WorldWideScience

Sample records for amperometry

  1. Exocytosis: using amperometry to study presynaptic mechanisms of neurotoxicity

    NARCIS (Netherlands)

    Westerink, R.H.S.

    2004-01-01

    The development of carbon fiber microelectrode amperometry enabled detailed investigation of the presynaptic response at the single cell level with single vesicle resolution. Consequently, amperometry allowed for detailed studies into the presynaptic mechanisms underlying neurotoxicity. This review

  2. Substrate-Dependent Kinetics in Tyrosinase-based Biosensing: Amperometry vs. Spectrophotometry

    NARCIS (Netherlands)

    Rassaei, Liza; Cui, Jin; Goluch, E.D.; Lemay, Serge Joseph Guy

    2012-01-01

    Despite the broad use of enzymes in electroanalytical biosensors, the influence of enzyme kinetics on the function of prototype sensors is often overlooked or neglected. In the present study, we employ amperometry as an alternative or complementary method to study the kinetics of tyrosinase, whose

  3. Rapid Detection of Bacillus anthracis Spores Using Immunomagnetic Separation and Amperometry

    Directory of Open Access Journals (Sweden)

    David F. Waller

    2016-12-01

    Full Text Available Portable detection and quantitation methods for Bacillus anthracis (anthrax spores in pure culture or in environmental samples are lacking. Here, an amperometric immunoassay has been developed utilizing immunomagnetic separation to capture the spores and remove potential interferents from test samples followed by amperometric measurement on a field-portable instrument. Antibody-conjugated magnetic beads and antibody-conjugated glucose oxidase were used in a sandwich format for the capture and detection of target spores. Glucose oxidase activity of spore pellets was measured indirectly via amperometry by applying a bias voltage after incubation with glucose, horseradish peroxidase, and the electron mediator 2,2′-azino-bis (3-ethylbenzthiazoline-6-sulphonic acid. Target capture was mediated by polyclonal antisera, whereas monoclonal antibodies were used for signal generation. This strategy maximized sensitivity (500 target spores, 5000 cfu/mL, while also providing a good specificity for Bacillus anthracis spores. Minimal signal deviation occurs in the presence of environmental interferents including soil and modified pH conditions, demonstrating the strengths of immunomagnetic separation. The simultaneous incubation of capture and detection antibodies and rapid substrate development (5 min result in short sample-to-signal times (less than an hour. With attributes comparable or exceeding that of ELISA and LFDs, amperometry is a low-cost, low-weight, and practical method for detecting anthrax spores in the field.

  4. Single cell amperometry reveals curcuminoids modulate the release of neurotransmitters during exocytosis from PC12 cells

    Science.gov (United States)

    Li, Xianchan; Mohammadi, Amir Saeid; Ewing, Andrew G.

    2016-01-01

    We used single cell amperometry to examine whether curcumin and bisdemethoxycurcumin (BDMC), substances that are suggested to affect learning and memory, can modulate monoamine release from PC12 cells. Our results indicate both curcumin and BDMC need long-term treatment (72 h in this study) to influence exocytosis effectively. By analyzing the parameters calculated from single exocytosis events, it can be concluded that curcumin and BDMC affect exocytosis through different mechanisms. Curcumin accelerates the event dynamics with no significant change of the monoamine amount released from single exocytotic events, whereas BDMC attenuates the amount from single exocytotic event with no significant change of the event dynamics. This comparison of the effect of curcumin and BDMC on exocytosis at the single cell level brings insight into their different mechanisms, which might lead to different biological actions. The effect of curcumin and BDMC on the opening and closing of the exocytotic fusion pore were also investigated. These results might be helpful for understanding the improvement of learning and memory and the anti-depression properties of curcuminoids. PMID:28579928

  5. Linear chrono-amperometry using re-dissolution: application to halides

    International Nuclear Information System (INIS)

    Perchard, J.-P.; Buvet, M.; Molina, R.

    1966-06-01

    The possibility of applying linear chrono-amperometry to analysis was studied using a falling-drop mercury electrode. Measurements of the cations were carried out by direct reduction or by prior formation of an amalgam, which is then oxidized. Using the first technique, the minimum concentration that can be attained is about 10 -6 M and the reproducibility of the results is of the order of 2%. With the second method the sensitivity is much improved: in the concentration range of 10 -7 to 10 -8 M, the scatter of the results is less than 10% if the agitation and temperature conditions are kept constant. The halides are determined by re-dissolving the mercurous halide deposit formed by electrolysis. From the analytical point of view, the sensitivity is limited in the domain where the phenomena can be interpreted and used. In the case of the chloride ion the lower limit of this zone is close to 10 -5 M; it is 10 -6 M for the bromide and less than 10 -7 M for the iodide. For lower concentrations, simple laws that might be applied in analysis are no longer valid. However, the splitting of the peak observed during the reduction of the mercurous iodide deposit was interpreted as showing that the mono-molecular Hg 2 I 2 layer formed on the drop has particular electrochemical properties. (authors) [fr

  6. Probing the redox metabolism in the strictly anaerobic, extremely thermophilic, hydrogen-producing Caldicellulosiruptor saccharolyticus using amperometry

    DEFF Research Database (Denmark)

    Kostesha, Natalie; Willquist, Karin; Emnéus, Jenny

    2011-01-01

    Changes in the redox metabolism in the anaerobic, extremely thermophilic, hydrogen-forming bacterium Caldicellulosiruptor saccharolyticus were probed for the first time in vivo using mediated amperometry with ferricyanide as a thermotolerant external mediator. Clear differences in the intracellul...... in the intracellular electron flow and to probe redox enzyme properties of a strictly anaerobic thermophile in vivo.......Changes in the redox metabolism in the anaerobic, extremely thermophilic, hydrogen-forming bacterium Caldicellulosiruptor saccharolyticus were probed for the first time in vivo using mediated amperometry with ferricyanide as a thermotolerant external mediator. Clear differences in the intracellular...... the NADH-dependent lactate dehydrogenase, upon which more NADH was directed to membrane-associated enzymes for ferricyanide reduction, leading to a higher electrochemical signal. The method is noninvasive and the results presented here demonstrate that this method can be used to accurately detect changes...

  7. Novel microfluidic system for online monitoring of biofilm dynamics by electrical impedance spectroscopy and amperometry

    Science.gov (United States)

    Bruchmann, Julia; Sachsenheimer, Kai; Schwartz, Thomas; Rapp, Bastian E.

    2016-03-01

    Biofilm formation is ubiquitous in nature where microorganisms attach to surfaces and form highly adapted and protected communities. In technical and industrial systems like drinking water supply, food production or shipping industry biofilms are a major cause of product contamination, biofouling, and biocorrosion. Therefore, understanding of biofilm formation and means of preventing biofilm formation is important to develop novel biofilm treatment strategies. A system allowing directly online detection and monitoring biofilm formation is necessary. However, until today, there are little to none technical systems featuring a non-destructive real-time characterization of biofilm formation in a highthroughput manner. This paper presents such a microfluidic system based on electrical impedance spectroscopy (EIS) and amperomertic current measurement. The sensor consists of four modules, each housing 24 independent electrodes within 12 microfluidic channels. Attached biomass on the electrodes is monitored as increased inhibition in charge transfer by EIS and a change in metabolic activity is measured as change in produced electric current by amperometry. This modular sensor system is highly adaptable and suitable for a broad range of microbiological applications. Among others, biofilm formation processes can be characterized online, biofilm manipulation like inactivation or destabilization can be monitored in real-time and gene expression can be analyzed in parallel. The use of different electrode designs allows effective biofilm studies during all biofilm phases. The whole system was recently extended by an integrated pneumatic microfluidic pump which enables easy handling procedures. Further developments of this pumping module will allow a fully- automated computer-controlled valving and pumping.

  8. Surface-modified CMOS IC electrochemical sensor array targeting single chromaffin cells for highly parallel amperometry measurements.

    Science.gov (United States)

    Huang, Meng; Delacruz, Joannalyn B; Ruelas, John C; Rathore, Shailendra S; Lindau, Manfred

    2018-01-01

    Amperometry is a powerful method to record quantal release events from chromaffin cells and is widely used to assess how specific drugs modify quantal size, kinetics of release, and early fusion pore properties. Surface-modified CMOS-based electrochemical sensor arrays allow simultaneous recordings from multiple cells. A reliable, low-cost technique is presented here for efficient targeting of single cells specifically to the electrode sites. An SU-8 microwell structure is patterned on the chip surface to provide insulation for the circuitry as well as cell trapping at the electrode sites. A shifted electrode design is also incorporated to increase the flexibility of the dimension and shape of the microwells. The sensitivity of the electrodes is validated by a dopamine injection experiment. Microwells with dimensions slightly larger than the cells to be trapped ensure excellent single-cell targeting efficiency, increasing the reliability and efficiency for on-chip single-cell amperometry measurements. The surface-modified device was validated with parallel recordings of live chromaffin cells trapped in the microwells. Rapid amperometric spikes with no diffusional broadening were observed, indicating that the trapped and recorded cells were in very close contact with the electrodes. The live cell recording confirms in a single experiment that spike parameters vary significantly from cell to cell but the large number of cells recorded simultaneously provides the statistical significance.

  9. Linear chrono-amperometry using re-dissolution: application to halides; La chronoamperometrie lineaire par redissolution: application aux halogenures

    Energy Technology Data Exchange (ETDEWEB)

    Perchard, J -P; Buvet, M; Molina, R [Commissariat a l' Energie Atomique, Centre d' Etudes Nucleaires de Fontenay-aux-Roses, 92 (France)

    1966-06-01

    The possibility of applying linear chrono-amperometry to analysis was studied using a falling-drop mercury electrode. Measurements of the cations were carried out by direct reduction or by prior formation of an amalgam, which is then oxidized. Using the first technique, the minimum concentration that can be attained is about 10{sup -6} M and the reproducibility of the results is of the order of 2%. With the second method the sensitivity is much improved: in the concentration range of 10{sup -7} to 10{sup -8} M, the scatter of the results is less than 10% if the agitation and temperature conditions are kept constant. The halides are determined by re-dissolving the mercurous halide deposit formed by electrolysis. From the analytical point of view, the sensitivity is limited in the domain where the phenomena can be interpreted and used. In the case of the chloride ion the lower limit of this zone is close to 10{sup -5} M; it is 10{sup -6} M for the bromide and less than 10{sup -7} M for the iodide. For lower concentrations, simple laws that might be applied in analysis are no longer valid. However, the splitting of the peak observed during the reduction of the mercurous iodide deposit was interpreted as showing that the mono-molecular Hg{sub 2}I{sub 2} layer formed on the drop has particular electrochemical properties. (authors) [French] Les possibilites analytiques de la chronoamperometrie lineaire ont ete etudiees en utilisant une electrode de mercure a goutte pendante. Le dosage des cations a ete effectue par reduction directe ou par formation prealable d'un amalgame puis oxydation de celui-ci. Par la premiere technique la concentration minimale que l'on peut atteindre est d'environ 10{sup -6} M et la reproductibilite des resultats est de l'ordre de 2%. Par la seconde methode la sensibilite se trouve grandement amelioree; dans une zone de concentration comprise entre 10{sup -7} et 10{sup -8} M, la dispersion des determinations est inferieure a 10% si les conditions

  10. An improved method for direct estimation of free cyanide in drinking water by Ion Chromatography-Pulsed Amperometry Detection (IC-PAD) on gold working electrode.

    Science.gov (United States)

    Kumar Meher, Alok; Labhsetwar, Nitin; Bansiwal, Amit

    2018-02-01

    In the present work a fast, reliable and safe Ion Exchange Chromatography-Pulsed Amperometry Detection (IC-PAD) method for direct determination of free cyanide in drinking water has been reported. To the best of our knowledge for the first time we are reporting the application of Gold working electrode for detection of free cyanide in a chromatography system. The system shows a wide linear range up to 8000µg/L. The electrode was found to have improved sensitivity and selectivity in the presence of interfering ions. The detection limit of the system was calculated to be 2µg/L. Long term evaluation of the electrode was found to be stable. Reproducible results were obtained from analysis of drinking water samples with recoveries of 98.3-101.2% and Relative Standard Deviations (RSD) of cyanide in drinking water. Copyright © 2017 Elsevier Ltd. All rights reserved.

  11. Assessment of functional changes in nanoparticle-exposed neuroendocrine cells with amperometry: exploring the generalizability of nanoparticle-vesicle matrix interactions.

    Science.gov (United States)

    Love, Sara A; Haynes, Christy L

    2010-09-01

    Using two of the most commonly synthesized noble metal nanoparticle preparations, citrate-reduced Au and Ag, the impacts of short-term accidental nanoparticle exposure are examined in primary culture murine adrenal medullary chromaffin cells. Transmission electron microscopy (TEM), inductively coupled plasma atomic emission spectroscopy (ICP-AES) and Alamar Blue viability studies revealed that nanoparticles are taken up by cells but do not decrease cell viability within 48 hours of exposure. Carbon-fiber microelectrode amperometry (CFMA) examination of exocytosis in nanoparticle-exposed cells revealed that nanoparticle exposure does lead to decreased secretion of chemical messenger molecules, of up to 32.5% at 48 hours of Au exposure. The kinetics of intravesicular species liberation also slows after nanoparticle exposure, between 30 and 50% for Au and Ag, respectively. Repeated stimulation of exocytosis demonstrated that these effects persisted during subsequent stimulations, meaning that nanoparticles do not interfere directly with the vesicle recycling machinery but also that cellular function is unable to recover following vesicle content expulsion. By comparing these trends with parallel studies done using mast cells, it is clear that similar exocytosis perturbations occur across cell types following noble metal nanoparticle exposure, supporting a generalizable effect of nanoparticle-vesicle interactions.

  12. Iodometric determination of platinum(4) using amperometry

    International Nuclear Information System (INIS)

    Zakharov, V.A.; Gavva, N.F.; Songina, O.A.

    1976-01-01

    The possibility of iodometric determination of platinum (4) by amperometric titration has been investigated. Titration has been conducted at zero potential of platinum reference electrode. Voltampere curves and absorption spectra of the solutions have been recorded to elucidate the nature of platinum (4) interaction with iodide-ion. It has been established that in the case of small excess of iodide complex [PtI 6 ] 2- is formed. When there is a considerable excess of KI, platinum (4) is reduced to Pt(2) with the formation of [PtI 4 ] 2 - and liberation of free iodine. Optimal for iodometric titration of Pt(4) is the use of acetate ot phosphate background solution with pH 6-8 with respect to 1M KI which is attained by adding 3 g of solid KI to 20 ml of the solution being titrated. Under these conditions the limit of platinum detection is 0.5 mkg/ml. Determination of Pt (4) is not hindered by the presence of 200-fold amounts of Cr(6), V(5), and Ni(2) as well as by 20-10-fold amounts of As(5), Sb(5), Se(4), Te(4), Rh(3), and Ir(3), Determination is hindered by the presence of Pd(2), Fe(3), Ir(4), and Cu(2) which, however, can easily be overcome. The possibility has been shown of using the developed technique for analysis of platinum catalysts and alloys

  13. Improved bacteria detection by coupling magneto-immunocapture and amperometry at flow-channel microband electrodes

    DEFF Research Database (Denmark)

    Laczka, Olivier; Maesa, José-María; Godino, Neus

    2011-01-01

    This paper describes the first immunosensing system reported for the detection of bacteria combining immunomagnetic capture and amperometric detection in a one-step sandwich format, and in a microfluidic environment. Detection is based on the electrochemical monitoring of the activity of horserad......This paper describes the first immunosensing system reported for the detection of bacteria combining immunomagnetic capture and amperometric detection in a one-step sandwich format, and in a microfluidic environment. Detection is based on the electrochemical monitoring of the activity...... product is then pumped along a microchannel, where it is amperometrically detected by a set of microelectrodes. This design avoids direct contact of the biocomponents with the electrode, which lowers the risk of electrode fouling. The whole assay can be completed in 1h. The experiments performed...... with Escherichia coli evidenced a linear response for concentrations ranging 102–108cellml−1, with a limit of detection of 55cellsml−1 in PBS, without pre-enrichment steps. Furthermore, 100cellsml−1 could be detected in milk, and with negligible interference by non-target bacteria such as Pseudomonas....

  14. Finding out egyptian gods' secret using analytical chemistry: biomedical properties of egyptian black makeup revealed by amperometry at single cells.

    Science.gov (United States)

    Tapsoba, Issa; Arbault, Stéphane; Walter, Philippe; Amatore, Christian

    2010-01-15

    Lead-based compounds were used during antiquity as both pigments and medicines in the formulation of makeup materials. Chemical analysis of cosmetics samples found in Egyptians tombs and the reconstitution of ancient recipes as reported by Greco-Roman authors have shown that two non-natural lead chlorides (laurionite Pb(OH)Cl and phosgenite Pb(2)Cl(2)CO(3)) were purposely synthesized and were used as fine powders in makeup and eye lotions. According to ancient Egyptian manuscripts, these were essential remedies for treating eye illness and skin ailments. This conclusion seems amazing because today we focus only on the well-recognized toxicity of lead salts. Here, using ultramicroelectrodes, we obtain new insights into the biochemical interactions between lead(II) ions and cells, which support the ancient medical use of sparingly soluble lead compounds. Submicromolar concentrations of Pb(2+) ions are shown to be sufficient for eliciting specific oxidative stress responses of keratinocytes. These consist essentially of an overproduction of nitrogen monoxide (NO degrees ). Owing to the biological role of NO degrees in stimulating nonspecific immunological defenses, one may argue that these lead compounds were deliberately manufactured and used in ancient Egyptian formulations to prevent and treat eye illnesses by promoting the action of immune cells.

  15. Electrochemical sensing of total antioxidant capacity and polyphenol content in wine samples using amperometry online-coupled with microdialysis.

    Science.gov (United States)

    Jakubec, Petr; Bancirova, Martina; Halouzka, Vladimir; Lojek, Antonin; Ciz, Milan; Denev, Petko; Cibicek, Norbert; Vacek, Jan; Vostalova, Jitka; Ulrichova, Jitka; Hrbac, Jan

    2012-08-15

    This work describes the method for total antioxidant capacity (TAC) and/or total content of phenolics (TCP) analysis in wines using microdialysis online-coupled with amperometric detection using a carbon microfiber working electrode. The system was tested on 10 selected wine samples, and the results were compared with total reactive antioxidant potential (TRAP), oxygen radical absorbance capacity (ORAC), and chemiluminescent determination of total antioxidant capacity (CL-TAC) methods using Trolox and catechin as standards. Microdialysis online-coupled with amperometric detection gives similar results to the widely used cyclic voltammetry methodology and closely correlates with ORAC and TRAP. The problem of electrode fouling is overcome by the introduction of an electrochemical cleaning step (1-2 min at the potential of 0 V vs Ag/AgCl). Such a procedure is sufficient to fully regenerate the electrode response for both red and white wine samples as well as catechin/Trolox standards. The appropriate size of microdialysis probes enables easy automation of the electrochemical TAC/TCP measurement using 96-well microtitration plates.

  16. Electrochemical Sensing of Total Antioxidant Capacity and Polyphenol Content in Wine Samples Using Amperometry Online-Coupled with Microdialysis

    Czech Academy of Sciences Publication Activity Database

    Jakubec, P.; Bančíčová, M.; Halouzka, V.; Lojek, Antonín; Číž, Milan; Denev, P.; Cibiček, N.; Vacek, J.; Vostálová, J.; Ulrichová, J.; Hrbáč, J.

    2012-01-01

    Roč. 60, č. 32 (2012), s. 7836-7843 ISSN 0021-8561 Grant - others:GA ČR(CZ) GAP303/12/G163; GA MPO(CZ) FR-TI4/457; PrF(CZ) PrF_2011_025 Program:GA Institutional research plan: CEZ:AV0Z50040702 Institutional support: RVO:68081707 Keywords : wine * antioxidant capacity * phenolics Subject RIV: BO - Biophysics Impact factor: 2.906, year: 2012

  17. Conductive Polymer Microelectrodes for on-chip measurement of transmitter release from living cells

    DEFF Research Database (Denmark)

    Larsen, Simon Tylsgaard; Matteucci, Marco; Taboryski, Rafael J.

    2012-01-01

    driven cell trapping inside closed chip devices. Conductive polymer microelectrodes were used to measure transmitter release using electrochemical methods such as cyclic voltammetry and constant potential amperometry. By measuring the oxidation current at a cyclic voltammogram, the concentration...

