispersions containing nifedipine (NIF) and either poly(vinyl) pyrrolidone (PVP) or hydroxypropyl methylcellulose acetate succinate (HPMCAS). The shape of the dielectric response (permittivity versus log time) curve was observed to be independent of temperature. Thus, for the pure NIF as well as the dispersions, the validity of the time-temperature superposition principle was established. Furthermore, though the shape of the full dielectric response varied with polymer concentration, the regime related to the α- or structural relaxation was found to superimpose for the dispersions, though not with the response of the NIF itself. Hence, there is a limited time-temperature-concentration superposition for these systems as well. Therefore, in this polymer concentration range, calculation of long relaxation times in these glass-forming systems becomes possible. We found that strong drug-polymer hydrogen bonding interactions improved the physical stability (i.e., delayed crystallization) by reducing the molecular mobility. The strength of hydrogen bonding, structural relaxation time, and crystallization followed the order: NIF-PV P>NIF-HPMCAS>NIF. With an increase in polymer concentration, the relaxation times were longer indicating a decrease in molecular mobility. The temperature dependence of relaxation time, in other words fragility, was independent of polymer concentration. This is the first application of the superposition principle to characterize structural relaxation in glassy pharmaceutical dispersions.

  18. Integration of Advanced Source and Drain Extension Process Using Carbon/Fluorine Co-Implants and Spike Anneal in 65nm PMOS Devices

    NASA Astrophysics Data System (ADS)

    Li, C. I.; Wang, H. Y.; Chien, C. C.; Chain, M.; Yang, C. L.; Tzou, S. F.; Graoui, H.; Foad, M. A.; Ting, Richard

    2006-11-01

    Carbon and fluorine co-implantation have shown encouraging junction formation improvement, especially for P-type junctions. In this paper, Xj of 20 nm, Rs of 730 ohms/sq and abruptness of 3.5 nm/decade were obtained using carbon co-implantation at 6 keV, 2×1015 ions/cm2, BF2 implant and spike annealing. With LSA, the sheet resistance decreases to 640 ohm/sq. Rs decreased 7% at 1050°C RTP and decreased 13% at 1000°C RTP combined with laser spike annealing. We implemented germanium, carbon, and fluorine co-implanted junctions for SDE fabrication for 65 nm node devices. Results indicated that both decrease in overlap capacitance and junction leakage have proportional correlation with C co-implant dosage. However, Vt needs to be optimized. Device optimization by combining C co-implantation with LSA can yield better control of short channel effects due to the co-implantation and better activation due to the LSA.

  19. Cranioplasty with individual carbon fibre reinforced polymere (CFRP) medical grade implants based on CAD/CAM technique.

    PubMed

    Saringer, W; Nöbauer-Huhmann, I; Knosp, E

    2002-11-01

    The authors present a new method for the reconstruction of large or complex-formed cranial bone defects using prefabricated, computer-generated, individual CFRP (carbon fibre reinforced plastics) medical grade implants. CFRP is a composite material containing carbon fibres embedded in an epoxy resin matrix. It is radiolucent, heat-resistant, extremely strong and light (its weight is 20% that of steel), has a modulus of elasticity close to that of bone, and an established biocompatibility. The utilisation of a CAD/CAM (computer aided design/computer aided manufacture) technique based on digitised computed tomography (CT) data, with stereolithographic modelling as intermediate step, enabled the production of individual, prefabricated CFRP medical grade implants with an arithmetical maximum aberration in extension of less than +/-0.25 mm. Between 1995 and February 2002, 29 patients (15 men and 14 women; mean age, 39.9 years; range, 16 to 67 years) underwent cranioplasty with CFRP medical grade implants at the neurosurgical department of the University of Vienna. Twenty-four patients were repaired secondarily (delayed cranioplasty) while 5 were repaired immediately following craniectomy (single stage cranioplasty). All cases were assessed for the accuracy of the intra-operative fit of the implant, restoration of the natural skull contour and aesthetics and adverse symptoms. The intra-operative fit was excellent in 93.1% and good in 6.9% of the implants. In two cases minor adjustments of the bony margin of the defect were required. The operating time for insertion ranged from 16 to 38 minutes, median 21 minutes. Postoperatively, 86.2% of the patients graded the restoration of their natural skull shape and symmetry as excellent while 13.8% termed it good. In one patient a non-space occupying subdural hygroma was found at the follow-up, but required no intervention. Two patients experienced atrophy of the frontal portion of the temporal muscle while one patient had a