  18. TAPIR: a device for automatic titration with incremental weighing of the titration reagent

    International Nuclear Information System (INIS)

    Ganivet, Michel

    TAPIR is a titration device enabling automatic analyses with weighting of the titration reagent. The titration method used can be based on potentiometry, amperometry, color indicator change... The reproducibility is about 3.10 -4 [fr

  19. A Lab-on-a-disc platform for trapping of cells, monitoring of cell behaviour and evaluation of redox metabolism

    DEFF Research Database (Denmark)

    Amato, Letizia; Kuldeep, Kuldeep; Esmail Tehrani, Sheida

    2015-01-01

    In this work, we demonstrate an integrated electrochemical system on a centrifugal microfluidic platform for cell studies by combining electrochemical impedance spectroscopy and amperometry, and comparison of different cleaning protocols for gold electrodes on plastic substrate.......In this work, we demonstrate an integrated electrochemical system on a centrifugal microfluidic platform for cell studies by combining electrochemical impedance spectroscopy and amperometry, and comparison of different cleaning protocols for gold electrodes on plastic substrate....

  20. Study of electrochemical phosphate conversion coating of metallic surfaces

    International Nuclear Information System (INIS)

    Gougelin, Patrick

    1985-01-01

    After an overview on phosphate conversion coating processes, on models of iron electrochemical dissolution, on the passivation phenomenon, and on the phosphate conversion coating treatment, this research thesis reports a detailed study of this last process. The author presents the experimental method, reports the study of this process and of passivation under constant polarization. He reports the use of various techniques and conditions: chrono-amperometry, chrono-potentiometry, cyclic volt-amperometry

  1. Flow electrochemical biosensors based on enzymatic porous reactor and tubular detector of silver solid amalgam

    Czech Academy of Sciences Publication Activity Database

    Josypčuk, Bohdan; Barek, J.; Josypčuk, Oksana

    2013-01-01

    Roč. 778, MAY 2013 (2013), s. 24-30 ISSN 0003-2670 R&D Projects: GA ČR GAP206/11/1638 Institutional support: RVO:61388955 Keywords : flow analysis * amperometry * silver solid amalgam Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 4.517, year: 2013

  2. A novel non-enzymatic H{sub 2}O{sub 2} sensor based on polypyrrole nanofibers–silver nanoparticles decorated reduced graphene oxide nano composites

    Energy Technology Data Exchange (ETDEWEB)

    Moozarm Nia, Pooria, E-mail: pooriamn@yahoo.com; Lorestani, Farnaz, E-mail: farnaz.lorestani@siswa.um.edu.my; Meng, Woi Pei, E-mail: pmwoi@um.edu.my; Alias, Y., E-mail: yatimah70@um.edu.my

    2015-03-30

    Graphical abstract: - Highlights: • Decorating silver nanoparticles on the surface of graphene oxide nanocomposites. • Using and comparing two different electrochemical methods for reducing graphene oxide. • Investigating the effect of cyclic voltammetry and amperometry on electropolymerization of polypyrrole nanofibers. • The senor shows superior performances (LOD, LOQ, selectivity, repeatability, reproducibility and stability) towards H{sub 2}O{sub 2}. - Abstract: Graphene oxide (GO) decorated with silver nanoparticles (AgNPs), was electrochemically reduced on glassy carbon electrode (GCE) by an amperometry method (AMP-AgNPs-rGO/GCE). Then, Pyrrole was electropolymerized on the surface of the modified electrode through amperometry process in order to obtain nanofibers of polypyrrole (AMP-PpyNFs-AgNPs-rGO). Fourier-transform infrared transmission spectroscopy and X-ray diffraction approved that during the amperometry process, the GO and Ppy nanofibers were reduced and polymerized respectively and the silver nanoparticles were formed. Field emission scanning electron microscope images indicated that the silver nanoparticles were homogeneously distributed on the rGO surface with a narrow nano size distribution and polypyrrole synthesized in the form of nanofibers with diameter around 100 nm. The first linear section was in the range of 0.1–5 mM with a limit of detection of 1.099 and the second linear section raised to 90 mM with a correlation factor of 0.085 (S/N of 3)

  3. A novel non-enzymatic H2O2 sensor based on polypyrrole nanofibers–silver nanoparticles decorated reduced graphene oxide nano composites

    International Nuclear Information System (INIS)

    Moozarm Nia, Pooria; Lorestani, Farnaz; Meng, Woi Pei; Alias, Y.

    2015-01-01

    Graphical abstract: - Highlights: • Decorating silver nanoparticles on the surface of graphene oxide nanocomposites. • Using and comparing two different electrochemical methods for reducing graphene oxide. • Investigating the effect of cyclic voltammetry and amperometry on electropolymerization of polypyrrole nanofibers. • The senor shows superior performances (LOD, LOQ, selectivity, repeatability, reproducibility and stability) towards H 2 O 2 . - Abstract: Graphene oxide (GO) decorated with silver nanoparticles (AgNPs), was electrochemically reduced on glassy carbon electrode (GCE) by an amperometry method (AMP-AgNPs-rGO/GCE). Then, Pyrrole was electropolymerized on the surface of the modified electrode through amperometry process in order to obtain nanofibers of polypyrrole (AMP-PpyNFs-AgNPs-rGO). Fourier-transform infrared transmission spectroscopy and X-ray diffraction approved that during the amperometry process, the GO and Ppy nanofibers were reduced and polymerized respectively and the silver nanoparticles were formed. Field emission scanning electron microscope images indicated that the silver nanoparticles were homogeneously distributed on the rGO surface with a narrow nano size distribution and polypyrrole synthesized in the form of nanofibers with diameter around 100 nm. The first linear section was in the range of 0.1–5 mM with a limit of detection of 1.099 and the second linear section raised to 90 mM with a correlation factor of 0.085 (S/N of 3)

  4. Electrochemical Detection of Structurally Different Aminoacids by Thin Layers of Undoped and Doped ZnO.

    Czech Academy of Sciences Publication Activity Database

    Dytrych, Pavel; Klusoň, Petr; Stanovský, Petr; Šolcová, Olga

    2016-01-01

    Roč. 3, č. 10 (2016), s. 5706-5712 ISSN 2458-9403 R&D Projects: GA ČR GA15-14228S; GA ČR GA15-04790S Institutional support: RVO:67985858 Keywords : doped semiconductors * aminoacids * open circuit amperometry Subject RIV: CI - Industrial Chemistry, Chemical Engineering

  5. Amperometric Sensor for Heparin: Sensing Mechanism and Application in Human Blood Plasma Analysis

    Czech Academy of Sciences Publication Activity Database

    Langmaier, Jan; Olšák, J.; Samcová, E.; Samec, Zdeněk; Trojánek, Antonín

    2006-01-01

    Roč. 18, 13-14 (2006), s. 1329-1338 ISSN 1040-0397 R&D Projects: GA ČR GA203/04/0424 Institutional research plan: CEZ:AV0Z40400503 Keywords : heparin * amperometry * PVC membrane electrode * sensing mechanism * human blood plasma Subject RIV: CG - Electrochemistry Impact factor: 2.444, year: 2006

  6. Toluene-induced, Ca2+-dependent vesicular catecholamine release in rat PC12 cells

    NARCIS (Netherlands)

    Westerink, R.H.S.|info:eu-repo/dai/nl/239425952; Vijverberg, H.P.M.|info:eu-repo/dai/nl/068856474

    2002-01-01

    Acute effects of toluene on vesicular catecholamine release from intact PC12 phaeochromocytoma cells have been investigated using carbon fiber microelectrode amperometry. The frequency of vesicles released is low under basal conditions and is enhanced by depolarization. Toluene causes an increase in

  7. Amperometric Noise at Thin Film Band Electrodes

    DEFF Research Database (Denmark)

    Larsen, Simon T.; Heien, Michael L.; Taboryski, Rafael

    2012-01-01

    Background current noise is often a significant limitation when using constant-potential amperometry for biosensor application such as amperometric recordings of transmitter release from single cells through exocytosis. In this paper, we fabricated thin-film electrodes of gold and conductive...

  8. Toward a hydrogen peroxide sensor for exhaled breath analysis

    NARCIS (Netherlands)

    Wiedemair, Justyna; van Dorp, Henriëtte; Olthuis, Wouter; van den Berg, Albert

    2011-01-01

    In this contribution a chip-integrated amperometric sensor for the detection of H2O2 in exhaled breath condensate (EBC) is reported. The electrode chip is characterized, and detection of H2O2 in an aqueous phase is shown by means of cyclic voltammetry (CV) and amperometry. Variation of conditions

  9. Electrochemical Biosensors Based on Enzymatic Reactor of Silver Solid Amalgam Powder for Measurements in Flow Systems

    Czech Academy of Sciences Publication Activity Database

    Josypčuk, Oksana; Barek, J.; Josypčuk, Bohdan

    2014-01-01

    Roč. 26, č. 8 (2014), s. 1729-1738 ISSN 1040-0397 R&D Projects: GA ČR GAP206/11/1638 Institutional support: RVO:61388955 Keywords : Electrochemical biosensors * flow systems * Amperometry Subject RIV: CG - Electrochemistry Impact factor: 2.138, year: 2014

  10. 110 1*Atkuru Veera Venkata Naga Krishna Sunil Kumar, 2Chandra ...

    African Journals Online (AJOL)

    of VDL in biological fluids. These include HPLC with amperometry detection [3], HPLC with UV detection [4], HPLC with fluorescence detection. [5], LC-MS [6,7], GC-MS [8,9] and square-wave adsorption ... stability indicating liquid chromatography with. UV detection ... in drug analysis and the spectrophotometric methods ...

  11. Electro-active bio-films: formation, characterization and mechanisms

    International Nuclear Information System (INIS)

    Parot, Sandrine

    2007-01-01

    Some bacteria, which are able to exchange electrons with a conductive material without mediator form on conductive surfaces electro-active bio-films. This bacterial property has been recently discovered (2001). Objectives of this work are to develop electro-active bio-films in various natural environments from indigenous flora, then through complementary electrochemical techniques (chrono-amperometry and cyclic voltammetry), to evaluate electro-activity of isolates coming from so-formed bio-films and to characterize mechanisms of electron transfer between bacteria and materials. First, electro-active bio-films have been developed under chrono-amperometry in garden compost and in water coming from Guyana mangrove. These bio-films were respectively able to use an electrode as electron acceptor (oxidation) or as electron donor (reduction). In compost, results obtained in chrono-amperometry and cyclic voltammetry suggest a two-step electron transfer: slow substrate consumption, then rapid electron transfer between bacteria and the electrode. Thereafter, the ability to reduce oxygen was demonstrated with cyclic voltammetry for facultative aerobic isolates from compost bio-films (Enterobacter spp. and Pseudomonas spp.) and for aerobic isolates obtained from marine electro-active bio-films (Roseobacter spp. in majority). Finally, bio-films inducing current increase in chrono-amperometry were developed in bioreactor with synthetic medium from a pure culture of isolates. Hence, for the first time, electro-activity of several anaerobic strains of Geobacter bremensis isolated from compost bio-films was highlighted. (author) [fr

  12. Fabrication and Characterization of Ultrathin-ring Electrodes for Pseudo-steady-state Amperometric Detection.

    Science.gov (United States)

    Kitazumi, Yuki; Hamamoto, Katsumi; Noda, Tatsuo; Shirai, Osamu; Kano, Kenji

    2015-01-01

    The fabrication of ultrathin-ring electrodes with a diameter of 2 mm and a thickness of 100 nm is established. The ultrathin-ring electrodes provide a large density of pseudo-steady-state currents, and realize pseudo-steady-state amperometry under quiescent conditions without a Faraday cage. Under the limiting current conditions, the current response at the ultrathin-ring electrode can be well explained by the theory of the microband electrode response. Cyclic voltammograms at the ultrathin-ring electrode show sigmoidal characteristics with some hysteresis. Numerical simulation reveals that the hysteresis can be ascribed to the time-dependence of pseudo-steady-state current. The performance of amperometry with the ultrathin-ring electrode has been verified in its application to redox enzyme kinetic measurements.

  13. Studies on preparation of some alkaloid complexes and solvent extraction

    Energy Technology Data Exchange (ETDEWEB)

    Mohamed, A A

    1990-12-31

    Describes the various methods available in the literature for the determination of different classes of alkaloids spectrochemical (e.g.spectrophotometry and colorimetry, fluorimetry and phosphorimetry, nephelometry and reiractometry), electrochemical (e.g. polarography, amperometry, conductometry, coulometry and potentiometry), volumetric (e.q. acid-base, iodometry , bromimetry , oxidimetry, complexometry and precipitation ) and miscellaneous methods (e.g.gasliquid chromatography, gravimetry, thermometry and rediometry ) has been discussed. 31 tabs; 29 figs; 402 refs.

  14. Electrochemical analysis

    International Nuclear Information System (INIS)

    Hwang, Hun

    2007-02-01

    This book explains potentiometry, voltametry, amperometry and basic conception of conductometry with eleven chapters. It gives the specific descriptions on electrochemical cell and its mode, basic conception of electrochemical analysis on oxidation-reduction reaction, standard electrode potential, formal potential, faradaic current and faradaic process, mass transfer and overvoltage, potentiometry and indirect potentiometry, polarography with TAST, normal pulse and deferential pulse, voltammetry, conductometry and conductometric titration.

  15. Studies on preparation of some alkaloid complexes and solvent extraction

    International Nuclear Information System (INIS)

    Mohamed, A.A.

    1989-01-01

    Describes the various methods available in the literature for the determination of different classes of alkaloids spectrochemical (e.g.spectrophotometry and colorimetry, fluorimetry and phosphorimetry, nephelometry and reiractometry), electrochemical (e.g. polarography, amperometry, conductometry, coulometry and potentiometry), volumetric (e.q. acid-base, iodometry , bromimetry , oxidimetry, complexometry and precipitation ) and miscellaneous methods (e.g.gasliquid chromatography, gravimetry, thermometry and rediometry ) has been discussed

  16. Polymer electrolytes based on aromatic lithium sulfonyl-imide compounds; Electrolytes polymeres a base de sulfonylimidures de lithium aromatiques

    Energy Technology Data Exchange (ETDEWEB)

    Reibel, L.; Bayoudh, S. [Centre National de la Recherche Scientifique (CNRS), 67 - Strasbourg (France). Institut Charles Sadron; Baudry, P. [Electricite de France, 77 - Moret sur Loing (France). Direction des Etudes et Recherches; Majastre, H. [Bollore Technologies, 29 - Quimper (France); Herlem, G. [UFR de Sciences et Techniques, L.E.S., 25 - Besancon (France)

    1996-12-31

    This paper presents ionic conductivity results obtained with polymer electrolytes and also with propylene carbonate solutions. The domain of electrochemical activity of this salt has been determined using cycle volt-amperometry in propylene carbonate. Preliminary experiments on the stability of the polymer electrolyte with respect to the lithium electrode have been carried out for a possible subsequent use in lithium batteries. (J.S.) 4 refs.

  17. Coupling conducting polymers and mediated electrochemical responses for the detection of Listeria

    International Nuclear Information System (INIS)

    Minett, A.I.; Barisci, J.N.; Wallace, G.G.

    2003-01-01

    Different signal generation techniques were investigated for the development of a biosensor for Listeria monocytogenes. Conventional amperometry at an antibody-containing polypyrrole film electrode was found to be unsuccessful in detecting levels below 10 6 cells ml -1 . More successful was the coupling of a covalently modified film with the use of electron mediators in a single device. This sensor was capable of reproducibly detecting Listeria at levels of 10 5 cells ml -1 in 30 min

  18. Amperometric Adhesion Signals of Liposomes, Cells and Droplets

    OpenAIRE

    Ivošević DeNardis, N.; Žutić, V.; Svetličić, V.; Frkanec, R.

    2009-01-01

    Individual soft microparticles (liposomes, living cells and organic droplets) in aqueous media are characterized by their adhesion signals using amperometry at the dropping mercury electrode. We confirmed that the general mechanism established for adhesion of hydrocarbon droplets and cells is valid as well for liposome adhesion within a wide range of surface charge densities. Incidents and shape of adhesion signals in liposome suspensions reflect liposome polydispersity, surface charge den...

  19. A planar, solid-state amperometric sensor for nitrogen dioxide, employing an ionic liquid electrolyte contained in a polymeric matrix

    Czech Academy of Sciences Publication Activity Database

    Nádherná, M.; Opekar, F.; Reiter, Jakub; Stulík, K.

    2012-01-01

    Roč. 161, č. 1 (2012), s. 811-817 ISSN 0925-4005 R&D Projects: GA MŠk LC523; GA AV ČR KJB200320901 Institutional research plan: CEZ:AV0Z40320502 Keywords : Amperometry * Gas sensor * Solid-state sensor * Planar sensor * Ionic liquid * Solid polymer electrolyte * Gold minigrid electrode * Nitrogen dioxide Subject RIV: CG - Electrochemistry Impact factor: 3.535, year: 2012

  20. Paper-Based Digital Microfluidic Chip for Multiple Electrochemical Assay Operated by a Wireless Portable Control System

    DEFF Research Database (Denmark)

    Ruecha, Nipapan; Lee, Jumi; Chae, Heedo

    2017-01-01

    for multiple analysis assays are fabricated by affordable printing techniques. For enhanced sensitivity of the sensor, the working electrode is modified through the electrochemical method, namely by reducing graphene with voltammetry and coating gold nanoparticles by amperometry. Detachable sensor and absorber...... designed portable power supply and wireless control system, the active paper-based chip platform can be utilized as an advanced point-of-care device for multiple assays in digital microfluidics....

  1. ELECTROCHEMICAL STUDY OF RHENIUM-TELLURIUM-COPPER SYSTEM

    OpenAIRE

    E.A.Salakhova*1, D.B.Tagiyev2, P.E.Kalantarova3 and A.M.Askerova4

    2017-01-01

    The formation of the triple alloys Re-Te-Cu on the platinum electrode at volt amperemetric cycling has been studied. The investigation was carried out from chloride acidic solution containing tellurium acid, potassium perrhenate, chloride copper. The kinetics of the processes was controlled using the measurements by the method of cyclic volt-amperometry on the device İVİUMSTAT. For the analysis of composition and structure the methods of XRD (X-ray diffraction analysis) were used, and the inv...

  2. Electrochemical Quantification of the Antioxidant Capacity of Medicinal Plants Using Biosensors

    OpenAIRE

    Erika Rodríguez-Sevilla; María-Teresa Ramírez-Silva; Mario Romero-Romo; Pedro Ibarra-Escutia; Manuel Palomar-Pardavé

    2014-01-01

    The working area of a screen-printed electrode, SPE, was modified with the enzyme tyrosinase (Tyr) using different immobilization methods, namely entrapment with water-soluble polyvinyl alcohol (PVA), cross-linking using glutaraldehyde (GA), and cross-linking using GA and human serum albumin (HSA); the resulting electrodes were termed SPE/Tyr/PVA, SPE/Tyr/GA and SPE/Tyr/HSA/GA, respectively. These biosensors were characterized by means of amperometry and EIS techniques. From amperometric eval...

  3. Real-time multi-parameter cell-based analysis platform

    DEFF Research Database (Denmark)

    Caviglia, Claudia

    biomedical diagnostic techniques, drug discovery and screening. My project focused on the further development, improvement and exploration of the EXCELL microfluidic platform with particular interest in drug kinetic monitoring and neurotransmitter detection. The aim was to perform multi-parameter real...... of protocols and procedures for performing different cellular assays. (2) Electrochemical impedance spectroscopy (EIS) applied for drug screening and drug delivery in cancer research and wound healing studies. (3) Amperometry for monitoring of neurotransmitter exocytosis, relevant in research on Parkinson...

  4. Polymer electrolytes based on aromatic lithium sulfonyl-imide compounds; Electrolytes polymeres a base de sulfonylimidures de lithium aromatiques

    Energy Technology Data Exchange (ETDEWEB)

    Reibel, L; Bayoudh, S [Centre National de la Recherche Scientifique (CNRS), 67 - Strasbourg (France). Institut Charles Sadron; Baudry, P [Electricite de France, 77 - Moret sur Loing (France). Direction des Etudes et Recherches; Majastre, H [Bollore Technologies, 29 - Quimper (France); Herlem, G [UFR de Sciences et Techniques, L.E.S., 25 - Besancon (France)

    1997-12-31

    This paper presents ionic conductivity results obtained with polymer electrolytes and also with propylene carbonate solutions. The domain of electrochemical activity of this salt has been determined using cycle volt-amperometry in propylene carbonate. Preliminary experiments on the stability of the polymer electrolyte with respect to the lithium electrode have been carried out for a possible subsequent use in lithium batteries. (J.S.) 4 refs.

  5. A novel non-enzymatic H2O2 sensor based on polypyrrole nanofibers-silver nanoparticles decorated reduced graphene oxide nano composites

    Science.gov (United States)

    Moozarm Nia, Pooria; Lorestani, Farnaz; Meng, Woi Pei; Alias, Y.

    2015-03-01

    Graphene oxide (GO) decorated with silver nanoparticles (AgNPs), was electrochemically reduced on glassy carbon electrode (GCE) by an amperometry method (AMP-AgNPs-rGO/GCE). Then, Pyrrole was electropolymerized on the surface of the modified electrode through amperometry process in order to obtain nanofibers of polypyrrole (AMP-PpyNFs-AgNPs-rGO). Fourier-transform infrared transmission spectroscopy and X-ray diffraction approved that during the amperometry process, the GO and Ppy nanofibers were reduced and polymerized respectively and the silver nanoparticles were formed. Field emission scanning electron microscope images indicated that the silver nanoparticles were homogeneously distributed on the rGO surface with a narrow nano size distribution and polypyrrole synthesized in the form of nanofibers with diameter around 100 nm. The first linear section was in the range of 0.1-5 mM with a limit of detection of 1.099 and the second linear section raised to 90 mM with a correlation factor of 0.085 (S/N of 3)

  6. A novel bi-enzyme electrochemical biosensor for selective and sensitive determination of methyl salicylate.

    Science.gov (United States)

    Fang, Yi; Umasankar, Yogeswaran; Ramasamy, Ramaraja P

    2016-07-15

    An amperometric sensor based on a bi-enzyme modified electrode was fabricated to detect methyl salicylate, a volatile organic compound released by pathogen-infected plants via systemic response. The detection is based on cascadic conversion reactions that result in an amperometric electrochemical signal. The bi-enzyme electrode is made of alcohol oxidase and horseradish peroxidase enzymes immobilized on to a carbon nanotube matrix through a molecular tethering method. Methyl salicylate undergoes hydrolysis to form methanol, which is consumed by alcohol oxidase to form formaldehyde while simultaneously reducing oxygen to hydrogen peroxide. The hydrogen peroxide will be further reduced to water by horseradish peroxidase, which results in an amperometric signal via direct electron transfer. The bi-enzyme biosensor was evaluated by cyclic voltammetry and constant potential amperometry using hydrolyzed methyl salicylate as the analyte. The sensitivity of the bi-enzyme biosensor as determined by cyclic voltammetry and constant potential amperometry were 112.37 and 282.82μAcm(-2)mM(-1) respectively, and the corresponding limits of detection were 22.95 and 0.98μM respectively. Constant potential amperometry was also used to evaluate durability, repeatability and interference from other compounds. Wintergreen oil was used for real sample study to establish the application of the bi-enzyme sensor for selective determination of plant pathogen infections. Copyright © 2016 Elsevier B.V. All rights reserved.

  7. All polymer chip for amperometric studies of transmitter release from large groups of neuronal cells

    DEFF Research Database (Denmark)

    Larsen, Simon T.; Taboryski, Rafael

    2012-01-01

    We present an all polymer electrochemical chip for simple detection of transmitter release from large groups of cultured PC 12 cells. Conductive polymer PEDOT:tosylate microelectrodes were used together with constant potential amperometry to obtain easy-to-analyze oxidation signals from potassium......-induced release of transmitter molecules. The nature of the resulting current peaks is discussed, and the time for restoring transmitter reservoirs is studied. The relationship between released transmitters and potassium concentration was found to fit to a sigmoidal dose–response curve. Finally, we demonstrate...

  8. A new approach of the understanding of sulfur dioxide reduction in non-aqueous solvent; Une nouvelle approche de la comprehension de la reduction du dioxyde de soufre en solvant non aqueux

    Energy Technology Data Exchange (ETDEWEB)

    Potteau, E.; Levillain, E.; Lelieur, J.P. [Laboratoire de Spectrochimie Infrarouge et Raman (LASIR, UPR 2631 CNRS) Haute Etudes Industrielles (HEI), 59 - Lille (France)

    1996-12-31

    The study of SO{sub 2} reduction in non-aqueous solvent can help to understand the functioning of Li/SO{sub 2} batteries and to find a simpler way for the synthesis of Li{sub 2}S{sub 2}O{sub 4} dithionite. This paper presents the results of electrochemical studies (cycle volt-amperometry in semi-infinite and thin film diffusion conditions, visible spectro-electrochemistry) and spectroscopic studies (UV, visible and RPE) performed on SO{sub 2} solutions. A mechanism of SO{sub 2} reduction is proposed and discussed. (J.S.) 18 refs.

  9. Interference-Free Electrochemical Detection of Nanomolar Dopamine Using Doped Polypyrrole and Silver Nanoparticles

    OpenAIRE

    Saha, Suparna; Sarkar, Priyabrata; Turner, Anthony

    2014-01-01

    This paper presents a new approach to detect dopamine in nanomolar range using an electrochemical sensor utilizing a composite made of chitosan-stabilized silver nanoparticles and p-toluene sulfonic acid-doped ultrathin polypyrrole film. Studies included cyclic voltammogram, amperometry, differential pulse voltammetry and also investigation by electrochemical impedance spectroscopy. A detection limit of 0.58 nM was achieved in the linear range 1 x 10(-9) M to 1.2 x 10(-7) M. High sensitivity ...

  10. Fundamentals of electrochemical detection techniques for CE and MCE.

    Science.gov (United States)

    Kubán, Pavel; Hauser, Peter C

    2009-10-01

    The electroanalytical techniques of amperometry, conductometry and potentiometry match well with the instrumental simplicity of CE. Indeed, all three detection approaches have been reported for electrophoretic separations. However, the characteristics of the three methods are quite distinct and these are not related to the optical methods more commonly employed. A detailed discussion of the underlying principles of each is given. The issue of possible effects of the separation voltage on the electrochemical detection techniques is considered in depth, and approaches to the elimination of such interferences are also discussed for each case.

  11. Electrochemistry in hollow-channel paper analytical devices.

    Science.gov (United States)

    Renault, Christophe; Anderson, Morgan J; Crooks, Richard M

    2014-03-26

    In the present article we provide a detailed analysis of fundamental electrochemical processes in a new class of paper-based analytical devices (PADs) having hollow channels (HCs). Voltammetry and amperometry were applied under flow and no flow conditions yielding reproducible electrochemical signals that can be described by classical electrochemical theory as well as finite-element simulations. The results shown here provide new and quantitative insights into the flow within HC-PADs. The interesting new result is that despite their remarkable simplicity these HC-PADs exhibit electrochemical and hydrodynamic behavior similar to that of traditional microelectrochemical devices.

  12. A new approach of the understanding of sulfur dioxide reduction in non-aqueous solvent; Une nouvelle approche de la comprehension de la reduction du dioxyde de soufre en solvant non aqueux

    Energy Technology Data Exchange (ETDEWEB)

    Potteau, E; Levillain, E; Lelieur, J P [Laboratoire de Spectrochimie Infrarouge et Raman (LASIR, UPR 2631 CNRS) Haute Etudes Industrielles (HEI), 59 - Lille (France)

    1997-12-31

    The study of SO{sub 2} reduction in non-aqueous solvent can help to understand the functioning of Li/SO{sub 2} batteries and to find a simpler way for the synthesis of Li{sub 2}S{sub 2}O{sub 4} dithionite. This paper presents the results of electrochemical studies (cycle volt-amperometry in semi-infinite and thin film diffusion conditions, visible spectro-electrochemistry) and spectroscopic studies (UV, visible and RPE) performed on SO{sub 2} solutions. A mechanism of SO{sub 2} reduction is proposed and discussed. (J.S.) 18 refs.

  13. [Application of iodine metabolism analysis methods in thyroid diseases].

    Science.gov (United States)

    Han, Jian-hua; Qiu, Ling

    2013-08-01

    The main physiological role of iodine in the body is to synthesize thyroid hormone. Both iodine deficiency and iodine excess can lead to severe thyroid diseases. While its role in thyroid diseases has increasingly been recognized, few relevant platforms and techniques for iodine detection have been available in China. This paper summarizes the advantages and disadvantages of currently iodine detection methods including direct titration, arsenic cerium catalytic spectrophotometry, chromatography with pulsed amperometry, colorimetry based on automatic biochemistry, inductively coupled plasma mass spectrometry, so as to optimize the iodine nutrition for patients with thyroid diseases.

  14. Fabrication of an Amperometric Flow-Injection Microfluidic Biosensor Based on Laccase for In Situ Determination of Phenolic Compounds

    Directory of Open Access Journals (Sweden)

    Juan C. Gonzalez-Rivera

    2015-01-01

    Full Text Available We aim to develop an in situ microfluidic biosensor based on laccase from Trametes pubescens with flow-injection and amperometry as the transducer method. The enzyme was directly immobilized by potential step chronoamperometry, and the immobilization was studied using cyclic voltammetry and electrochemical impedance spectroscopy. The electrode response by amperometry was probed using ABTS and syringaldazine. A shift of interfacial electron transfer resistance and the electron transfer rate constant from 18.1 kΩ to 3.9 MΩ and 4.6 × 10−2 cm s−1 to 2.1 × 10−4 cm s−1, respectively, evidenced that laccase was immobilized on the electrode by the proposed method. We established the optimum operating conditions of temperature (55°C, pH (4.5, injection flow rate (200 µL min−1, and applied potential (0.4 V. Finally, the microfluidic biosensor showed better lower limit of detection (0.149 µM and sensitivity (0.2341 nA µM−1 for ABTS than previous laccase-based biosensors and the in situ operation capacity.

  15. Electrocatalytic Determination of Isoniazid by a Glassy Carbon Electrode Modified with Poly (Eriochrome Black T

    Directory of Open Access Journals (Sweden)

    Karim Asadpour-Zeynali

    2017-06-01

    Full Text Available In this work poly eriochrome black T (EBT was electrochemically synthesized on the glassy carbon electrode as electrode modifier. On the modified electrode, voltammetric behavior of isoniazid (INH was investigated. The poly (EBT-modified glassy carbon electrode has excellent electrocatalytic ability for the electrooxidation of isoniazid. This fact was appeared as a reduced overpotential of INH oxidation in a wide operational pH range from 2 to 13. It has been found that the catalytic peak current depends on the concentration of INH and solution pH. The number of electrons involved in the rate determining step was found 1. The diffusion coefficient of isoniazid was also estimated using chronoamperometry technique. The experimental results showed that the mediated oxidation peak current of isoniazid is linearly dependent on the concentration of isoniazid in the ranges of 8.0 × 10-6 – 1.18 × 10-3 M and 2.90 × 10-5 M – 1.67× 10-3 M with differential pulse voltammetry (DPV and amperometry methods, respectively. The detection limits (S/N = 3 were found to be 6.0 μM and 16.4 μM by DPV and amperometry methods, respectively. This developed method was applied to the determination of isoniazid in tablet samples with satisfactory results.

  16. Tin oxide quantum dots embedded iron oxide composite as efficient lead sensor

    Science.gov (United States)

    Dutta, Dipa; Bahadur, Dhirendra

    2018-04-01

    SnO2 quantum dots (QDs) embedded iron oxide (IO) nanocomposite is fabricated and explored as a capable sensor for lead detection. Square wave anodic stripping voltammetry (SWASV) and amperometry have been used to explore the proposed sensor's response towards lead detection. The modified electrode shows linear current response for concentration of lead ranging from 99 nM to 6.6 µM with limit of detection 0.42 µM (34 ppb). Amperometry shows a detection limit as low as 0.18 nM (0.015 ppb); which is far below the permissible limit of lead in drinking water by World Health Organization. This proposed sensor shows linear current response (R2 = 0.98) for the lead concentration ranging from 133 × 10-9 to 4.4 × 10-6M. It also exhibits rapid response time of 12 sec with an ultra high sensitivity of 5.5 µA/nM. These detection properties promise the use of SnO2 QDs -IO composite for detection of lead in environmental sample with great ease.

  17. Recent developments in cyanide detection: A review

    International Nuclear Information System (INIS)

    Ma Jian; Dasgupta, Purnendu K.

    2010-01-01

    The extreme toxicity of cyanide and environmental concerns from its continued industrial use continue to generate interest in facile and sensitive methods for cyanide detection. In recent years, there is also additional recognition of HCN toxicity from smoke inhalation and potential use of cyanide as a weapon of terrorism. This review summarizes the literature since 2005 on cyanide measurement in different matrices ranging from drinking water and wastewater, to cigarette smoke and exhaled breath to biological fluids like blood, urine and saliva. The dramatic increase in the number of publications on cyanide measurement is indicative of the great interest in this field not only from analytical chemists, but also researchers from diverse environmental, medical, forensic and clinical arena. The recent methods cover both established and emerging analytical disciplines and include naked eye visual detection, spectrophotometry/colorimetry, capillary electrophoresis with optical absorbance detection, fluorometry, chemiluminescence, near-infrared cavity ring down spectroscopy, atomic absorption spectrometry, electrochemical methods (potentiometry/amperometry/ion chromatography-pulsed amperometry), mass spectrometry (selected ion flow tube mass spectrometry, electrospray ionization mass spectrometry, gas chromatography-mass spectrometry), gas chromatography (nitrogen phosphorus detector, electron capture detector) and quartz crystal mass monitors.

  18. Recent developments in cyanide detection: A review

    Energy Technology Data Exchange (ETDEWEB)

    Ma Jian [Department of Chemistry and Biochemistry, University of Texas, 700 Planetarium Place, Arlington, TX 76019-0065 (United States); Dasgupta, Purnendu K., E-mail: Dasgupta@uta.edu [Department of Chemistry and Biochemistry, University of Texas, 700 Planetarium Place, Arlington, TX 76019-0065 (United States)

    2010-07-19

    The extreme toxicity of cyanide and environmental concerns from its continued industrial use continue to generate interest in facile and sensitive methods for cyanide detection. In recent years, there is also additional recognition of HCN toxicity from smoke inhalation and potential use of cyanide as a weapon of terrorism. This review summarizes the literature since 2005 on cyanide measurement in different matrices ranging from drinking water and wastewater, to cigarette smoke and exhaled breath to biological fluids like blood, urine and saliva. The dramatic increase in the number of publications on cyanide measurement is indicative of the great interest in this field not only from analytical chemists, but also researchers from diverse environmental, medical, forensic and clinical arena. The recent methods cover both established and emerging analytical disciplines and include naked eye visual detection, spectrophotometry/colorimetry, capillary electrophoresis with optical absorbance detection, fluorometry, chemiluminescence, near-infrared cavity ring down spectroscopy, atomic absorption spectrometry, electrochemical methods (potentiometry/amperometry/ion chromatography-pulsed amperometry), mass spectrometry (selected ion flow tube mass spectrometry, electrospray ionization mass spectrometry, gas chromatography-mass spectrometry), gas chromatography (nitrogen phosphorus detector, electron capture detector) and quartz crystal mass monitors.

  19. EDTA assisted synthesis of hydroxyapatite nanoparticles for electrochemical sensing of uric acid

    Energy Technology Data Exchange (ETDEWEB)

    Kanchana, P.; Sekar, C., E-mail: Sekar2025@gmail.com

    2014-09-01

    Hydroxyapatite nanoparticles have been synthesized using EDTA as organic modifier by a simple microwave irradiation method and its application for the selective determination of uric acid (UA) has been demonstrated. Electrochemical behavior of uric acid at HA nanoparticle modified glassy carbon electrode (E-HA/GCE) has been investigated by electrochemical impedance spectroscopy (EIS), cyclic voltammetry (CV), linear sweep voltammetry (LSV) and amperometry. The E-HA modified electrode exhibits efficient electrochemical activity towards uric acid sensing without requiring enzyme or electron mediator. Amperometry studies revealed that the fabricated electrode has excellent sensitivity for uric acid with the lowest detection limit of 142 nM over a wide concentration range from 1 × 10{sup −7} to 3 × 10{sup −5} M. Moreover, the studied E-HA modified GC electrode exhibits a good reproducibility and long-term stability and an admirable selectivity towards the determination of UA even in the presence of potential interferents. The analytical performance of this sensor was evaluated for the detection of uric acid in human urine and blood serum samples. - Highlights: • EDTA- hydroxyapatite (HA) nanoparticles have been synthesized by microwave irradiation method. • A novel amperometric Uric Acid biosensor has been fabricated using E-HA/GCE. • The fabricated sensor exhibits a wide linear range, good stability and high reproducibility. • The sensor was applied for the detection of UA in human blood serum and urine.

  20. EDTA assisted synthesis of hydroxyapatite nanoparticles for electrochemical sensing of uric acid

    International Nuclear Information System (INIS)

    Kanchana, P.; Sekar, C.

    2014-01-01

    Hydroxyapatite nanoparticles have been synthesized using EDTA as organic modifier by a simple microwave irradiation method and its application for the selective determination of uric acid (UA) has been demonstrated. Electrochemical behavior of uric acid at HA nanoparticle modified glassy carbon electrode (E-HA/GCE) has been investigated by electrochemical impedance spectroscopy (EIS), cyclic voltammetry (CV), linear sweep voltammetry (LSV) and amperometry. The E-HA modified electrode exhibits efficient electrochemical activity towards uric acid sensing without requiring enzyme or electron mediator. Amperometry studies revealed that the fabricated electrode has excellent sensitivity for uric acid with the lowest detection limit of 142 nM over a wide concentration range from 1 × 10 −7 to 3 × 10 −5 M. Moreover, the studied E-HA modified GC electrode exhibits a good reproducibility and long-term stability and an admirable selectivity towards the determination of UA even in the presence of potential interferents. The analytical performance of this sensor was evaluated for the detection of uric acid in human urine and blood serum samples. - Highlights: • EDTA- hydroxyapatite (HA) nanoparticles have been synthesized by microwave irradiation method. • A novel amperometric Uric Acid biosensor has been fabricated using E-HA/GCE. • The fabricated sensor exhibits a wide linear range, good stability and high reproducibility. • The sensor was applied for the detection of UA in human blood serum and urine

  1. EDTA assisted synthesis of hydroxyapatite nanoparticles for electrochemical sensing of uric acid.

    Science.gov (United States)

    Kanchana, P; Sekar, C

    2014-09-01

    Hydroxyapatite nanoparticles have been synthesized using EDTA as organic modifier by a simple microwave irradiation method and its application for the selective determination of uric acid (UA) has been demonstrated. Electrochemical behavior of uric acid at HA nanoparticle modified glassy carbon electrode (E-HA/GCE) has been investigated by electrochemical impedance spectroscopy (EIS), cyclic voltammetry (CV), linear sweep voltammetry (LSV) and amperometry. The E-HA modified electrode exhibits efficient electrochemical activity towards uric acid sensing without requiring enzyme or electron mediator. Amperometry studies revealed that the fabricated electrode has excellent sensitivity for uric acid with the lowest detection limit of 142 nM over a wide concentration range from 1 × 10(-7) to 3 × 10(-5)M. Moreover, the studied E-HA modified GC electrode exhibits a good reproducibility and long-term stability and an admirable selectivity towards the determination of UA even in the presence of potential interferents. The analytical performance of this sensor was evaluated for the detection of uric acid in human urine and blood serum samples. Copyright © 2014. Published by Elsevier B.V.

  2. Amperometric sensing of NADH and ethanol using a hybrid film electrode modified with electrochemically fabricated zirconia nanotubes and poly (acid fuchsin)

    International Nuclear Information System (INIS)

    Liu, X.; Li, B.; Zhan, G.; Liu, C.; Li, C.; Ma, M.