  20. Uniform implantation of CNTs on total activated carbon surfaces: a smart engineering protocol for commercial supercapacitor applications

    NASA Astrophysics Data System (ADS)

    Jiang, Jian; Li, Linpo; Liu, Yani; Liu, Siyuan; Xu, Maowen; Zhu, Jianhui

    2017-04-01

    The main obstacles to building better supercapacitors are still trade-offs between energy and power parameters. To promote commercial supercapacitor behaviors, proper optimization toward electrode configurations/architectures may be a feasible and effective way. We herein propose a smart and reliable electrode engineering protocol, by in situ implantation of carbon nanotubes (CNTs) on total activated carbon (AC) surfaces via a mild chemical vapor deposition process at ∼550 °C, using nickel nitrate hydroxide (NNH) thin films and waste ethanol solvents as the catalyst and carbon sources, respectively. The direct and conformal growth of NNH layers onto carbonaceous scaffold guarantees the later uniform implantation of long and high-quality CNTs on total AC outer surfaces. Such fluffy and entangled CNTs preserve ionic diffusion channels, well connect neighboring ACs and function as superhighways for electrons transfer, endowing electrodes with outstanding capacitive behaviors including large output capacitances of ∼230 F g‑1 in 1 M Na2SO4 neutral solution and ∼502.5 F g‑1 in 6 M KOH using Ni valence state variation, and very negligible capacity decay in long-term cycles. Furthermore, a full symmetric supercapacitor device of CNTs@ACs//CNTs@ACs has been constructed, capable of delivering both high specific energy and power densities (maximum values reaching up to ∼97.2 Wh kg‑1 and ∼10.84 kW kg‑1), which holds great potential in competing with current mainstream supercapacitors.

  1. Uniform implantation of CNTs on total activated carbon surfaces: a smart engineering protocol for commercial supercapacitor applications.

    PubMed

    Jiang, Jian; Li, Linpo; Liu, Yani; Liu, Siyuan; Xu, Maowen; Zhu, Jianhui

    2017-04-07

    The main obstacles to building better supercapacitors are still trade-offs between energy and power parameters. To promote commercial supercapacitor behaviors, proper optimization toward electrode configurations/architectures may be a feasible and effective way. We herein propose a smart and reliable electrode engineering protocol, by in situ implantation of carbon nanotubes (CNTs) on total activated carbon (AC) surfaces via a mild chemical vapor deposition process at ∼550 °C, using nickel nitrate hydroxide (NNH) thin films and waste ethanol solvents as the catalyst and carbon sources, respectively. The direct and conformal growth of NNH layers onto carbonaceous scaffold guarantees the later uniform implantation of long and high-quality CNTs on total AC outer surfaces. Such fluffy and entangled CNTs preserve ionic diffusion channels, well connect neighboring ACs and function as superhighways for electrons transfer, endowing electrodes with outstanding capacitive behaviors including large output capacitances of ∼230 F g(-1) in 1 M Na2SO4 neutral solution and ∼502.5 F g(-1) in 6 M KOH using Ni valence state variation, and very negligible capacity decay in long-term cycles. Furthermore, a full symmetric supercapacitor device of CNTs@ACs//CNTs@ACs has been constructed, capable of delivering both high specific energy and power densities (maximum values reaching up to ∼97.2 Wh kg(-1) and ∼10.84 kW kg(-1)), which holds great potential in competing with current mainstream supercapacitors.