    2012-01-01

    We report on a glassy carbon electrode (GCE) modified with a film of chitosin containing acid fuchsin (AF) adsorbed onto zirconia nanotubes. The mixture was polymerized by cyclic voltammetric scannings in the potential range from - 0. 8 V to +1. 3 V in buffer solution to produce a hybrid film electrode (nano-ZrO 2 /PAF/GCE). The morphology of the hybrid film electrode surface was characterized by scanning electron microscopy. Its electrochemical properties were studied via electrochemical impedance spectroscopy. The electrochemical response of nicotinamide adenine dinucleotide (NADH) was investigated by differential pulse voltammetry and amperometry. The results indicated that the nano-ZrO 2 /PAF/GCE possesses well synergistic catalytic activity towards NADH. Compared to an unmodified GCE, the oxidation overpotential is negatively shifted by 224 mV, and the oxidation current is significantly increased. Under optimal conditions, the amperometric response is linearly proportional to the concentration of NADH in the 1. 0 - 100. 0 μM concentration range. Ethanol also can be determined by amperometry if alcohol dehydrogenase and NADH are added to the sample. Two linear relationships between current and alcohol concentration were obtained. They cover the range from 0. 03 to 1. 0 mM, and from 1. 0 to 12. 0 mM. (author)

  3. Recent developments in cyanide detection: A review

    Science.gov (United States)

    Ma, Jian; Dasgupta, Purnendu K.

    2010-01-01

    The extreme toxicity of cyanide and environmental concerns from its continued industrial use continue to generate interest in facile and sensitive methods for cyanide detection. In recent years there is also additional recognition of HCN toxicity from smoke inhalation and potential use of cyanide as a weapon of terrorism. This review summarizes the literature since 2005 on cyanide measurement in different matrices ranging from drinking water and wastewater, to cigarette smoke and exhaled breath to biological fluids like blood, urine and saliva. The dramatic increase in the number of publications on cyanide measurement is indicative of the great interest in this field not only from analytical chemists, but also researchers from diverse environmental, medical, forensic and clinical arena. The recent methods cover both established and emerging analytical disciplines and include naked eye visual detection, spectrophotometry/colorimetry, capillary electrophoresis with optical absorbance detection, fluorometry, chemiluminescence, near-infrared cavity ring down spectroscopy, atomic absorption spectrometry, electrochemical methods (potentiometry/amperometry/ion chromatography-pulsed amperometry), mass spectrometry (selected ion flow tube mass spectrometry, electrospray ionization mass spectrometry, gas chromatography-mass spectrometry), gas chromatography (nitrogen phosphorus detector, electron capture detector) and quartz crystal mass monitors. PMID:20599024

  4. Structure and electrochemical properties of copper wires with seamless 1D nanostructures

    Directory of Open Access Journals (Sweden)

    Yutong Wu

    2018-04-01

    Full Text Available A seamless Cu nanowire array grown on Cu wire is prepared by combining thermal oxidation method and electrochemical reduction. The data set described in this paper includes the structure of the Cu nanowires electrode, electrocatalytic active surface area, linear sweep voltammetry and amperometry measurement for nitrate sensing. The electrochemical data show that Cu nanowire arrays exhibited a linear response to nitrate ions over a concentration range from 50 μM to 600 μM (R2 = 0.9974 with a sensitivity of 0.357 μA μM−1 cm−1 and detection limit of 12.2 μM at a signal-to-noise ratio of 3, respectively.

  5. Stabilization of glucose-oxidase in the graphene paste for screen-printed glucose biosensor

    Science.gov (United States)

    Pepłowski, Andrzej; Janczak, Daniel; Jakubowska, Małgorzata

    2015-09-01

    Various methods and materials for enzyme stabilization within screen-printed graphene sensor were analyzed. Main goal was to develop technology allowing immediate printing of the biosensors in single printing process. Factors being considered were: toxicity of the materials used, ability of the material to be screen-printed (squeezed through the printing mesh) and temperatures required in the fabrication process. Performance of the examined sensors was measured using chemical amperometry method, then appropriate analysis of the measurements was conducted. The analysis results were then compared with the medical requirements. Parameters calculated were: correlation coefficient between concentration of the analyte and the measured electrical current (0.986) and variation coefficient for the particular concentrations of the analyte used as the calibration points. Variation of the measured values was significant only in ranges close to 0, decreasing for the concentrations of clinical importance. These outcomes justify further development of the graphene-based biosensors fabricated through printing techniques.

  6. Electrocatalytic oxidation of hydrazine at overoxidized polypyrrole film modified glassy carbon electrode

    Energy Technology Data Exchange (ETDEWEB)

    Majidi, Mir Reza [Department of Analytical Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz 51664 (Iran, Islamic Republic of); Jouyban, Abolghasem [Faculty of Pharmacy and Drug Applied Research Center, Tabriz University of Medical Sciences, Tabriz 51664 (Iran, Islamic Republic of); Asadpour-Zeynali, Karim [Department of Analytical Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz 51664 (Iran, Islamic Republic of)]. E-mail: asadpour@tabrizu.ac.ir

    2007-06-20

    Electrocatalytic oxidation of hydrazine (HZ) was studied on an overoxidized polypyrrole (OPPy) modified glassy carbon electrode using cyclic voltammetry and chronoamperometry techniques. The OPPy-modified glassy carbon electrode has very high catalytic ability for electrooxidation of HZ, which appeared as a reduced overpotential in a wide operational pH range of 5-10. The overall numbers of electrons involved in the catalytic oxidation of HZ, the number of electrons involved in the rate-determining and diffusion coefficient of HZ were estimated using cyclic voltammetry and chronoamperometry. It has been shown that using the OPPy-modified electrode, HZ can be determined by cyclic voltammetry and amperometry with limit of detection 36 and 3.7 {mu}M, respectively. The results of the analysis suggest that the proposed method promises accurate results and could be employed for the routine determination of HZ.

  7. Brain Tissue Oxygen: In Vivo Monitoring with Carbon Paste Electrodes

    Directory of Open Access Journals (Sweden)

    John P. Lowry

    2005-11-01

    Full Text Available In this communication we review selected experiments involving the use ofcarbon paste electrodes (CPEs to monitor and measure brain tissue O2 levels in awakefreely-moving animals. Simultaneous measurements of rCBF were performed using the H2clearance technique. Voltammetric techniques used include both differential pulse (O2 andconstant potential amperometry (rCBF. Mild hypoxia and hyperoxia produced rapidchanges (decrease and increase respectively in the in vivo O2 signal. Neuronal activation(tail pinch and stimulated grooming produced similar increases in both O2 and rCBFindicating that CPE O2 currents provide an index of increases in rCBF when such increasesexceed O2 utilization. Saline injection produced a transient increase in the O2 signal whilechloral hydrate produced slower more long-lasting changes that accompanied the behavioralchanges associated with anaesthesia. Acetazolamide increased O2 levels through an increasein rCBF.

  8. Multichannel Bipotentiostat Integrated With a Microfluidic Platform for Electrochemical Real-Time Monitoring of Cell Cultures

    DEFF Research Database (Denmark)

    Vergani, Marco; Carminati, Marco; Ferrari, Giorgio

    2012-01-01

    An electrochemical detection system specifically designed for multi-parameter real-time monitoring of stem cell culturing/differentiation in a microfluidic system is presented. It is composed of a very compact 24-channel electronic board, compatible with arrays of microelectrodes and coupled...... to a microfluidic cell culture system. A versatile data acquisition software enables performing amperometry, cyclic voltammetry and impedance spectroscopy in each of the 12 independent chambers over a 100 kHz bandwidth with current resolution down to 5 pA for 100 ms measuring time. The design of the platform, its...... realization and experimental characterization are reported, with emphasis on the analysis of impact of input capacitance (i.e., microelectrode size) and microfluidic pump operation on current noise. Programmable sequences of successive injections of analytes (ferricyanide and dopamine) and rinsing buffer...

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

    Science.gov (United States)

    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.

  10. Fast BIA-amperometric determination of isoniazid in tablets.

    Science.gov (United States)

    Quintino, Maria S M; Angnes, Lúcio

    2006-09-26

    This paper proposes a new, fast and precise method to analyze isoniazid based on the electrochemical oxidation of the analyte at a glassy carbon electrode in 0.1M NaOH. The quantification was performed utilizing amperometry associated with batch injection analysis (BIA) technique. Fast sequential analysis (60 determinations h(-1)) in an unusually wide linear dynamic range (from 2.5 x 10(-8) to 1.0 x 10(-3)M), with high sensitivity and low limits of detection (4.1 x 10(-9)M) and quantification (1.4 x 10(-8)M), was achieved. Such characteristics allied to a good repeatability of the current responses (relative standard deviation of 0.79% for 30 measurements), were explored for the specific determination of isoniazid in isoniazid-rifampin tablet.

  11. Electrocatalysis of the oxidations of some organic compounds on noble-metal electrodes by foreign-metal ad-atoms

    International Nuclear Information System (INIS)

    Tsang, R.W.

    1981-10-01

    Electrochemical oxidation of formic acid was studied on Pt electrodes in acid, and that of dextrose was studied on Pt and Au in alkali. Poisoning was observed on Pt but not on Au. Several heavy-metal ad-atoms (Pb, Bi, Tl) enhance greatly the anodic currents on Pt, while transition metals (Cu, Zn) inhibit the oxidation on Pt. The enhancement effect of the metal ad-atoms is correlated with electron structure. All metal ad-atoms showed an inhibitory effect on Au. Amperometry showed that Pt electrodes are completely deactivated within 10 s during dextrose oxidation without ad-atoms, while Au retains much of its activity even after 10 min. Ad-atoms maintains the Pt activity over much more than 10 s. 50 figures, 38 tables

  12. Electrochemical Analysis of Neurotransmitters

    Science.gov (United States)

    Bucher, Elizabeth S.; Wightman, R. Mark

    2015-07-01

    Chemical signaling through the release of neurotransmitters into the extracellular space is the primary means of communication between neurons. More than four decades ago, Ralph Adams and his colleagues realized the utility of electrochemical methods for the study of easily oxidizable neurotransmitters, such as dopamine, norepinephrine, and serotonin and their metabolites. Today, electrochemical techniques are frequently coupled to microelectrodes to enable spatially resolved recordings of rapid neurotransmitter dynamics in a variety of biological preparations spanning from single cells to the intact brain of behaving animals. In this review, we provide a basic overview of the principles underlying constant-potential amperometry and fast-scan cyclic voltammetry, the most commonly employed electrochemical techniques, and the general application of these methods to the study of neurotransmission. We thereafter discuss several recent developments in sensor design and experimental methodology that are challenging the current limitations defining the application of electrochemical methods to neurotransmitter measurements.

  13. Titanium electroplating of copper in molten salt media

    International Nuclear Information System (INIS)

    Renaud, Denis

    1985-01-01

    After a bibliographical survey on electroplating in molten salt media and on the electrolytic production of titanium, the author explains the reasons for the choice of the LiF-NaF-KF eutectic mix as solvent. He recalls the main properties which are used, and describes the conventional and convolutional processing of data obtained by linear volt-amperometry. He presents the electrolyte preparation mode which takes into account the existence of titanium ions with intermediate oxidation degree, and the reactivity of titanium with oxygenated species. Experimental results are discussed. Then, after the study of the mechanism of reduction of trivalent titanium into titanium on molybdenum (intermetallic diffusion is here negligible), he reports the study of this mechanism on copper (it is a more complicated situation, due to combinations between titanium and copper). The effect of different parameters (electrolyte purity, current density, electrode potential and temperature) is interpreted in order to identify optimal conditions for titanium electroplating of copper [fr

  14. Toxicity assessment using different bioassays and microbial biosensors.

    Science.gov (United States)

    Hassan, Sedky H A; Van Ginkel, Steven W; Hussein, Mohamed A M; Abskharon, Romany; Oh, Sang-Eun

    2016-01-01

    Toxicity assessment of water streams, wastewater, and contaminated sediments, is a very important part of environmental pollution monitoring. Evaluation of biological effects using a rapid, sensitive and cost effective method can indicate specific information on ecotoxicity assessment. Recently, different biological assays for toxicity assessment based on higher and lower organisms such as fish, invertebrates, plants and algal cells, and microbial bioassays have been used. This review focuses on microbial biosensors as an analytical device for environmental, food, and biomedical applications. Different techniques which are commonly used in microbial biosensing include amperometry, potentiometry, conductometry, voltammetry, microbial fuel cells, fluorescence, bioluminescence, and colorimetry. Examples of the use of different microbial biosensors in assessing a variety of environments are summarized. Copyright © 2016 Elsevier Ltd. All rights reserved.

  15. Hydrogen Monitoring in Nuclear Power Cycles

    International Nuclear Information System (INIS)

    Maurer, Heini; Staub, Lukas

    2012-09-01

    Maintaining constant Hydrogen levels in Nuclear power cycles is always associated with the challenge to determine the same reliably. Grab sample analysis is complicated and costly and online instruments currently known are difficult to maintain, verify and calibrate. Although amperometry has been proven to be the most suitable measuring principle for online instruments, it has never been thoroughly investigated what electrode materials would best perform in terms of measurement drift and regeneration requirements. This paper we will cover the findings of a research program, conducted at the R and D centre of Swan Analytische Instrumente AG in Hinwil Switzerland, aimed to find ideal electrode materials and sensor design to provide the nuclear industry with an enhanced method to determine dissolved hydrogen in nuclear power cycles. (authors)

  16. Characterization of poly(3,4-ethylenedioxythiophene):tosylate conductive polymer microelectrodes for transmitter detection

    DEFF Research Database (Denmark)

    Larsen, Simon T.; Vreeland, Richard F.; Heien, Michael L.

    2012-01-01

    applications such as capillary electrophoresis, high-performance liquid chromatography, and constant potential amperometry at living cells. Band electrodes with widths down to 3 μm were fabricated on polymer substrates using UV lithographic methods. The electrodes are electrochemically stable in a range......In this paper we investigate the physical and electrochemical properties of micropatterned poly(3,4-ethylenedioxythiophene):tosylate (PEDOT:tosylate) microelectrodes for neurochemical detection. PEDOT:tosylate is a promising conductive polymer electrode material for chip-based bioanalytical...... between −200 mV and 700 mV vs. Ag/AgCl and show a relatively low resistance. A wide range of transmitters is shown to oxidize readily on the electrodes. Kinetic rate constants and half wave potentials are reported. The capacitance per area was found to be high (1670 ± 130 μF cm−2) compared to other thin...

  17. Development of a Novel Cu(II Complex Modified Electrode and a Portable Electrochemical Analyzer for the Determination of Dissolved Oxygen (DO in Water

    Directory of Open Access Journals (Sweden)

    Salvatore Gianluca Leonardi

    2016-04-01

    Full Text Available The development of an electrochemical dissolved oxygen (DO sensor based on a novel Cu(II complex-modified screen printed carbon electrode is reported. The voltammetric behavior of the modified electrode was investigated at different scan rates and oxygen concentrations in PBS (pH = 7. An increase of cathodic current (at about −0.4 vs. Ag/AgCl with the addition of oxygen was observed. The modified Cu(II complex electrode was demonstrated for the determination of DO in water using chronoamperometry. A small size and low power consumption home-made portable electrochemical analyzer based on custom electronics for sensor interfacing and operating in voltammetry and amperometry modes has been also designed and fabricated. Its performances in the monitoring of DO in water were compared with a commercial one.

  18. A uric acid sensor based on electrodeposition of nickel hexacyanoferrate nanoparticles on an electrode modified with multi-walled carbon nanotubes

    International Nuclear Information System (INIS)

    Fang, B.; Feng, Y.; Wang, G.; Zhang, C.; Gu, A.; Liu, M.

    2011-01-01

    An electrode sensitive to uric acid was prepared by electrodeposition of nickel(II) hexacyanoferrate(III) on the surface of a glassy carbon electrode modified with multi-walled carbon nanotubes. The morphology of the material was characterized by scanning electron microscopy and Fourier transform infrared spectrometry. The modified electrode were characterized via cyclic voltammetry and amperometry (i - t). It exhibited efficient electron transfer ability and a strong and fast (< 3 s) response towards uric acid which is linear in the range from 0.1 μM to 18 μM, with a lower detection limit of 50 nM (at an S/N ratio of 3). In addition, the electrode exhibited good reproducibility and long-term stability. (author)

  19. Comparative study on the electrocatalytic activities of ordered mesoporous carbons and graphene

    International Nuclear Information System (INIS)

    Wang Huan; Qi Bin; Lu Baoping; Bo Xiangjie; Guo Liping

    2011-01-01

    In this work, a comparative study on the electrocatalytic activities of ordered mesoporous carbons (OMCs) and graphene (GR) is presented. Using voltammetry and amperometry as detection methods, four DNA bases, double-stranded DNA (dsDNA), six important electroactive compounds and various biomolecules were employed to investigate their electrochemical responses on OMC and GR modified glassy carbon electrodes (OMC/GCE and GR/GCE). The results show that OMC/GCE enhances the electron transfer kinetics of these compounds compared to GR/GCE. The discrepancy in electrochemical activities can be attributed to the different microstructures of OMC and GR, which were examined by transmission electron microscopy, X-ray photoelectron spectra, X-ray diffraction, Raman spectra and nitrogen adsorption-desorption.

  20. Corrosion in the presence of a complexing agent - application to the continuous determination of hydrofluoric acid in the atmosphere

    International Nuclear Information System (INIS)

    Chapron, J.

    1966-10-01

    After a presentation of the thermodynamics and kinetics involved during corrosion in the presence of a complexing agent, the first part of this report deals with the electrochemical properties of an aluminium electrode in the presence of fluoride solutions. Various physical and chemical parameters have been studied together with their influence on the aforementioned properties. From this first part are deduced the medium and the various parameters which lead to the maximum efficiency for the detection of fluorides by amperometry. The second part is an application of the results of the above work, which has made it possible to develop a cell having an original design. Its performances are described. They show that the cell has a greater sensitivity and a shorter response time than existing equipment. (author) [fr

  1. Mesoporous silica (MCM-41)-Fe2O3 as a novel magnetic nanosensor for determination of trace amounts of amino acids.

    Science.gov (United States)

    Hasanzadeh, Mohammad; Shadjou, Nasrin; Omidinia, Eskandar

    2013-08-01

    Magnetic (Fe2O3) mobile crystalline material-41 (MCM-41) was prepared and characterized using transmission electron microscopy (TEM) and nitrogen adsorption-desorption techniques. Due to the large surface area (1213 m(2)g(-1)) and remarkable electrocatalytic properties of MCM-41-Fe2O3, the MCM-41-Fe2O3 modified glassy carbon electrode (MCM-41-Fe2O3/GCE) exhibits potent electrocatalytic activity toward the electro-oxidation of amino acids. MCM-41-Fe2O3/GCE brings new capabilities for electrochemical sensing by combining the advantages of Fe2O3 magnetic nanoparticles and MCM-41 with very large surface area. Cyclic voltammetry, hydrodynamic amperometry and flow injection analysis used to determination of amino acids at higher concentration range. Fast response time, excellent catalytic activity, and ease of preparation are the advantages of the proposed amino acid sensor. Copyright © 2013 Elsevier B.V. All rights reserved.

  2. Simple electrochemical sensor for caffeine based on carbon and Nafion-modified carbon electrodes.

    Science.gov (United States)

    Torres, A Carolina; Barsan, Madalina M; Brett, Christopher M A

    2014-04-15

    A simple, economic, highly sensitive and highly selective method for the detection of caffeine has been developed at bare and Nafion-modified glassy carbon electrodes (GCE). The electrochemical behaviour of caffeine was examined in electrolyte solutions of phosphate buffer saline, sodium perchlorate, and in choline chloride plus oxalic acid, using analytical determinations by fixed potential amperometry, phosphate buffer saline being the best. Modifications of the GCE surface with poly(3,4-ethylenedioxythiophene) (PEDOT), Nafion, and multi-walled carbon nanotubes were tested in order to evaluate possible sensor performance enhancements, Nafion giving the most satisfactory results. The effect of interfering compounds usually found in samples containing caffeine was examined at GCE without and with Nafion coating, to exclude interferences, and the sensors were successfully applied to determine the caffeine content in commercial beverages and drugs. Copyright © 2013 Elsevier Ltd. All rights reserved.

  3. Nonenzymetic glucose sensing using carbon functionalized carbon doped ZnO nanorod arrays

    Science.gov (United States)

    Chakraborty, Pinak; Majumder, Tanmoy; Dhar, Saurab; Mondal, Suvra Prakash

    2018-04-01

    Fabrication of highly sensitive, long stability and low cost glucose sensors are attractive for biomedical applications and food industries. Most of the commercial glucose sensors are based on enzymatic detection which suffers from problems underlying in enzyme activities. Development of high sensitive, enzyme free sensors is a great challenge for next generation glucose sensing applications. In our study Zinc oxide nanorod sensing electrodes have been grown using low cost hydrothermal route and their nonenzymatic glucose sensing properties have been demonstrated with carbon functionalized, carbon doped ZnO nanorods (C-ZnO NRs) in neutral medium (0.1M PBS, pH 7.4) using cyclic voltammetry and amperometry measurements. The C-ZnO NRs electrodes demonstrated glucose sensitivity˜ 13.66 µAmM-1cm-2 in the concentration range 0.7 - 14 mM.

  4. Nanoscale film formation of ferritin and its application to biomemory device

    International Nuclear Information System (INIS)

    Kim, Sang-Uk; Lee, Taek; Lee, Jin-Ho; Yagati, Ajay Kumar; Min, Junhong; Choi, Jeong-Woo

    2009-01-01

    A redox protein, ferritin is used as a functional constituent of the developed biomemory device. The concept of molecular device mainly depends on the solidification of biomolecules of interest and on the realization of properties of molecule immobilized on a selected substrate. Here, we immobilized the biomolecule, ferritin protein on gold substrate using an organic linker 11-mercaptoundecanoic acid (11-MUA). The immobilization of the protein on the gold substrate was confirmed by surface plasmon spectroscopy, Raman spectroscopy, and atomic force microscopy (AFM). The basic two memory functions, reading and writing of the developed biomemory device, were investigated by open-circuit potential amperometry (OCPA) using the redox property of the biomolecule of interest. The surface topography investigation by scanning tunneling microscopy (STM) shows that the robustness of the ferritin-based biomemory device was validated by the repeated electrochemical performance. These results show the developed biomemory device as a step towards the protein-based nanobiochip.

  5. Electroreduction of CO{sub 2} using copper-deposited on boron-doped diamond (BDD)

    Energy Technology Data Exchange (ETDEWEB)

    Panglipur, Hanum Sekar; Ivandini, Tribidasari A., E-mail: ivandini.tri@sci.ui.ac.id [Department of Chemistry, FMIPA, Universitas Indonesia, Kampus UI Depok (Indonesia); Einaga, Yasuaki [Department of Chemistry, Keio University (Japan); Wibowo, Rahmat

    2016-04-19

    Electroreduction of CO{sub 2} was studied at copper-modified boron-doped diamond (Cu-BDD) electrodes as the working electrode. The Cu-BDD electrodes were prepared by electrochemical reduction with various concentrations of CuSO{sub 4} solutions. FE-SEM was utilized to characterize the electrodes. At Cu-BDD electrodes, a reduction peak at around -1.2 V (vs Ag/AgCl) attributtable to CO{sub 2} reductions could be observed by cyclic voltammetry technique of CO{sub 2} bubbled in water containing 0.1M NaCl. Accordingly, electroreduction of CO{sub 2} was conducted at -1.2 V (vs Ag/AgCl) using amperometry technique. The chemical products of the electroreduction analyzed by using HPLC showed the formation of formaldehyde, formic acid, and acetic acid at Cu-BDD electrodes.

  6. Spectrophotometric and electrochemical studies of the interaction of cryptand 222 with DDQ and I2 in ethanol solution

    Directory of Open Access Journals (Sweden)

    Abolfazl Semnani

    2006-12-01

    Full Text Available Spectrophotometric and electrochemical studies concerning the interaction of cryptand 222 with DDQ and I2 have been performed in ethanol solution. In the case of DDQ, the results are indicative of the formation of C222¬+ and DDQ- through an equilibrium reaction. The results of I2 indicate the formation of I2-ethanol complex and I3- in the absence of C222. In the presence of C222, the formation of C222I¬+ and I3- through a non-equilibrium reaction is confirmed. The equilibrium constant of the redox reaction between DDQ and C222 has been calculated from the absorbance mole ratio data, using the nonlinear least square program “KINFIT”. The electrochemical reversibility of I-/I2 couple and irreversibility of DDQ/DDQ- is indicated by amperometry. The behavior of DDQ and I2 has been compared. A comparison with aprotic solvents has also been made.

  7. Forecasting approach of electrochemical valorisation of CO2 in alkali molten carbonates

    International Nuclear Information System (INIS)

    Chery, Deborah

    2015-01-01

    Carbon Dioxide is a greenhouse which can be valorised by means of electrochemical valorisation into carbon monoxide. The main goals of the thesis consist in the theoretical determination of the conductive conditions leading to this electrochemical valorisation in alkali molten carbonates along with the study of the feasibility of this electrochemical reduction in binary and ternary eutectics under experimental condition. CO 2 solubility has been determined by manometric measure and increase along with the temperature. CO 2 electrochemical experimental feasibility into CO in eutectics on gold plate electrode and graphite carbon has been proved by cyclic volt-amperometry for temperatures exceeding 550 C, without gold plate electrode pretreatment and with gold plate pretreatment by an pre-electrolysis at potential slightly negative as the CO 2 reduction potential. A global approach of reactional mechanisms implied in CO 2 reduction is proposed. (author)

  8. Nano-scale islands of ruthenium oxide as an electrochemical sensor for iodate and periodate determination

    International Nuclear Information System (INIS)

    Chatraei, Fatemeh; Zare, Hamid R.

    2013-01-01

    In this study, a promising electrochemical sensor was fabricated by the electrodeposition of nano-scale islands of ruthenium oxide (ruthenium oxide nanoparticles, RuON) on a glassy carbon electrode (RuON–GCE). Then, the electrocatalytic oxidation of iodate and periodate was investigated on it, using cyclic voltammetry, chronoamperometry and amperometry as diagnostic techniques. The charge transfer coefficient, α, and the charge transfer rate constant, k s , for electron transfer between RuON and GCE were calculated as 0.5 ± 0.03 and 9.0 ± 0.7 s −1 respectively. A comparison of the data obtained from the electrocatalytic reduction of iodate and periodate at a bare GCE (BGCE) and RuON–GCE clearly shows that the unique electronic properties of nanoparticles definitely improve the characteristics of iodate and periodate electrocatalytic reduction. The kinetic parameters such as the electron transfer coefficient, α, and the heterogeneous electron transfer rate constant, k′, for the reduction of iodate and periodate at RuON–GCE surface were determined using cyclic voltammetry. Amperometry revealed a good linear relationship between the peak current and the concentration of iodate and periodate. The detection limits of 0.9 and 0.2 μM were calculated for iodate and periodate respectively. Highlights: ► Ruthenium oxide nanoparticles, RuON, were used for electrocatalytic reduction iodate and periodate. ► Formal potential, E 0 ′, of the surface redox couple of RuON is pH-dependent. ► The heterogeneous electron transfer rate constant values between both analytes and RuON were calculated.

  9. Sensitive and selective determination of gallic acid in green tea samples based on an electrochemical platform of poly(melamine) film

    Energy Technology Data Exchange (ETDEWEB)

    Su, Ya-Ling; Cheng, Shu-Hua, E-mail: shcheng@ncnu.edu.tw

    2015-12-11

    In this work, an electrochemical sensor coupled with an effective flow-injection amperometry (FIA) system is developed, targeting the determination of gallic acid (GA) in a mild neutral condition, in contrast to the existing electrochemical methods. The sensor is based on a thin electroactive poly(melamine) film immobilized on a pre-anodized screen-printed carbon electrode (SPCE*/PME). The characteristics of the sensing surface are well-characterized by field emission scanning electron microscopy (FE-SEM), X-ray photoelectron spectroscopy (XPS) and surface water contact angle experiments. The proposed assay exhibits a wide linear response to GA in both pH 3 and pH 7.0 phosphate buffer solutions (PBS) under the optimized flow-injection amperometry. The detection limit (S/N = 3) is 0.076 μM and 0.21 μM in the pH 3 and pH 7 solutions, respectively. A relative standard deviation (RSD) of 3.9% is obtained for 57 successive measurements of 50 μM GA in pH 7 solutions. Interference studies indicate that some inorganic salts, catechol, caffeine and ascorbic acid do not interfere with the GA assay. The interference effects from some orthodiphenolic compounds are also investigated. The proposed method and a conventional Folin–Ciocalteu method are applied to detect GA in green tea samples using the standard addition method, and satisfactory spiked recoveries are obtained. - Highlights: • A nitrogen-rich conducting polymer was used for electroanalysis of gallic acid. • The sensor exhibits excellent electrochemical activity in both acidic and neutral media. • Good analytical results in terms of low detection limit and wide linear range are obtained. • The flow-injection amperometric assay is highly stable for continuous 57 replicates measurement (RSD = 3.9%). • The assay shows good recovery for green tea samples.

  10. An electrochemical methanol sensor based on a Pd-Ni/SiNWs catalytic electrode

    International Nuclear Information System (INIS)

    Tao Bairui; Zhang Jian; Hui Shichao; Chen Xuejiao; Wan Lijuan

    2010-01-01

    A novel electrochemical methanol sensor based on a catalytic electrode of palladium-nickel/silicon nanowires (Pd-Ni/SiNWs) is presented in this paper. Scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), and electrochemical methods are employed to investigate the Pd-Ni/SiNWs electrode materials. These nanocomposite materials exhibit a highly ordered, wire-like structure with a wire length of ∼50 μm and a wire diameter ranging from 100 to 300 nm. The substrate has good electrocatalytic activity towards the oxidation of methanol in alkaline solutions. The performances of the prototype sensor are characterized by cyclic voltammetry and fixed potential amperometry techniques. In a 1 mol L -1 KOH solution containing different methanol concentrations, the sensor exhibits a good sensitivity of 1.96 mA mmol -1 L cm -2 with R 2 = 0.99 and the corresponding detection limit of 18 μmol L -1 (signal-to-noise ratio = 3, S/N = 3) for cyclic voltammetry. Meanwhile, the electrode also displays a sensitivity of 0.48 mA mmol -1 L cm -2 with R 2 = 0.98 and the corresponding detection limit of 25 μmol L -1 (S/N = 3) for a fixed potential amperometry at -0.3 V versus an Ag/AgCl reference electrode. The results demonstrate that the Pd-Ni/SiNWs catalytic electrode has potential as an efficient and integrated sensor for methanol detection.

  11. Sensitive and selective determination of gallic acid in green tea samples based on an electrochemical platform of poly(melamine) film

    International Nuclear Information System (INIS)

    Su, Ya-Ling; Cheng, Shu-Hua

    2015-01-01

    In this work, an electrochemical sensor coupled with an effective flow-injection amperometry (FIA) system is developed, targeting the determination of gallic acid (GA) in a mild neutral condition, in contrast to the existing electrochemical methods. The sensor is based on a thin electroactive poly(melamine) film immobilized on a pre-anodized screen-printed carbon electrode (SPCE*/PME). The characteristics of the sensing surface are well-characterized by field emission scanning electron microscopy (FE-SEM), X-ray photoelectron spectroscopy (XPS) and surface water contact angle experiments. The proposed assay exhibits a wide linear response to GA in both pH 3 and pH 7.0 phosphate buffer solutions (PBS) under the optimized flow-injection amperometry. The detection limit (S/N = 3) is 0.076 μM and 0.21 μM in the pH 3 and pH 7 solutions, respectively. A relative standard deviation (RSD) of 3.9% is obtained for 57 successive measurements of 50 μM GA in pH 7 solutions. Interference studies indicate that some inorganic salts, catechol, caffeine and ascorbic acid do not interfere with the GA assay. The interference effects from some orthodiphenolic compounds are also investigated. The proposed method and a conventional Folin–Ciocalteu method are applied to detect GA in green tea samples using the standard addition method, and satisfactory spiked recoveries are obtained. - Highlights: • A nitrogen-rich conducting polymer was used for electroanalysis of gallic acid. • The sensor exhibits excellent electrochemical activity in both acidic and neutral media. • Good analytical results in terms of low detection limit and wide linear range are obtained. • The flow-injection amperometric assay is highly stable for continuous 57 replicates measurement (RSD = 3.9%). • The assay shows good recovery for green tea samples.

  12. A preparation of homogeneous distribution of palladium nanoparticle on poly (acrylic acid)-functionalized graphene oxide modified electrode for formalin oxidation

    International Nuclear Information System (INIS)

    Kongkaew, Supatinee; Kanatharana, Proespichaya; Thavarungkul, Panote; Limbut, Warakorn

    2017-01-01

    An excellent electrocatalytic activity, repeatability and stability of electrochemical sensor for formalin detection was fabricated based on a homogeneous distribution of ellipsoidal palladium nanoparticle (PdNPs) on poly (acrylic acid)-functionalized graphene oxide (PAA-GO) modified on a glassy carbon electrode (GCE) (PdNPs-PAA-GO/GCE) with incorporated flow injection amperometry (FI-Amp). Homogeneous distribution of ellipsoidal palladium nanoparticles (PdNPs) were dispersed on PAA-GO via an electroless deposition method. The surface morphology and electrochemical behavior of the PdNPs-PAA-GO/GCE were characterized by transmission electron microscopy, fourier transform infrared spectroscopy, cyclic voltammetry and amperometry. The PdNPs-PAA-GO/GCE exhibited excellent electrocatalytic activity toward formalin oxidation. Then this modified electrode was incorporated with FI-Amp for formalin sensor development. In order to obtain good analytical performances, many parameters such as the amount of PdNPs-PAA-GO, applied potential, flow rate and sample volume were optimized. Under optimal conditions, this sensor provided a wide linear range, 50-50,000 μmol L −1 , with high sensitivity (320 μA mmol L −1 cm −2 ). The limit of detection and limit of quantitation were 16 μmol L −1 and 53 μmol L −1 , respectively. This proposed sensor exhibited good repeatability (RSD < 3.5%), excellence stability (RSD = 1.5%, n = 500) and high sample throughput (60 samples h −1 ). This method was applied to the determination of formalin in soaked fresh food samples with satisfactory recovery.

  13. Corrosion of construction steel in pore simulated solution

    International Nuclear Information System (INIS)

    Valdes, Matias; Vasquez, Marcela

    2004-01-01

    The corrosion of steel for reinforcing reinforced cement structures is a common problem particularly in structures that are exposed to a marine environment. Loosened masonry originating by the diametrical stress that iron oxides place on the cement is not unusual. These situations involve risk to people and goods and make it necessary to repair the structure to prolong its useful service life. Some preliminary results are presented from the reproduction of the corrosive process with the use of a solution that simulates the chemical surroundings in the concrete pores. These results will help to evaluate the incidence of contaminants (CO 2 , chloride ions), inhibitors and coatings, among others, in the following stages by conveniently adjusting the solution's composition. The composition of the chosen solution is: 0.01 mol NaOH - 0.002 mol/l Ca(OH) 2 . The effect was evaluated of a passive film generated on the surface of the steel of the reinforcements at 100 mV for 14 minutes and for 12 hours. This potential corresponds to the passive region, as determined by recording tests with cyclic volt amperometry and in accordance with the Pourbaix diagram for steel. The corrosion current was defined by recording the resistance to polarization using different electrochemical methods: potential sweep, potentiostatic jump and sweep electrochemical impedance. The results show that neither of the two times selected are enough to generate the metal's passive state and that the potential of 100 mV used to generate the passive film may be too low to produce a compact and long lasting layer, considering that the passive zone interval comes to 700 mV, according to the volt amperometry readings (CW)

  14. Corrosion in the presence of a complexing agent - application to the continuous determination of hydrofluoric acid in the atmosphere; Corrosion en presence de complexant. - Application a la determination en continu de l'acide fluorhydrique dans l'atmosphere

    Energy Technology Data Exchange (ETDEWEB)

    Chapron, J [Commissariat a l' Energie Atomique, Centre d' Etudes Nucleaires de Fontenay-aux-Roses, 92 (France)

    1966-10-01

    After a presentation of the thermodynamics and kinetics involved during corrosion in the presence of a complexing agent, the first part of this report deals with the electrochemical properties of an aluminium electrode in the presence of fluoride solutions. Various physical and chemical parameters have been studied together with their influence on the aforementioned properties. From this first part are deduced the medium and the various parameters which lead to the maximum efficiency for the detection of fluorides by amperometry. The second part is an application of the results of the above work, which has made it possible to develop a cell having an original design. Its performances are described. They show that the cell has a greater sensitivity and a shorter response time than existing equipment. (author) [French] Apres un rappel sur la thermodynamique et la cinetique de la corrosion en presence de complexant, la premiere partie du memoire est consacree a l'etude des proprietes electrochimiques de l'electrode d'aluminium, en presence de solutions de fluorure. Differents parametres physiques et chimiques ont ete etudies ainsi que leurs influences sur les dites proprietes. De cette premiere partie on en a deduit le milieu et les divers parametres a fixer de facon a obtenir un rendement optimum au vue de la detection des fluorures par amperometrie. La deuxieme partie, qui est l'application des renseignements tires du travail deja cite, a permis de mettre au point une cellule de conception nouvelle. Ses performances sont decrites. Elles indiquent une sensibilite plus grande, un temps de reponse plus court que les appareils existants. (auteur)

  15. Corrosion in the presence of a complexing agent - application to the continuous determination of hydrofluoric acid in the atmosphere; Corrosion en presence de complexant. - Application a la determination en continu de l'acide fluorhydrique dans l'atmosphere

    Energy Technology Data Exchange (ETDEWEB)

    Chapron, J. [Commissariat a l' Energie Atomique, Centre d' Etudes Nucleaires de Fontenay-aux-Roses, 92 (France)

    1966-10-01

    After a presentation of the thermodynamics and kinetics involved during corrosion in the presence of a complexing agent, the first part of this report deals with the electrochemical properties of an aluminium electrode in the presence of fluoride solutions. Various physical and chemical parameters have been studied together with their influence on the aforementioned properties. From this first part are deduced the medium and the various parameters which lead to the maximum efficiency for the detection of fluorides by amperometry. The second part is an application of the results of the above work, which has made it possible to develop a cell having an original design. Its performances are described. They show that the cell has a greater sensitivity and a shorter response time than existing equipment. (author) [French] Apres un rappel sur la thermodynamique et la cinetique de la corrosion en presence de complexant, la premiere partie du memoire est consacree a l'etude des proprietes electrochimiques de l'electrode d'aluminium, en presence de solutions de fluorure. Differents parametres physiques et chimiques ont ete etudies ainsi que leurs influences sur les dites proprietes. De cette premiere partie on en a deduit le milieu et les divers parametres a fixer de facon a obtenir un rendement optimum au vue de la detection des fluorures par amperometrie. La deuxieme partie, qui est l'application des renseignements tires du travail deja cite, a permis de mettre au point une cellule de conception nouvelle. Ses performances sont decrites. Elles indiquent une sensibilite plus grande, un temps de reponse plus court que les appareils existants. (auteur)

  16. D-Amino acid oxidase bio-functionalized platforms: Toward an enhanced enzymatic bio-activity

    Science.gov (United States)

    Herrera, Elisa; Valdez Taubas, Javier; Giacomelli, Carla E.

    2015-11-01

    The purpose of this work is to study the adsorption process and surface bio-activity of His-tagged D-amino acid oxidase (DAAO) from Rhodotorula gracilis (His6-RgDAAO) as the first step for the development of an electrochemical bio-functionalized platform. With such a purpose this work comprises: (a) the His6-RgDAAO bio-activity in solution determined by amperometry, (b) the adsorption mechanism of His6-RgDAAO on bare gold and carboxylated modified substrates in the absence (substrate/COO-) and presence of Ni(II) (substrate/COO- + Ni(II)) determined by reflectometry, and (c) the bio-activity of the His6-RgDAAO bio-functionalized platforms determined by amperometry. Comparing the adsorption behavior and bio-activity of His6-RgDAAO on these different solid substrates allows understanding the contribution of the diverse interactions responsible for the platform performance. His6-RgDAAO enzymatic performance in solution is highly improved when compared to the previously used pig kidney (pk) DAAO. His6-RgDAAO exhibits an amperometrically detectable bio-activity at concentrations as low as those expected on a bio-functional platform; hence, it is a viable bio-recognition element of D-amino acids to be coupled to electrochemical platforms. Moreover, His6-RgDAAO bio-functionalized platforms exhibit a higher surface activity than pkDAAO physically adsorbed on gold. The platform built on Ni(II) modified substrates present enhanced bio-activity because the surface complexes histidine-Ni(II) provide with site-oriented, native-like enzymes. The adsorption mechanism responsible of the excellent performance of the bio-functionalized platform takes place in two steps involving electrostatic and bio-affinity interactions whose prevalence depends on the degree of surface coverage.

  17. Layer-by-layer self-assembling copper tetrasulfonated phthalocyanine on carbon nanotube modified glassy carbon electrode for electro-oxidation of 2-mercaptoethanol

    International Nuclear Information System (INIS)

    Shaik, Mahabul; Rao, V.K.; Gupta, Manish; Pandey, P.