  2. Suppression of boron deactivation and diffusion in preamorphized silicon after nonmelt laser annealing by carbon co-implantation

    NASA Astrophysics Data System (ADS)

    Poon, Chyiu Hyia; See, Alex; Tan, Yunling; Zhou, Meisheng; Gui, Dong

    2008-04-01

    For preamorphized boron-implanted samples subjected to nonmelt laser spike annealing (LSA), increasing the LSA temperature at temperatures below 1250 °C results in negligible sheet resistance changes due to the formation of inactive boron-interstitial clusters (BICs). These clusters, which are evidenced as a kink in the boron profile beyond the amorphous/crystalline interface, result chiefly from the inadequate removal of end-of-range (EOR) defects. When the LSA temperature is elevated beyond 1250 °C, sheet resistance improvement takes place due to the increase in active boron dose from the dissolution of the BIC at higher temperatures. Cluster dissolution also gives rise to a supersaturation of silicon interstitials that deepen the junctions as a result of transient enhanced diffusion (TED). With an additional post-LSA treatment, severe deactivation, especially at lower LSA temperatures, and further TED is observed. Two concurrent mechanisms, namely, boron clustering (which gives rise to deactivation and sheet resistance degradation) and dissolution of the BIC (which gives rise to TED) formed during the LSA step, are believed to take place during the post-LSA thermal budget. As the LSA temperature increases, TED from the as-LSA profile upon rapid thermal annealing (RTA) is significantly reduced as a result of the improved effectiveness of the EOR defect dissolution during the higher temperature LSA step. When carbon co-implantation is performed, deactivation and TED is successfully suppressed with the reduction in free silicon interstitial concentration due to the formation of complexes of carbon and silicon interstitials. The amount of deactivation upon RTA becomes independent of LSA temperature for the carbon-implanted samples, largely because boron clustering becomes limited by the small concentration of free silicon interstitials present instead of the LSA temperatures used.

  3. 21 CFR 878.3500 - Polytetrafluoroethylene with carbon fibers composite implant material.

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ..., DEPARTMENT OF HEALTH AND HUMAN SERVICES (CONTINUED) MEDICAL DEVICES GENERAL AND PLASTIC SURGERY DEVICES... material intended to be implanted during surgery of the chin, jaw, nose, or bones or tissue near the eye...

  4. 21 CFR 878.3500 - Polytetrafluoroethylene with carbon fibers composite implant material.

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ..., DEPARTMENT OF HEALTH AND HUMAN SERVICES (CONTINUED) MEDICAL DEVICES GENERAL AND PLASTIC SURGERY DEVICES... material intended to be implanted during surgery of the chin, jaw, nose, or bones or tissue near the eye...

  5. 21 CFR 878.3500 - Polytetrafluoroethylene with carbon fibers composite implant material.

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ..., DEPARTMENT OF HEALTH AND HUMAN SERVICES (CONTINUED) MEDICAL DEVICES GENERAL AND PLASTIC SURGERY DEVICES... material intended to be implanted during surgery of the chin, jaw, nose, or bones or tissue near the eye...

  6. 21 CFR 878.3500 - Polytetrafluoroethylene with carbon fibers composite implant material.

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ..., DEPARTMENT OF HEALTH AND HUMAN SERVICES (CONTINUED) MEDICAL DEVICES GENERAL AND PLASTIC SURGERY DEVICES... material intended to be implanted during surgery of the chin, jaw, nose, or bones or tissue near the eye or...

  7. 21 CFR 878.3500 - Polytetrafluoroethylene with carbon fibers composite implant material.

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ..., DEPARTMENT OF HEALTH AND HUMAN SERVICES (CONTINUED) MEDICAL DEVICES GENERAL AND PLASTIC SURGERY DEVICES... material intended to be implanted during surgery of the chin, jaw, nose, or bones or tissue near the eye or...

  8. Carbon implanted waveguides in soda lime glass doped with Yb3+ and Er3+ for visible light emission

    NASA Astrophysics Data System (ADS)

    Vázquez, G. V.; Valiente, R.; Gómez-Salces, S.; Flores-Romero, E.; Rickards, J.; Trejo-Luna, R.