    2012-01-01

    This paper describes the electrocatalytic activity of layer-by-layer self-assembled copper tetrasulfonated phthalocyanine (CuPcTS) on carbon nanotube (CNT)-modified glassy carbon (GC) electrode. CuPcTS is immobilized on the negatively charged CNT surface by alternatively assembling a cationic poly(diallyldimethylammonium chloride) (PDDA) layer and a CuPcTS layer. UV–vis absorption spectra and electrochemical measurements suggested the successive linear depositions of the bilayers of CuPcTs and PDDA on CNT. The surface morphology was observed using scanning electron microscopy. The viability of this CuPcTS/PDDA/CNT modified GC electrode as a redox mediator for the anodic oxidation and sensitive amperometric determination of 2-mercaptoethanol (2-ME) in alkaline conditions is described. The effect of number of bilayers of CuPcTS/PDDA and pH on electrochemical oxidation of 2-ME was studied. The proposed electrochemical sensor displayed excellent characteristics towards the determination of 2-ME in 0.1 M NaOH; such as low overpotentials (− 0.15 V vs Ag/AgCl), linear concentration range of 3 × 10 −5 M to 6 × 10 −3 M, and with a detection limit of 2.5 × 10 −5 M using simple amperometry. - Highlights: ► Carbon nanotubes (CNT) were drop-dried on glassy carbon electrode (GCE). ► Copper tetrasulfonated phthalocyanine (CuPcTS) was deposited on CNT/GCE. ► Layer-by-layer self-assembling method is used for depositing CuPcTS. ► Electrocatalytic oxidation of 2-mercaptoethanol (ME) was studied at this electrode ► The detection limit of ME at modified electrode was 25 μM by amperometry.

  18. Norepinephrine-modified glassy carbon electrode for the simultaneous determination of ascorbic acid and uric acid

    International Nuclear Information System (INIS)

    Zare, H.R.; Memarzadeh, F.; Ardakani, M. Mazloum; Namazian, M.; Golabi, S.M.

    2005-01-01

    The oxidation of norepinephrine (NE) on a preactivated glassy carbon electrode leads to the formation of a deposited layer of about 4.2 x 10 -10 mol cm -2 at the surface of the electrode. The electron transfer rate constant, k s , and charge transfer coefficient, α, for electron transfer between the electrode and immobilized NE film were calculated as 44 s -1 and 0.46, respectively. The NE-modified glassy carbon electrode exhibited good electrocatalytic properties towards ascorbic acid (AA) oxidation in phosphate buffer (pH 7.0) with an overpotential of about 475 mV lower than that of the bare electrode. The electrocatalytic response was evaluated by cyclic voltammetry, chronoamperometry, amperometry and rotating disk voltammetry. The overall number of electrons involved in the catalytic oxidation of AA and the number of electrons involved in the rate-determining step are 2 and 1, respectively. The rate constant for the catalytic oxidation of AA was evaluated by RDE voltammetry and an average value of k h was found to be 8.42 x 10 3 M -1 s -1 . Amperometric determination of AA in stirred solution exhibits a linear range of 2.0-1300.0 μM (correlation coefficient 0.9999) and a detection limit of 0.076 μM. The precision of amperometry was found to be 1.9% for replicate determination of a 49.0 μM solution of AA (n = 6). In differential pulse voltammetric measurements, the NE-modified glassy carbon electrode can separate the AA and uric acid (UA) signals. Ascorbic acid oxidizes at more negative potential than UA. Also, the simultaneous determination of UA and AA is achieved at the NE-modified electrode

  19. Sensitive and selective determination of gallic acid in green tea samples based on an electrochemical platform of poly(melamine) film.

    Science.gov (United States)

    Su, Ya-Ling; Cheng, Shu-Hua

    2015-12-11

    In this work, an electrochemical sensor coupled with an effective flow-injection amperometry (FIA) system is developed, targeting the determination of gallic acid (GA) in a mild neutral condition, in contrast to the existing electrochemical methods. The sensor is based on a thin electroactive poly(melamine) film immobilized on a pre-anodized screen-printed carbon electrode (SPCE*/PME). The characteristics of the sensing surface are well-characterized by field emission scanning electron microscopy (FE-SEM), X-ray photoelectron spectroscopy (XPS) and surface water contact angle experiments. The proposed assay exhibits a wide linear response to GA in both pH 3 and pH 7.0 phosphate buffer solutions (PBS) under the optimized flow-injection amperometry. The detection limit (S/N = 3) is 0.076 μM and 0.21 μM in the pH 3 and pH 7 solutions, respectively. A relative standard deviation (RSD) of 3.9% is obtained for 57 successive measurements of 50 μM GA in pH 7 solutions. Interference studies indicate that some inorganic salts, catechol, caffeine and ascorbic acid do not interfere with the GA assay. The interference effects from some orthodiphenolic compounds are also investigated. The proposed method and a conventional Folin-Ciocalteu method are applied to detect GA in green tea samples using the standard addition method, and satisfactory spiked recoveries are obtained. Copyright © 2015 Elsevier B.V. All rights reserved.

  20. Facile hydrothermal growth graphene/ZnO nanocomposite for development of enhanced biosensor.

    Science.gov (United States)

    Low, Sze Shin; Tan, Michelle T T; Loh, Hwei-San; Khiew, Poi Sim; Chiu, Wee Siong

    2016-01-15

    Graphene/zinc oxide nanocomposite was synthesised via a facile, green and efficient approach consisted of novel liquid phase exfoliation and solvothermal growth for sensing application. Highly pristine graphene was synthesised through mild sonication treatment of graphite in a mixture of ethanol and water at an optimum ratio. The X-ray diffractometry (XRD) affirmed the hydrothermal growth of pure zinc oxide nanoparticles from zinc nitrate hexahydrate precursor. The as-prepared graphene/zinc oxide (G/ZnO) nanocomposite was characterised comprehensively to evaluate its morphology, crystallinity, composition and purity. All results clearly indicate that zinc oxide particles were homogenously distributed on graphene sheets, without any severe aggregation. The electrochemical performance of graphene/zinc oxide nanocomposite-modified screen-printed carbon electrode (SPCE) was evaluated using cyclic voltammetry (CV) and amperometry analysis. The resulting electrode exhibited excellent electrocatalytic activity towards the reduction of hydrogen peroxide (H2O2) in a linear range of 1-15 mM with a correlation coefficient of 0.9977. The sensitivity of the graphene/zinc oxide nanocomposite-modified hydrogen peroxide sensor was 3.2580 μAmM(-1) with a limit of detection of 7.4357 μM. An electrochemical DNA sensor platform was then fabricated for the detection of Avian Influenza H5 gene based on graphene/zinc oxide nanocomposite. The results obtained from amperometry study indicate that the graphene/zinc oxide nanocomposite-enhanced electrochemical DNA biosensor is significantly more sensitive (P < 0.05) and efficient than the conventional agarose gel electrophoresis. Copyright © 2015 Elsevier B.V. All rights reserved.

  1. Mechanism of nitric acid reduction and kinetic modelling

    International Nuclear Information System (INIS)

    Sicsic, David; Balbaud-Celerier, Fanny; Tribollet, Bernard

    2014-01-01

    In France, the recycling of nuclear waste fuels involves the use of hot concentrated nitric acid. The understanding and prediction of the behaviour of the structural materials (mainly austenitic stainless steels) requires the determination and modelling of the nitric acid reduction process. Nitric acid is indirectly reduced by an autocatalytic mechanism depending on the cathodic overpotential and acid concentration. This mechanism has been widely studied. All the authors agree on its autocatalytic nature, characterized by the predominant role of the reduction products. It is also generally admitted that neither nitric acid nor the nitrate ion is the electro-active species. However, the nature of the electro-active species, the place where the catalytic species regenerates and the thermodynamic and kinetic behaviour of the reaction intermediates remain uncertain. The aim of this study was to clarify some of these uncertainties by performing an electrochemical investigation of the reduction of 4 M nitric acid at 40 C at an inert electrode (platinum or gold). An inert electrode was chosen as the working electrode in a first step to avoid its oxidation and focus the research on the reduction mechanism. This experimental work enabled us to suggest a coherent sequence of electrochemical and chemical reactions. Kinetic modelling of this sequence was then carried out for a gold rotating disk electrode. A thermodynamic study at 25 C allowed the composition of the liquid and gaseous phases of nitric acid solutions in the concentration range 0.5-22 M to be evaluated. The kinetics of the reduction of 4 M nitric acid was investigated by cyclic voltammetry and chrono-amperometry at an inert electrode at 40 C. The coupling of chrono-amperometry and FTIR spectroscopy in the gaseous phase led to the identification of the gaseous reduction products as a function of the cathodic overpotential. The results showed that the reduction process is autocatalytic for potentials between 0

  2. Manganese mediated oxidation of progesterone in alkaline medium: Mechanism study and quantitative determination

    International Nuclear Information System (INIS)

    Shamsipur, Mojtaba; Pashabadi, Afshin; Taherpour, Avat; Bahrami, Kiumars; Sharghi, Hashem

    2017-01-01

    Highlights: • This is first report on oxidation of progesterone in alkaline medium using a new manganese (III) Schiff base complex. • Utilizing QM and MM, we modelled and interpreted the observed electrochemical behavior of complex on carbon and gold materials as platform. • The long term stability of proposed sensor is improved relative to previously reported immunosensors for P4. • A detailed mechanism was developed for the oxidation of P4. • The proposed sensor was applied to quantify P4 in cow’s milk. - Abstract: We report here a non-immunosensing approach for the electrocatalytic oxidation of progesterone (P4) in alkaline medium using a salen-type manganese Schiff base complex (Mn(III)-SB) as a suitable electrocatalyst. We explored the role of carbon surface at glassy carbon electrode (GCE) and gold surface at glassy carbon/gold nanoparticles modified electrode (GCE/AuNPs) on immobilization of the Mn(III)-SB complex using cyclic voltammetry (CV) and density functional theory (DFT) calculations. The GCE/Mn(III)-SB displayed a pair of small redox peaks attributed to Mn(II) ⇄ Mn(III) with a small peak-to-peak separation (ΔE p ), while GCE/AuNP/Mn(III)-SB displayed redox peaks with larger densities, but with a wider ΔE p . A combined molecular mechanics (MM) and quantum mechanics (QM) study were carried out to investigate the variation of surface configuration and energy barrier, when the Mn(III)-SB immobilization was modeled on GCE and GCE/Au surface. Cyclic voltammetry and hydrodynamic amperometry were used for the quantitative determination of P4. A limit of detection (LOD) of 11.4 nM was obtained using amperometry. The sensor retained 91% of its original response after 3 months, which is improved compared to previously reported P4 immunosensors. For the first time, a detailed mechanism for oxidation of P4 in alkaline medium was suggested. The proposed sensor was utilized to determine progesterone in milk samples.

  3. Facile hydrothermal growth graphene/ZnO nanocomposite for development of enhanced biosensor

    Energy Technology Data Exchange (ETDEWEB)

    Low, Sze Shin [Department of Electrical and Electronic Engineering, Faculty of Engineering, University of Nottingham Malaysia Campus, Jalan Broga, 43500 Semenyih, Selangor (Malaysia); Division of Materials, Mechanics and Structures, Center of Nanotechnology and Advanced Materials, Faculty of Engineering, University of Nottingham Malaysia Campus, Jalan Broga, 43500 Semenyih, Selangor (Malaysia); Tan, Michelle T.T., E-mail: Michelle.Tan@nottingham.edu.my [Department of Electrical and Electronic Engineering, Faculty of Engineering, University of Nottingham Malaysia Campus, Jalan Broga, 43500 Semenyih, Selangor (Malaysia); Division of Materials, Mechanics and Structures, Center of Nanotechnology and Advanced Materials, Faculty of Engineering, University of Nottingham Malaysia Campus, Jalan Broga, 43500 Semenyih, Selangor (Malaysia); Loh, Hwei-San [School of Biosciences, Faculty of Science, University of Nottingham Malaysia Campus, Jalan Broga, 43500 Semenyih, Selangor (Malaysia); Biotechnology Research Centre, University of Nottingham Malaysia Campus, Jalan Broga, 43500 Semenyih, Selangor (Malaysia); Khiew, Poi Sim [Division of Materials, Mechanics and Structures, Center of Nanotechnology and Advanced Materials, Faculty of Engineering, University of Nottingham Malaysia Campus, Jalan Broga, 43500 Semenyih, Selangor (Malaysia); Chiu, Wee Siong [Low Dimensional Materials Research Center, Department of Physics, Faculty of Science, University Malaya, 50603 Kuala Lumpur (Malaysia)

    2016-01-15

    Graphene/zinc oxide nanocomposite was synthesised via a facile, green and efficient approach consisted of novel liquid phase exfoliation and solvothermal growth for sensing application. Highly pristine graphene was synthesised through mild sonication treatment of graphite in a mixture of ethanol and water at an optimum ratio. The X-ray diffractometry (XRD) affirmed the hydrothermal growth of pure zinc oxide nanoparticles from zinc nitrate hexahydrate precursor. The as-prepared graphene/zinc oxide (G/ZnO) nanocomposite was characterised comprehensively to evaluate its morphology, crystallinity, composition and purity. All results clearly indicate that zinc oxide particles were homogenously distributed on graphene sheets, without any severe aggregation. The electrochemical performance of graphene/zinc oxide nanocomposite-modified screen-printed carbon electrode (SPCE) was evaluated using cyclic voltammetry (CV) and amperometry analysis. The resulting electrode exhibited excellent electrocatalytic activity towards the reduction of hydrogen peroxide (H{sub 2}O{sub 2}) in a linear range of 1–15 mM with a correlation coefficient of 0.9977. The sensitivity of the graphene/zinc oxide nanocomposite-modified hydrogen peroxide sensor was 3.2580 μAmM{sup −1} with a limit of detection of 7.4357 μM. An electrochemical DNA sensor platform was then fabricated for the detection of Avian Influenza H5 gene based on graphene/zinc oxide nanocomposite. The results obtained from amperometry study indicate that the graphene/zinc oxide nanocomposite-enhanced electrochemical DNA biosensor is significantly more sensitive (P < 0.05) and efficient than the conventional agarose gel electrophoresis. - Highlights: • One step, green and facile exfoliation of graphite in ethanol/water mixture. • G/ZnO nanocomposite prepared via simple, green low temperature solvothermal method. • CV and amperometric study of G/ZnO nanocomposite towards H{sub 2}O{sub 2} with R{sup 2} of 0.9977.

  4. Some aspects of surfactant action mechanism in the organic reagents - metal ions systems

    Energy Technology Data Exchange (ETDEWEB)

    Chernova, R K; Shtykov, S N; Beloliptseva, G M; Sukhova, L K; Amelin, V G; Kulapina, E G [Saratovskij Gosudarstvennyj Univ. (USSR)

    1984-06-01

    Results are reviewed of investigations into the interaction of ions of Mo(6), W, Zr, Be, Sc, Nb, Ta, J, rare earths, a. o. with organic reagents of triphenylmethane class in the 8M H/sub 2/SO/sub 4/-pH14 acidity range and the 1x10/sup -3/-5x10/sup -6/ M concentration range both in the presence and absence of different surfactant type (cetylpyridine, methyltrimethylammonium, synthanols, etc). Three types of effects, determining enhancement of the sensitivity and selectivity of reactions jn the Me-R-surfactant systems, were determined: an increase in the number of coordinated ligands, the activating effect of cation surfactants resulting in a potential complexing in acid media, multicenter interaction of polydentate ligands both via chelating groups and auxochrome groups in the presence of cation surfactants. Protolytic and flotation properties of ionic associates are considered. The observed effects are explained from the viewpoint of electrostatic and hydrophobic interactions in the R-surfactant systems, observed by the methods of NMR, polarography amperometry, conductometry. A possible use of the investigated M-R-surfactant systems as complexonometric indicators was evaluated. A possibility was shown of using them for direct titrimetric determination of hundredth milligram portions of Cu, Ga, In and Sc at a titrant concentratjon of less than 0.01 M. It follows from the estimation of basic optical parameters of the Me-R-surfactant systems that detection.

  5. Some aspects of surfactant action mechanism in the organic reagents - metal ions systems

    International Nuclear Information System (INIS)

    Chernova, R.K.; Shtykov, S.N.; Beloliptseva, G.M.; Sukhova, L.K.; Amelin, V.G.; Kulapina, E.G.

    1984-01-01

    Results are reviewed of investigations into the interaction of ions of Mo(6), W, Zr, Be, Sc, Nb, Ta, J, rare earths, a. o. with organic reagents of triphenylmethane class in the 8M H 2 SO 4 -pH14 acidity range and the 1x10 -3 -5x10 -6 M concentration range both in the presence and absence of different surfactant type (cetylpyridine, methyltrimethylammonium, synthanols, etc). Three types of effects, determining enhancement of the sensitivity and selectivity of reactions jn the Me-R-surfactant systems, were determined: an increase in the number of coordinated ligands, the activating effect of cation surfactants resulting in a potential complexing in acid media, multicenter interaction of polydentate ligands both via chelating groups and auxochrome groups in the presence of cation surfactants. Protolytic and flotation properties of ionic associates are considered. The observed effects are explained from the viewpoint of electrostatic and hydrophobic interactions in the R-surfactant systems, observed by the methods of NMR, polarography amperometry, conductometry. A possible use of the investigated M-R-surfactant systems as complexonometric indicators was evaluated. A possibility was shown of using them for direct titrimetric determination of hundredth milligram portions of Cu, Ga, In and Sc at a titrant concentratjon of less than 0.01 M. It follows from the estimation of basic optical parameters of the Me-R-surfactant systems that detection

  6. Conducting polymer‐coated, palladium‐functionalized multi‐walled carbon nanotubes for the electrochemical sensing of hydroxylamine

    International Nuclear Information System (INIS)

    Lee, Eunhee; Ahmed, Mohammad Shamsuddin; You, Jung-Min; Kim, Seul Ki; Jeon, Seungwon

    2012-01-01

    Electrochemical sensors of hydroxylamine were fabricated on glassy carbon electrodes (GCEs) by the electropolymerization of 3,4‐ethylenedioxypyrrole (EDOP) and 3,4‐ethylenedioxythiophene (EDOT) on palladium (Pd) nanoparticles attached to thiolated multi‐walled carbon nanotubes (MWCNTs), denoted as PEDOP/MWCNT‐Pd/GCE and PEDOT/MWCNT‐Pd/GCE. The sensors were characterized by field emission scanning electron microscopy and electrochemical impedance spectroscopy. They showed strong catalytic activity toward the oxidation of hydroxylamine. Cyclic voltammetry and amperometry were used to characterize the sensors' performances. The detection limits of hydroxylamine by PEDOP/MWCNT‐Pd/GCE and PEDOT/MWCNT‐Pd/GCE were 0.22 and 0.24 μM (S/N = 3), respectively. The sensors' sensitivity, selectivity, and stability were also investigated. - Highlights: ► Multi-wall carbon nanotubes-Pd nanoparticles (MWCNT-Pd) based electrodes. ► Electropolymerized electrodes by poly3,4-ethylenedioxythiophene(PEDOT). ► PEDOT/MWCNT-Pd has a low detection limit of 0.24 µM for hydroxylamine. ► PEDOT/MWCNT-Pd exhibits a wide linear range from 1 µM to 6 mM hydroxylamine. ► The resulting sensor shows fast response and good stability.

  7. Conducting polymer-coated, palladium-functionalized multi-walled carbon nanotubes for the electrochemical sensing of hydroxylamine

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Eunhee; Ahmed, Mohammad Shamsuddin; You, Jung-Min; Kim, Seul Ki; Jeon, Seungwon, E-mail: swjeon@chonnam.ac.kr

    2012-08-31

    Electrochemical sensors of hydroxylamine were fabricated on glassy carbon electrodes (GCEs) by the electropolymerization of 3,4-ethylenedioxypyrrole (EDOP) and 3,4-ethylenedioxythiophene (EDOT) on palladium (Pd) nanoparticles attached to thiolated multi-walled carbon nanotubes (MWCNTs), denoted as PEDOP/MWCNT-Pd/GCE and PEDOT/MWCNT-Pd/GCE. The sensors were characterized by field emission scanning electron microscopy and electrochemical impedance spectroscopy. They showed strong catalytic activity toward the oxidation of hydroxylamine. Cyclic voltammetry and amperometry were used to characterize the sensors' performances. The detection limits of hydroxylamine by PEDOP/MWCNT-Pd/GCE and PEDOT/MWCNT-Pd/GCE were 0.22 and 0.24 {mu}M (S/N = 3), respectively. The sensors' sensitivity, selectivity, and stability were also investigated. - Highlights: Black-Right-Pointing-Pointer Multi-wall carbon nanotubes-Pd nanoparticles (MWCNT-Pd) based electrodes. Black-Right-Pointing-Pointer Electropolymerized electrodes by poly3,4-ethylenedioxythiophene(PEDOT). Black-Right-Pointing-Pointer PEDOT/MWCNT-Pd has a low detection limit of 0.24 Micro-Sign M for hydroxylamine. Black-Right-Pointing-Pointer PEDOT/MWCNT-Pd exhibits a wide linear range from 1 Micro-Sign M to 6 mM hydroxylamine. Black-Right-Pointing-Pointer The resulting sensor shows fast response and good stability.

  8. Electrooxidation of borohydride on platinum and gold electrodes: implications for direct borohydride fuel cells

    International Nuclear Information System (INIS)

    Gyenge, Elod

    2004-01-01

    The electrochemical oxidation of BH 4 - in 2 M NaOH on Pt and Au (i.e. catalytic and non-catalytic electrodes, respectively, for BH 4 - hydrolysis accompanied by H 2 evolution) has been studied by cyclic voltammetry, chrono-techniques (i.e., potentiometry, amperometry, coulometry) and electrochemical impedance spectroscopy. In the case of Pt the cyclic voltammetry behaviour of BH 4 - is influenced by both, the catalytic hydrolysis of BH 4 - yielding H 2 (followed by electrooxidation of the latter at peak potentials between -0.7 and -0.9 V versus Ag/AgCl, KCl std ) and direct oxidation of BH 4 - at more positive potentials, i.e., between -0.15 and -0.05 V. Thiourea (TU, 1.5x10 -3 M) was an effective inhibitor of the catalytic hydrolysis associated with BH 4 - electrooxidation on Pt. Therefore, in the presence of TU, only the direct oxidation of BH 4 - has been detected, with peak potentials between -0.2 and 0 V. It is proposed that TU could improve the BH 4 - utilization efficiency and the coulombic efficiency of direct borohydride fuel cells using catalytic anodes. The electrooxidation of BH 4 - on Pt/TU is an overall four-electron process, instead of the maximum eight electrons reported for Au, and it is affected by adsorbed species such as BH 4 - (fractional surface coverage ∼0.3), TU and possibly reaction intermediates

  9. Electrochemical studies of iron/carbonates system applied to the formation of thin layers of siderite on inert substrates; Etudes electrochimiques du systeme fer/carbonates appliquees a la formation de couches minces de siderite sur des substrats inertes

    Energy Technology Data Exchange (ETDEWEB)

    Ithurbide, A. [CEA Saclay, Dept. de Physico-Chimie (DEN/DPC/SECR/L3MR), 91 - Gif sur Yvette (France); Peulon, S. [Univ. d' Evry-val-d' Essonne, UMR 8587, CNRS, 91 - Evry (France); Mandin, Ph. [Ecole Nationale Superieure de Chimie de Paris (ENSCP), UMR 7575, 75 - Paris (France); Beaucaire, C. [CEA Saclay, Dept. de Physico-Chimie (DEN/DPC/SECR/L3MR), 91 - Gif sur Yvette (France); Chausse, A. [Univ. d' Evry-val-d' Essonne, UMR 8587, CNRS, 91 - Evry (France)

    2007-07-01

    In order to understand the complex mechanisms of the reactions occurring, a methodology is developed. It is based on the use of compounds electrodeposited under the form of thin layers and which are used then as electrodes to study their interactions with the toxic species. It is in this framework that is studied the electrodeposition of siderite on inert substrates. At first, have been studied iron electrochemical systems in carbonated solutions. These studies have been carried out with classical electrochemical methods (cyclic voltametry, amperometry) coupled to in-situ measurements: quartz microbalance, pH. Different compounds have been obtained under the form of homogeneous and adherent thin layers. The analyses of these depositions, by different ex-situ characterizations (XRD, IR, SEM, EDS..) have revealed particularly the presence of siderite. Then, the influence of several experimental parameters (substrate, potential, medium composition, temperature) on the characteristics of siderite thin layers has been studied. From these experimental results, models have been proposed. (O.M.)

  10. Electrochemical studies of iron/carbonates system applied to the formation of thin layers of siderite on inert substrates

    International Nuclear Information System (INIS)

    Ithurbide, A.; Peulon, S.; Mandin, Ph.; Beaucaire, C.; Chausse, A.

    2007-01-01

    In order to understand the complex mechanisms of the reactions occurring, a methodology is developed. It is based on the use of compounds electrodeposited under the form of thin layers and which are used then as electrodes to study their interactions with the toxic species. It is in this framework that is studied the electrodeposition of siderite on inert substrates. At first, have been studied iron electrochemical systems in carbonated solutions. These studies have been carried out with classical electrochemical methods (cyclic voltametry, amperometry) coupled to in-situ measurements: quartz microbalance, pH. Different compounds have been obtained under the form of homogeneous and adherent thin layers. The analyses of these depositions, by different ex-situ characterizations (XRD, IR, SEM, EDS..) have revealed particularly the presence of siderite. Then, the influence of several experimental parameters (substrate, potential, medium composition, temperature) on the characteristics of siderite thin layers has been studied. From these experimental results, models have been proposed. (O.M.)

  11. Modified gold surfaces by 6-(ferrocenyl)hexanethiol/dendrimer/gold nanoparticles as a platform for the mediated biosensing applications

    Energy Technology Data Exchange (ETDEWEB)

    Karadag, Murat; Geyik, Caner; Demirkol, Dilek Odaci [Ege University, Faculty of Science, Biochemistry Department, 35100 Bornova-Izmir (Turkey); Ertas, F. Nil [Ege University, Faculty of Science, Chemistry Department, 35100, Bornova-Izmir (Turkey); Timur, Suna, E-mail: suna.timur@ege.edu.tr [Ege University, Faculty of Science, Biochemistry Department, 35100 Bornova-Izmir (Turkey)

    2013-03-01

    An electrochemical biosensor mediated by using 6-(Ferrocenyl) hexanethiol (FcSH) was fabricated by construction of gold nanoparticles (AuNPs) on the surface of polyamidoamine dendrimer (PAMAM) modified gold electrode. Glucose oxidase (GOx) was used as a model enzyme and was immobilized onto the gold surface forming a self assembled monolayer via FcSH and cysteamine. Cyclic voltammetry and amperometry were used for the characterization of electrochemical response towards glucose substrate. Following the optimization of medium pH, enzyme loading, AuNP and FcSH amount, the linear range for the glucose was studied and found as 1.0 to 5.0 mM with the detection limit (LOD) of 0.6 mM according to S/N = 3. Finally, the proposed Au/AuNP/(FcSH + Cyst)/PAMAM/GOx biosensor was successfully applied for the glucose analysis in beverages, and the results were compared with those obtained by HPLC. Highlights: Black-Right-Pointing-Pointer Immobilized mediator in SAM layer and dendrimeric structure to expand surface area. Black-Right-Pointing-Pointer Au nanoparticles for enhanced electron transfer. Black-Right-Pointing-Pointer Satisfactory Limit of Detection with 0.6 mM.

  12. Immobilization of Glucose Oxidase on a Carbon Nanotubes/Dendrimer-Ferrocene Modified Electrode for Reagentless Glucose Biosensing.

    Science.gov (United States)

    Zhou, Juan; Li, Huan; Yang, Huasong; Cheng, Hui; Lai, Guosong

    2017-01-01

    Ferrocene-grafted dendrimer was covalently linked to the surface of a carbon nanotubes (CNTs)-chitosan (CS) nanocomposite modified electrode for immobilizing high-content glucose oxidase (GOx), which resulted in the successful development a novel reagentless glucose biosensor. Electrochemical impedance spectroscopy, cyclic voltammetry, and amperometry were used to characterize the preparation process and the enzymatically catalytic response of this biosensor. Due to the excellent electron transfer acceleration of the CNTs and the high-content loading of the GOx biomolecule and ferrocene mediator on the electrode matrix, this biosensor showed excellent analytical performance such as fast response time less than 10 s, wide linear range from 0.02 to 2.91 mM and low detection limit down to 7.5 μM as well as satisfactory stability and reproducibility toward the amperometric glucose determination. In addition, satisfactory result was obtained when it was used for the glucose measurements in human blood samples. Thus this biosensor provides great potentials for practical applications.

  13. An amperometric enzyme biosensor for real-time measurements of cellobiohydrolase activity on insoluble cellulose

    DEFF Research Database (Denmark)

    Cruys-Bagger, Nicolaj; Guilin, Ren; Tatsumi, Hirosuke

    2012-01-01

    An amperometric enzyme biosensor for continuous detection of cellobiose has been implemented as an enzyme assay for cellulases. We show that the initial kinetics for cellobiohydrolase I, Cel7A from Trichoderma reesei, acting on different types of cellulose substrates, semi-crystalline and amorphous......, can be monitored directly and in real-time by an enzyme-modified electrode based on cellobiose dehydrogenase (CDH) from Phanerochaete chrysosporium (Pc). PcCDH was cross-linked and immobilized on the surface of a carbon paste electrode which contained a mediator, benzoquinone. An oxidation current...... of the reduced mediator, hydroquinone, produced by the CDH-catalyzed reaction with cellobiose, was recorded under constant-potential amperometry at +0.5 V (vs. Ag/AgCl). The CDH-biosensors showed high sensitivity (87.7 µA mM−1 cm−2), low detection limit (25 nM), and fast response time (t95% ∼ 3 s...

  14. Feeding induced by cannabinoids is mediated independently of the melanocortin system.

    Directory of Open Access Journals (Sweden)

    Puspha Sinnayah

    2008-05-01

    Full Text Available Cannabinoids, the active components of marijuana, stimulate appetite, and cannabinoid receptor-1 (CB1-R antagonists suppress appetite and promote weight loss. Little is known about how CB1-R antagonists affect the central neurocircuitry, specifically the melanocortin system that regulates energy balance.Here, we show that peripherally administered CB1-R antagonist (AM251 or agonist equally suppressed or stimulated feeding respectively in A(y , which lack a functional melanocortin system, and wildtype mice, demonstrating that cannabinoid effects on feeding do not require melanocortin circuitry. CB1-R antagonist or agonist administered into the ventral tegmental area (VTA equally suppressed or stimulated feeding respectively, in both genotypes. In addition, peripheral and central cannabinoid administration similarly induced c-Fos activation in brain sites suggesting mediation via motivational dopaminergic circuitry. Amperometry-detected increases in evoked dopamine (DA release by the CB1-R antagonist in nucleus accumbens slices indicates that AM251 modulates DA release from VTA terminals.Our results demonstrate that the effects of cannabinoids on energy balance are independent of hypothalamic melanocortin circuitry and is primarily driven by the reward system.

  15. Trace lead analysis based on carbon-screen-printed-electrodes modified via 4-carboxy-phenyl diazonium salt electroreduction

    International Nuclear Information System (INIS)

    Bouden, Sarra; Chausse, Annie; Dorbes, Stephane; El Tall, Omar; Bellakhal, Nizar; Dachraoui, Mohamed; Vautrin-Ul, Christine

    2013-01-01

    This paper describes the use of 4-carboxyphenyl-grafted screen-printed carbon electrodes (4-CP-SPEs) for trace lead analysis.These novel and simple use of electrodes were easily prepared by the electrochemical reduction of the corresponding diazonium salt. Pb detection was then performed by a three-steps method in order to avoid oxygen interference:(i)immersion of the grafted screen-printed electrode (SPE) in the sample and adsorption of Pb(II), (ii)reduction of adsorbed Pb(II) by chrono-amperometry (CA), and (iii) oxidation of Pb by Anodic Square Wave Voltammetry (SWV).The re-oxidation response was exploited for lead detection and quantification. In order to optimize the analytical responses, the influence of the adsorption medium pH and the adsorption time were investigated. Moreover, an interference study was carried out with Cu(II), Hg(II), Al(III), Mn(II), Zn(II), Cd(II) and no major interference can be expected to quantify Pb(II). The described method provided a limit of detection and a limit of quantification of 1.2*10 9 M and 4.1*10 9 M, respectively. These performances indicate that the 4-CP-SPE could be considered as an efficient tool for environmental analysis. (authors)

  16. Amperometric detector for gas chromatography based on a silica sol-gel solid electrolyte.

    Science.gov (United States)

    Steinecker, William H; Miecznikowski, Krzysztof; Kulesza, Pawel J; Sandlin, Zechariah D; Cox, James A

    2017-11-01

    An electrochemical cell comprising a silica sol-gel solid electrolyte, a working electrode that protrudes into a gas phase, and reference and counter electrodes that contact the solid electrolyte comprises an amperometric detector for gas chromatography. Under potentiostatic conditions, a current related to the concentration of an analyte in the gas phase is produced by its oxidation at the three-phase boundary among the sol-gel, working electrode, and the gas phase. The sol-gel is processed to contain an electrolyte that also serves as a humidistat to maintain a constant water activity even in the presence the gas chromatographic mobile phase. Response was demonstrated toward a diverse set of analytes, namely hydrogen, 1,2-ethandithiol, phenol, p-cresol, and thioanisole. Using flow injection amperometry of hydrogen with He as the carrier gas, 90% of the steady-state current was achieved in < 1s at a flow rate of 20mLmin -1 . A separation of 1,2-ethandithiol, phenol, p-cresol, and thioanisole at a 2.2mLmin -1 flow rate was achieved with respective detection limits (k = 3 criterion) of 4, 1, 3, and 70 ppmv when the working electrode potential was 800mV. Copyright © 2017 Elsevier B.V. All rights reserved.

  17. Real-time changes in hippocampal energy demands during a spatial working memory task.

    Science.gov (United States)

    Kealy, John; Bennett, Rachel; Woods, Barbara; Lowry, John P

    2017-05-30

    Activity-dependent changes in hippocampal energy consumption have largely been determined using microdialysis. However, real-time recordings of brain energy consumption can be more accurately achieved using amperometric sensors, allowing for sensitive real-time monitoring of concentration changes. Here, we test the theory that systemic pre-treatment with glucose in rats prevents activity-dependent decreases in hippocampal glucose levels and thus enhances their performance in a spontaneous alternation task. Male Sprague Dawley rats were implanted into the hippocampus with either: 1) microdialysis probe; or 2) an oxygen sensor and glucose biosensor co-implanted together. Animals were pre-treated with either saline or glucose (250mg/kg) 30min prior to performing a single 20-min spontaneous alternation task in a +-maze. There were no significant differences found between either treatment group in terms of spontaneous alternation performance. Additionally, there was a significant difference found between treatment groups on hippocampal glucose levels measured using microdialysis (a decrease associated with glucose pre-treatment in control animals) but not amperometry. There were significant increases in hippocampal oxygen during +-maze exploration. Combining the findings from both methods, it appears that hippocampal activity in the spontaneous alternation task does not cause an increase in glucose consumption, despite an increase in regional cerebral blood flow (using oxygen supply as an index of blood flow) and, as such, pre-treatment with glucose does not enhance spontaneous alternation performance. Copyright © 2017 Elsevier B.V. All rights reserved.

  18. Emerging nanotechnology-based strategies for the identification of microbial pathogenesis.

    Science.gov (United States)

    Kaittanis, Charalambos; Santra, Santimukul; Perez, J Manuel

    2010-03-18

    Infectious diseases are still a major healthcare problem. From food intoxication and contaminated water, to hospital-acquired diseases and pandemics, infectious agents cause disease throughout the world. Despite advancements in pathogens' identification, some of the gold-standard diagnostic methods have limitations, including laborious sample preparation, bulky instrumentation and slow data readout. In addition, new field-deployable diagnostic modalities are urgently needed in first responder and point-of-care applications. Apart from compact, these sensors must be sensitive, specific, robust and fast, in order to facilitate detection of the pathogen even in remote rural areas. Considering these characteristics, researchers have utilized innovative approaches by employing the unique properties of nanomaterials in order to achieve detection of infectious agents, even in complex media like blood. From gold nanoparticles and their plasmonic shifts to iron oxide nanoparticles and changes in magnetic properties, detection of pathogens, toxins, antigens and nucleic acids has been achieved with impressive detection thresholds. Additionally, as bacteria become resistant to antibiotics, nanotechnology has achieved the rapid determination of bacterial drug susceptibility and resistance using novel methods, such as amperometry and magnetic relaxation. Overall, these promising results hint to the adoption of nanotechnology-based diagnostics for the diagnosis of infectious diseases in diverse settings throughout the globe, preventing epidemics and safeguarding human and economic wellness. Copyright 2009 Elsevier B.V. All rights reserved.

  19. Determination of hydrogen peroxide and glucose using a novel sensor platform based on Co0.4Fe0.6LaO3 nanoparticles

    International Nuclear Information System (INIS)

    Zhang, Zhen; Gu, Shuqing; Ding, Yaping; Zhang, Fenfen; Jin, Jindi

    2013-01-01

    We report on a novel nonenzymatic sensor platform for the determination of hydrogen peroxide and glucose. It is based on a carbon paste electrode that was modified with Co 0.4 Fe 0.6 LaO 3 nanoparticles synthesized by the sol–gel method. The structure and morphology of Co 0.4 Fe 0.6 LaO 3 nanoparticles were characterized by X-ray diffraction, scanning electron microscopy, and transmission electron microscopy. The electrochemical performance of this sensor was evaluated by cyclic voltammetry and amperometry, and the results demonstrated that it exhibits strong electrocatalytical activity towards the oxidation of H 2 O 2 and glucose in an alkaline medium. The sensor has a limit of detection as low as 2.0 nM of H 2 O 2 and a linear range that extends from 0.01 to 800 μM. The response to glucose is characterized by two analytical ranges of different slope, viz. from 0.05 to 5 μM and from 5 to 500 μM, with a 10 nM limit of detection. The glucose sensor has a fast response and good long term stability. (author)

  20. Examining changes in cellular communication in neuroendocrine cells after noble metal nanoparticle exposure.

    Science.gov (United States)

    Love, Sara A; Liu, Zhen; Haynes, Christy L

    2012-07-07

    As nanoparticles enjoy increasingly widespread use in commercial applications, the potential for unintentional exposure has become much more likely during any given day. Researchers in the field of nanotoxicity are working to determine the physicochemical nanoparticle properties that lead to toxicity in an effort to establish safe design rules. This work explores the effects of noble metal nanoparticle exposure in murine chromaffin cells, focusing on examining the effects of size and surface functionality (coating) in silver and gold, respectively. Carbon-fibre microelectrode amperometry was utilized to examine the effect of exposure on exocytosis function, at the single cell level, and provided new insights into the compromised functions of cells. Silver nanoparticles of varied size, between 15 and 60 nm diameter, were exposed to cells and found to alter the release kinetics of exocytosis for those cells exposed to the smallest examined size. Effects of gold were examined after modification with two commonly used 'bio-friendly' polymers, either heparin or poly (ethylene glycol), and gold nanoparticles were found to induce altered cellular adhesion or the number of chemical messenger molecules released, respectively. These results support the body of work suggesting that noble metal nanoparticles perturb exocytosis, typically altering the number of molecules and kinetics of release, and supports a direct disruption of the vesicle matrix by the nanoparticle. Overall, it is clear that various nanoparticle physicochemical properties, including size and surface coating, do modulate changes in cellular communication via exocytosis.

  1. Electrochemical Quantification of the Antioxidant Capacity of Medicinal Plants Using Biosensors

    Directory of Open Access Journals (Sweden)

    Erika Rodríguez-Sevilla

    2014-08-01

    Full Text Available The working area of a screen-printed electrode, SPE, was modified with the enzyme tyrosinase (Tyr using different immobilization methods, namely entrapment with water-soluble polyvinyl alcohol (PVA, cross-linking using glutaraldehyde (GA, and cross-linking using GA and human serum albumin (HSA; the resulting electrodes were termed SPE/Tyr/PVA, SPE/Tyr/GA and SPE/Tyr/HSA/GA, respectively. These biosensors were characterized by means of amperometry and EIS techniques. From amperometric evaluations, the apparent Michaelis-Menten constant, Km′, of each biosensor was evaluated while the respective charge transfer resistance, Rct, was assessed from impedance measurements. It was found that the SPE/Tyr/GA had the smallest Km′ (57 ± 7 µM and Rct values. This electrode also displayed both the lowest detection and quantification limits for catechol quantification. Using the SPE/Tyr/GA, the Trolox Equivalent Antioxidant Capacity (TEAC was determined from infusions prepared with “mirto” (Salvia microphylla, “hHierba dulce” (Lippia dulcis and “salve real” (Lippia alba, medicinal plants commonly used in Mexico.