    2016-05-01

    Channel waveguides were fabricated by carbon implantation in soda lime glass samples doped with Er3+ and Yb3+, exhibiting good confinement and both monomode and multimode behaviour at 633 nm. Excitation at near infrared (NIR) and ultraviolet (UV) spectral ranges were used in order to obtain anti-Stokes (upconversion) and Stokes (downshift) emission in the visible range, respectively. The characteristic green and red bands of Er3+ transitions were observed, showing the potential of Yb3+ and Er3+ co-doping for the generation of visible guided emission under NIR excitation.

  9. Room-temperature continuous wave laser oscillations in Nd:YAG ceramic waveguides produced by carbon ion implantation

    NASA Astrophysics Data System (ADS)

    Tan, Y.; Zhang, C.; Chen, F.; Liu, F.-Q.; Jaque, D.; Lu, Q.-M.

    2011-06-01

    We report on the generation of continuous wave lasers at a wavelength of ˜1064 nm in a Nd:YAG ceramic waveguide at room temperature. The waveguide was fabricated by using 6 MeV carbon ion implantation at a fluence of 3×1014 ions/cm2. Laser operation has been realized with a slope efficiency as high as ˜11%. The pump threshold of an 808-nm laser beam for the waveguide laser oscillation is 19.5 mW.

  10. Simulation of lunar carbon chemistry. II - Lunar winds contribution

    NASA Technical Reports Server (NTRS)

    Bibring, J. P.; Langevin, Y.; Maurette, M.; Burlingame, A. L.; Wszolek, P. C.

    1974-01-01

    Simulation experiments, computations, and analysis of glassy agglutinates show that a directly condensed lunar wind vapor phase is strongly depleted in carbon and sulfur compounds and may recrystallize rapidly in the lunar thermal cycle and separate from host crystals. Factors preventing identification of low-energy species implanted from the lunar atmosphere are discussed. Computational results indicate that the implanted lunar winds carbon originates both from the vapor phases injected into the lunar atmosphere during thermal metamorphism of mature lunar soil grains and from direct volatization of impacting micrometeorites. It is suggested that microglass splashes and tiny crystalline grains possibly attached to the surface of coarser grains do not affect the characteristics of solar wind carbon chemistry in the lunar soil.

  11. An amperometric biosensor based on horseradish peroxidase immobilized onto maize tassel-multi-walled carbon nanotubes modified glassy carbon electrode for determination of heavy metal ions in aqueous solution.

    PubMed

    Moyo, Mambo; Okonkwo, Jonathan O; Agyei, Nana M

    2014-03-05

    A biosensor for trace metal ions based on horseradish peroxidase (HRP) immobilized on maize tassel-multiwalled carbon nanotube (MT-MWCNT) through electrostatic interactions is described herein. The biosensor was characterized using Fourier transform infrared (FTIR), UV-vis spectrometry, voltammetric and amperometric methods. The FTIR and UV-vis results inferred that HRP was not denatured during its immobilization on MT-MWCNT composite. The biosensing principle was based on the determination of the cathodic responses of the immobilized HRP to H₂O₂, before and after incubation in trace metal standard solutions. Under optimum conditions, the inhibition rates of trace metals were proportional to their concentrations in the range of 0.092-0.55 mg L⁻¹, 0.068-2 mg L⁻¹ for Pb²⁺ and Cu²⁺ respectively. The limits of detection were 2.5 μg L⁻¹ for Pb²⁺ and 4.2 μg L⁻¹ for Cu²⁺. Representative Dixon and Cornish-Bowden plots were used to deduce the mode of inhibition induced by the trace metal ions. The inhibition was reversible and mixed for both metal ions. Furthermore, the biosensor showed good stability, selectivity, repeatability and reproducibility. Copyright © 2013 Elsevier Inc. All rights reserved.

  12. Diffusion of co-implanted carbon and boron in silicon and its effect on excess self-interstitials

    SciTech Connect

    Uematsu, Masashi

    2012-04-01

    Diffusion of co-implanted carbon (C) and boron (B) in silicon (Si) and its effect on excess Si self-interstitials (I's) after annealing at 800 and 1000 deg. C were investigated by means of secondary ion mass spectrometry. The experimental results showed that C diffusion was not significant at 800 and 1000 deg. C but later became visible for longer annealing times at 1000 deg. C. B diffusion was reduced by the presence of C when no significant C diffusion was observed, but it was enhanced when C diffusion was observed. These results indicate that all implanted C atoms form immobile CI clusters with excess I in the amount of implanted C and that these CI clusters are stable and trap I to reduce B diffusion. On the contrary, CI clusters are dissolved to emit I for longer annealing times at 1000 deg. C and both B and C diffusion are enhanced. Diffusion simulation based on these models fits the experimental profiles of B and C.

  13. Haemocompatibility of hydrogenated amorphous carbon (a-C:H) films synthesized by plasma immersion ion implantation-deposition

    NASA Astrophysics Data System (ADS)

    Yang, P.; Kwok, S. C. H.; Chu, P. K.; Leng, Y. X.; Chen, J. Y.; Wang, J.; Huang, N.

    2003-05-01

    Diamond-like-carbon has attracted much attention recently as a potential biomaterial in blood contacting biomedical devices. However, previous reports in this area have not adequately addressed the biocompatibility and acceptability of the materials in blood contacting applications. In this study, hydrogenated amorphous carbon (a-C:H) films were fabricated on silicon wafers (1 0 0) using plasma immersion ion implantation-deposition. A series of a-C:H films with different structures and chemical bonds were fabricated under different substrate voltages. The results indicate that film graphitization is promoted at higher substrate bias. The film deposited at a lower substrate bias of -75 V possesses better blood compatibility than the films at higher bias and stainless steel. Our results suggest two possible paths to improve the blood compatibility, suppression of the endogenic clotting system and reduction of platelet activation.

  14. Evaluation of Carbon Interstitial in C-ion Implanted ZnO Bulk Single Crystals by a Nuclear Reaction Analysis Study: An Origin of Low Resistivity

    SciTech Connect

    Izawa, Y.; Matsumoto, K.; Oga, T.; Kuriyama, K.; Kushida, K.; Kinomura, A.

    2011-12-23

    Nuclear reaction analysis (NRA) of carbon-implanted ZnO bulk single crystals (carbon concentration: 1.5x10{sup 20} cm{sup -3}), in conjunction with the channeling technique, using the {sup 12}C(d,p){sup 13}C and {sup 16}O(d,p){sup 17}O reactions shows the presence of the interstitial carbon (C{sub i}) and the occupancy of substitute sites of oxygen atoms. These results suggest that the variation in resistivity from the order of 10{sup 4} {Omega}cm(for un-implanted samples) to that of 10 {Omega}cm (for as-implanted ones) is attributed to the C{sub i} and/or its complex defects, which would act as a shallow donor in ZnO.

  15. Prospective study on cranioplasty with individual carbon fiber reinforced polymer (CFRP) implants produced by means of stereolithography.

    PubMed

    Wurm, Gabriele; Tomancok, Berndt; Holl, Kurt; Trenkler, Johannes

    2004-12-01

    The aim of this study was to evaluate the value of carbon fiber reinforced polymer (CFRP) cranial implants produced by means of 3-dimensional (3D) stereolithography (SL) and template modeling for reconstructions of complex or extensive cranial defects. A series of 41 cranioplasties with individual CFRP implants was performed in 37 patients between April 1996 and November 2002. Only patients with complex and/or large cranial defects were included, most of them having extended scarring or dural calcification and poor quality of the overlying soft-tissue cover after infection or multiple preceding operations. Involvement of frontal sinus, a known risk factor for complications after cranioplasty, was the case in 21 patients (51.2%). A computer-based 3D model of the skull with the bony defect was generated by means of stereolithography after acquisition, evaluation and transfer of the patient's helical computed tomography (CT) data. A wax template of the defect that was used to design the individual prosthesis-shape was invested in dental stone. Then, the cranial implant was fabricated out of CFRP by loosen mold. Reconstruction of defects measuring up to 17 x 9 cm was performed. The intra-operative fit of the implants was excellent in 36 (87.8%), good in 1 (2.4%), and fair in 4 (9.8%) of the cases. Problems of implant fit occurred because of extended scarring and poor quality of soft-tissue cover. Adverse reactions were observed in 5 patients (1 subdural, 1 subcutaneous hematoma, 2 infections, 1 allergic reaction). Excellent contours and a solid stable reconstruction have been maintained in 30 out of 35 remaining plates (mean follow-up 3.6 years). No adverse effects concerning postoperative imaging, the accuracy of electroencephalograms and radiation therapy have been observed. The authors believe that this relatively new technique represents an advance in the management of complex and large cranial defects, but seems less suitable for simple defects because of cost

  16. Synthesis of SiC microstructures in Si technology by high dose carbon implantation: Etch-stop properties

    SciTech Connect

    Serre, C.; Perez-Rodriguez, A.; Romano-Rodriguez, A.; Calvo-Barrio, L.; Morante, J.R.; Esteve, J.; Acero, M.C.; Skorupa, W.; Koegler, R.

    1997-06-01

    The use of high dose carbon ion implantation in Si for the production of membranes and microstructures is investigated. Si wafers were implanted with carbon doses of 10{sup 17} and 5 {times} 10{sup 17} cm{sup {minus}2}, at an energy of 300 keV and a temperature of 500 C. The structural analysis of these samples revealed the formation of a highly stable buried layer of crystalline {beta}-SiC precipitates aligned with the Si matrix. The etch-stop properties of this layer have been investigated using tetramethyl-ammonium hydroxide as etchant solution. Secondary ion mass spectrometry measurements performed on the etched samples have allowed an estimate of the minimum dose needed for obtaining an etch-stop layer to a value in the range 2 to 3 {times} 10{sup 17} ions/cm{sup 2}. This behavior has been explained assuming the existence of a percolation process in a SiC/Si binary system. Finally, very thin crystalline membranes and self-standing structures with average surface roughness in the range 6 to 7 nm have been obtained.

  17. Biocompatibility and Biomechanical Effect of Single Wall Carbon Nanotubes Implanted in the Corneal Stroma: A Proof of Concept Investigation

    PubMed Central

    Rodriguez, Alejandra E.; Rodriguez-Reinoso, Francisco; Gomez-Tejedor, Jose A.; Antolinos-Turpin, Carmen M.; Bataille, Laurent; Alio, Jorge L.

    2016-01-01

    Corneal ectatic disorders are characterized by a progressive weakening of the tissue due to biomechanical alterations of the corneal collagen fibers. Carbon nanostructures, mainly carbon nanotubes (CNTs) and graphene, are nanomaterials that offer extraordinary mechanical properties and are used to increase the rigidity of different materials and biomolecules such as collagen fibers. We conducted an experimental investigation where New Zealand rabbits were treated with a composition of CNTs suspended in balanced saline solution which was applied in the corneal tissue. Biocompatibility of the composition was assessed by means of histopathology analysis and mechanical properties by stress-strain measurements. Histopathology samples stained with blue Alcian showed that there were no fibrous scaring and no alterations in the mucopolysaccharides of the stroma. It also showed that there were no signs of active inflammation. These were confirmed when Masson trichrome staining was performed. Biomechanical evaluation assessed by means of tensile test showed that there is a trend to obtain higher levels of rigidity in those corneas implanted with CNTs, although these changes are not statistically significant (p > 0.05). Implanting CNTs is biocompatible and safe procedure for the corneal stroma which can lead to an increase in the rigidity of the collagen fibers. PMID:28116139

  18. Understanding rheological hysteresis in soft glassy materials.

    PubMed

    Radhakrishnan, Rangarajan; Divoux, Thibaut; Manneville, Sébastien; Fielding, Suzanne M

    2017-03-01

    Motivated by recent experimental studies of rheological hysteresis in soft glassy materials, we study numerically strain rate sweeps in simple yield stress fluids and viscosity bifurcating yield stress fluids. Our simulations of downward followed by upward strain rate sweeps, performed within fluidity models and t