  2. Electrochemical Quantification of the Antioxidant Capacity of Medicinal Plants Using Biosensors

    Science.gov (United States)

    Rodríguez-Sevilla, Erika; Ramírez-Silva, María-Teresa; Romero-Romo, Mario; Ibarra-Escutia, Pedro; Palomar-Pardavé, Manuel

    2014-01-01

    The working area of a screen-printed electrode, SPE, was modified with the enzyme tyrosinase (Tyr) using different immobilization methods, namely entrapment with water-soluble polyvinyl alcohol (PVA), cross-linking using glutaraldehyde (GA), and cross-linking using GA and human serum albumin (HSA); the resulting electrodes were termed SPE/Tyr/PVA, SPE/Tyr/GA and SPE/Tyr/HSA/GA, respectively. These biosensors were characterized by means of amperometry and EIS techniques. From amperometric evaluations, the apparent Michaelis-Menten constant, Km′, of each biosensor was evaluated while the respective charge transfer resistance, Rct, was assessed from impedance measurements. It was found that the SPE/Tyr/GA had the smallest Km′ (57 ± 7) μM and Rct values. This electrode also displayed both the lowest detection and quantification limits for catechol quantification. Using the SPE/Tyr/GA, the Trolox Equivalent Antioxidant Capacity (TEAC) was determined from infusions prepared with “mirto” (Salvia microphylla), “hHierba dulce” (Lippia dulcis) and “salve real” (Lippia alba), medicinal plants commonly used in Mexico. PMID:25111237

  3. Parsing glucose entry into the brain: novel findings obtained with enzyme-based glucose biosensors.

    Science.gov (United States)

    Kiyatkin, Eugene A; Wakabayashi, Ken T

    2015-01-21

    Extracellular levels of glucose in brain tissue reflect dynamic balance between its gradient-dependent entry from arterial blood and its use for cellular metabolism. In this work, we present several sets of previously published and unpublished data obtained by using enzyme-based glucose biosensors coupled with constant-potential high-speed amperometry in freely moving rats. First, we consider basic methodological issues related to the reliability of electrochemical measurements of extracellular glucose levels in rats under physiologically relevant conditions. Second, we present data on glucose responses induced in the nucleus accumbens (NAc) by salient environmental stimuli and discuss the relationships between local neuronal activation and rapid glucose entry into brain tissue. Third, by presenting data on changes in NAc glucose induced by intravenous and intragastric glucose delivery, we discuss other mechanisms of glucose entry into the extracellular domain following changes in glucose blood concentrations. Lastly, by showing the pattern of NAc glucose fluctuations during glucose-drinking behavior, we discuss the relationships between "active" and "passive" glucose entry to the brain, its connection to behavior-related metabolic activation, and the possible functional significance of these changes in behavioral regulation. These data provide solid experimental support for the "neuronal" hypothesis of neurovascular coupling, which postulates the critical role of neuronal activity in rapid regulation of vascular tone, local blood flow, and entry of glucose and oxygen to brain tissue to maintain active cellular metabolism.

  4. Sleep/wake dependent changes in cortical glucose concentrations.

    Science.gov (United States)

    Dash, Michael B; Bellesi, Michele; Tononi, Giulio; Cirelli, Chiara

    2013-01-01

    Most of the energy in the brain comes from glucose and supports glutamatergic activity. The firing rate of cortical glutamatergic neurons, as well as cortical extracellular glutamate levels, increase with time spent awake and decline throughout non rapid eye movement sleep, raising the question whether glucose levels reflect behavioral state and sleep/wake history. Here chronic (2-3 days) electroencephalographic recordings in the rat cerebral cortex were coupled with fixed-potential amperometry to monitor the extracellular concentration of glucose ([gluc]) on a second-by-second basis across the spontaneous sleep-wake cycle and in response to 3 h of sleep deprivation. [Gluc] progressively increased during non rapid eye movement sleep and declined during rapid eye movement sleep, while during wake an early decline in [gluc] was followed by an increase 8-15 min after awakening. There was a significant time of day effect during the dark phase, when rats are mostly awake, with [gluc] being significantly lower during the last 3-4 h of the night relative to the first 3-4 h. Moreover, the duration of the early phase of [gluc] decline during wake was longer after prolonged wake than after consolidated sleep. Thus, the sleep/wake history may affect the levels of glucose available to the brain upon awakening. © 2012 The Authors Journal of Neurochemistry © 2012 International Society for Neurochemistry.

  5. Graphene: The Missing Piece for Cancer Diagnosis?

    Science.gov (United States)

    Cruz, Sandra M. A.; Girão, André F.; Gonçalves, Gil; Marques, Paula A. A. P.

    2016-01-01

    This paper reviews recent advances in graphene-based biosensors development in order to obtain smaller and more portable devices with better performance for earlier cancer detection. In fact, the potential of Graphene for sensitive detection and chemical/biological free-label applications results from its exceptional physicochemical properties such as high electrical and thermal conductivity, aspect-ratio, optical transparency and remarkable mechanical and chemical stability. Herein we start by providing a general overview of the types of graphene and its derivatives, briefly describing the synthesis procedure and main properties. It follows the reference to different routes to engineer the graphene surface for sensing applications with organic biomolecules and nanoparticles for the development of advanced biosensing platforms able to detect/quantify the characteristic cancer biomolecules in biological fluids or overexpressed on cancerous cells surface with elevated sensitivity, selectivity and stability. We then describe the application of graphene in optical imaging methods such as photoluminescence and Raman imaging, electrochemical sensors for enzymatic biosensing, DNA sensing, and immunosensing. The bioquantification of cancer biomarkers and cells is finally discussed, particularly electrochemical methods such as voltammetry and amperometry which are generally adopted transducing techniques for the development of graphene based sensors for biosensing due to their simplicity, high sensitivity and low-cost. To close, we discuss the major challenges that graphene based biosensors must overcome in order to reach the necessary standards for the early detection of cancer biomarkers by providing reliable information about the patient disease stage. PMID:26805845

  6. Development and Characterization of a Diamond-Insulated Graphitic Multi Electrode Array Realized with Ion Beam Lithography

    Directory of Open Access Journals (Sweden)

    Federico Picollo

    2014-12-01

    Full Text Available The detection of quantal exocytic events from neurons and neuroendocrine cells is a challenging task in neuroscience. One of the most promising platforms for the development of a new generation of biosensors is diamond, due to its biocompatibility, transparency and chemical inertness. Moreover, the electrical properties of diamond can be turned from a perfect insulator into a conductive material (resistivity ~mΩ·cm by exploiting the metastable nature of this allotropic form of carbon. A 16‑channels MEA (Multi Electrode Array suitable for cell culture growing has been fabricated by means of ion implantation. A focused 1.2 MeV He+ beam was scanned on a IIa single-crystal diamond sample (4.5 × 4.5 × 0.5 mm3 to cause highly damaged sub-superficial structures that were defined with micrometric spatial resolution. After implantation, the sample was annealed. This process provides the conversion of the sub-superficial highly damaged regions to a graphitic phase embedded in a highly insulating diamond matrix. Thanks to a three-dimensional masking technique, the endpoints of the sub-superficial channels emerge in contact with the sample surface, therefore being available as sensing electrodes. Cyclic voltammetry and amperometry measurements of solutions with increasing concentrations of adrenaline were performed to characterize the biosensor sensitivity. The reported results demonstrate that this new type of biosensor is suitable for in vitro detection of catecholamine release.

  7. Simultaneous Voltammetric/Amperometric Determination of Sulfide and Nitrite in Water at BDD Electrode

    Directory of Open Access Journals (Sweden)

    Anamaria Baciu

    2015-06-01

    Full Text Available This work reported new voltammetric/amperometric-based protocols using a commercial boron-doped diamond (BDD electrode for simple and fast simultaneous detection of sulfide and nitrite from water. Square-wave voltammetry operated under the optimized working conditions of 0.01 V step potential, 0.5 V modulation amplitude and 10 Hz frequency allowed achieving the best electroanalytical parameters for the simultaneous detection of nitrite and sulfide. For practical in-field detection applications, the multiple-pulsed amperometry technique was operated under optimized conditions, i.e., −0.5 V/SCE for a duration of 0.3 s as conditioning step, +0.85 V/SCE for a duration of 3 s that assure the sulfide oxidation and +1.25 V/SCE for a duration of 0.3 s, where the nitrite oxidation occurred, which allowed the simultaneously detection of sulfide and nitrite without interference between them. Good accuracy was found for this protocol in comparison with standardized methods for each anion. Also, no interference effect was found for the cation and anion species, which are common in the water matrix.

  8. Investigation of sulfonated polysulfone membranes as electrolyte in a passive-mode direct methanol fuel cell mini-stack

    Energy Technology Data Exchange (ETDEWEB)

    Lufrano, F.; Baglio, V.; Staiti, P.; Stassi, A.; Arico, A.S.; Antonucci, V. [CNR - ITAE, Istituto di Tecnologie Avanzate per l' Energia ' ' Nicola Giordano' ' , Via Salita S. Lucia sopra Contesse n. 5 - 98126 S. Lucia - Messina (Italy)

    2010-12-01

    This paper reports on the development of polymer electrolyte membranes (PEMs) based on sulfonated polysulfone for application in a DMFC mini-stack operating at room temperature in passive mode. The sulfonated polysulfone (SPSf) with two degrees of sulfonation (57 and 66%) was synthesized by a well-known sulfonation process. SPSf membranes with different thicknesses were prepared and investigated. These membranes were characterized in terms of methanol/water uptake, proton conductivity, and fuel cell performance in a DMFC single cell and mini-stack operating at room temperature. The study addressed (a) control of the synthesis of sulfonated polysulfone, (b) optimization of the assembling procedure, (c) a short lifetime investigation and (d) a comparison of DMFC performance in active-mode operation vs. passive-mode operation. The best passive DMFC performance was 220 mW (average cell power density of about 19 mW cm{sup -2}), obtained with a thin SPSf membrane (70 {mu}m) at room temperature, whereas the performance of the same membrane-based DMFC in active mode was 38 mW cm{sup -2}. The conductivity of this membrane, SPSf (IEC = 1.34 mequiv. g{sup -1}) was 2.8 x 10{sup -2} S cm{sup -1}. A preliminary short-term test (200 min) showed good stability during chrono-amperometry measurements. (author)

  9. CE microchips: an opened gate to food analysis.

    Science.gov (United States)

    Escarpa, Alberto; González, María Cristina; Crevillén, Agustín González; Blasco, Antonio Javier

    2007-03-01

    CE microchips are the first generation of micrototal analysis systems (-TAS) emerging in the miniaturization scene of food analysis. CE microchips for food analysis are fabricated in both glass and polymer materials, such as PDMS and poly(methyl methacrylate) (PMMA), and use simple layouts of simple and double T crosses. Nowadays, the detection route preferred is electrochemical in both, amperometry and conductivity modes, using end-channel and contactless configurations, respectively. Food applications using CE microchips are now emerging since food samples present complex matrices, the selectivity being a very important challenge because the total integration of analytical steps into microchip format is very difficult. As a consequence, the first contributions that have recently appeared in the relevant literature are based primarily on fast separations of analytes of high food significance. These protocols are combined with different strategies to achieve selectivity using a suitable nonextensive sample preparation and/or strategically choosing detection routes. Polyphenolic compounds, amino acids, preservatives, and organic and inorganic ions have been studied using CE microchips. Thus, new and exciting future expectations arise in the domain of food analysis. However, several drawbacks could easily be found and assumed within the miniaturization map.

  10. Mechanism for optimization of signal-to-noise ratio of dopamine release based on short-term bidirectional plasticity.

    Science.gov (United States)

    Da Cunha, Claudio; McKimm, Eric; Da Cunha, Rafael M; Boschen, Suelen L; Redgrave, Peter; Blaha, Charles D

    2017-07-15

    Repeated electrical stimulation of dopamine (dopamine) fibers can cause variable effects on further dopamine release; sometimes there are short-term decreases while in other cases short-term increases have been reported. Previous studies have failed to discover what factors determine in which way dopamine neurons will respond to repeated stimulation. The aim of the present study was therefore to investigate what determines the direction and magnitude of this particular form of short-term plasticity. Fixed potential amperometry was used to measure dopamine release in the nucleus accumbens in response to two trains of electrical pulses administered to the ventral tegmental area of anesthetized mice. When the pulse trains were of equal magnitude we found that low magnitude stimulation was associated with short-term suppression and high magnitude stimulation with short-term facilitation of dopamine release. Secondly, we found that the magnitude of the second pulse train was critical for determining the sign of the plasticity (suppression or facilitation), while the magnitude of the first pulse train determined the extent to which the response to the second train was suppressed or facilitated. This form of bidirectional plasticity might provide a mechanism to enhance signal-to-noise ratio of dopamine neurotransmission. Copyright © 2017 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

    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.

  12. Electrochemical sensing of hydroxylamine using a wax impregnated graphite electrode modified with a nanocomposite consisting of ferric oxide and copper hexacyanoferrate

    International Nuclear Information System (INIS)

    Allibai Mohanan, Vinu Mohan; Kacheri Kunnummal, Aswini; Biju, Valsala Madhavan Nair

    2016-01-01

    The authors describe a wax-impregnated graphite electrode modified with ferric oxide (Fe_2O_3) and copper hexacyanoferrate(II), and its application as an electrochemical sensor for hydroxylamine. The presence of Fe_2O_3 nanoparticles enhance the electron transfer kinetics and electrocatalytic activities, and also enlarge the surface area of the modified electrode. As compared to the unmodified electrode, 16.9 and 30.1 fold enhancements in amperometric response was observed for copper hexacyanoferrate(II) and the nanocomposite modified electrodes, respectively. Also, the presence of Fe_2O_3 in the nanocomposite enhances the anodic current response by 1.78 fold when compared to copper hexacyanoferrate(II) alone modified electrode. The electron transfer coefficient, electron transfer rate constant, diffusion coefficient and catalytic rate constant for the electro-oxidation of hydroxylamine were determined. Amperometry performed at a working voltage of 750 mV (vs. Ag/AgCl) revealed a detection range that extends from 0.8 μM to 100 μM, a detection limit of 0.5 μM (at an S/N ratio of 3) and a sensitivity of 0.0924 mA⋅mM"−"1. The modified electrode is remarkably stable and was successfully applied to the determination of hydroxylamine in spiked water samples. (author)

  13. MWCNT-ruthenium oxide composite paste electrode as non-enzymatic glucose sensor.

    Science.gov (United States)

    Tehrani, Ramin M A; Ab Ghani, Sulaiman

    2012-01-01

    A non-enzymatic glucose sensor of multi-walled carbon nanotube-ruthenium oxide/composite paste electrode (MWCNT-RuO(2)/CPE) was developed. The electrode was characterized by using XRD, SEM, TEM and EIS. Meanwhile, cyclic voltammetry and amperometry were used to check on the performances of the MWCNT-RuO(2)/CPE towards glucose. The proposed electrode has displayed a synergistic effect of RuO(2) and MWCNT on the electrocatalytic oxidation of glucose in 3M NaOH. This was possible via the formation of transitions of two redox pairs, viz. Ru(VI)/Ru(IV) and Ru(VII)/Ru(VI). A linear range of 0.5-50mM glucose and a limit of detection of 33 μM glucose (S/N=3) were observed. There was no significant interference observable from the traditional interferences, viz. ascorbic acid and uric acid. Indeed, results so obtained have indicated that the developed MWCNT-RuO(2)/CPE would pave the way for a better future to glucose sensor development as its fabrication was without the use of any enzyme. Copyright © 2012 Elsevier B.V. All rights reserved.

  14. Preparation and characterization of nickel oxide nanoparticles and their application in glucose and methanol sensing

    Directory of Open Access Journals (Sweden)

    Mahsa Hasanzadeh

    2015-03-01

    Full Text Available In this work, a low cost glucose and methanol nonenzymatic sensor was prepared using nickel oxide (NiO nanofilm electrodeposited on a bare Cu electrode. Electrochemical deposition was assisted with cetyl trimethylammonium bromide (CTAB as a template. Scanning electron microscopy (SEM was applied to observe the surface morphology of the modified electrode. Cyclic voltammetry (CV and amperometry techniques were used to study the electrocatalytic behavior of NiO porous film in glucose and methanol detection. For glucose sensing, the electrode showed a linear relationship in the concentration range of 0.01-2.14 mM with a low limit of detection (LOD 1.7 µM (signal/noise ratio (S/N=3. Moreover, high sensitivities of 4.02 mA mM−1 cm−2 and 0.38 mA mM−1 cm−2 respectively in glucose and methanol monitoring suggested the modified electrode as an excellent sensor. The NiO-Cu modified electrode was relatively insensitive to common biological interferers. This sensor possessed good poison resistance towards chloride ions, and long term stability and significant selectivity towards glucose and methanol. Finally the proposed sensor was successfully applied for determination of glucose in human blood serum samples.

  15. A highly sensitive electrochemical sensor for the determination of methanol based on PdNPs@SBA-15-PrEn modified electrode.

    Science.gov (United States)

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

    2018-05-01

    In this study, a novel electrochemical sensor for the determination of methanol based on palladium nanoparticles supported on Santa barbara amorphous-15- PrNHEtNH 2 (PdNPs@SBA-15-PrEn) as nanocatalysis platform is presented. Scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and electrochemical methods are employed to characterize the PdNPs@SBA-15-PrEn nanocomposite. The Nafion-Pd@SBA-15-PrEn modified glassy carbon electrode (Nafion-PdNPs@SBA-15-PrEn/GCE) displayed the high electrochemical activity and excellent catalytic characteristic for electro-oxidation of methanol in an alkaline solution. The electro-oxidation performance of the proposed sensor was investigated using cyclic voltammetry (CV) and amperometry. The sensor exhibits a good sensitivity of 0.0905 Amol -1 Lcm -2 , linear range of 20-1000 μM and the corresponding detection limit of 12 μM (3σ). The results demonstrate that the Nafion-PdNPs@SBA-15-PrEn/GCE has potential as an efficient and integrated sensor for methanol detection. Copyright © 2018 Elsevier Inc. All rights reserved.

  16. Photoelectrochemical Performances and Potential Applications of TiO2 Nanotube Arrays Modified with Ag and Pt Nanoparticles

    International Nuclear Information System (INIS)

    Xu, Guangqing; Liu, Haipeng; Wang, Jinwen; Lv, Jun; Zheng, Zhixiang; Wu, Yucheng

    2014-01-01

    TiO 2 nanotube arrays (NTAs) modified with Ag (Ag/TiO 2 ) and Pt (Pt/TiO 2 ) nanoparticles were fabricated by anodic oxidation combined with photoreduction and hydrothermal methods, respectively. Structures, element components and morphologies of TiO 2 , Ag/TiO 2 and Pt/TiO 2 NTAs were measured by X-ray diffraction diffractometer, X-ray photoelectron spectroscopy, scanning electron microscope and transmission electron microscope. The photoeletrochemical performances of TiO 2 , Pt/TiO 2 and Ag/TiO 2 NTAs were characterized by cyclic voltammetry and amperometry in phosphate buffer solution in absence and presence of glucose. Modifications of Ag and Pt nanoparticles play different roles in the photoelectrochemical process and have different potential applications. Ag nanoparticles decrease the photocurrent in buffer solution but increase the photocurrent response to organic compounds, which is fit for electrochemical detection of organic compounds due to the low background photocurrent and high photocurrent response. Ag/TiO 2 NTAs achieve the best detection performance with sensitivity of 0.152 μA/μM and detection limit of 0.53 μM. On the contrary, Pt nanoparticles can enhance the photocurrent of TiO 2 NTAs in buffer solution but decrease the photocurrent response to organic compounds, which are benefit for photocatalytic water splitting but not for photoelectrochemical detection

  17. A novel, disposable, screen-printed amperometric biosensor for glucose in serum fabricated using a water-based carbon ink.

    Science.gov (United States)

    Crouch, Eric; Cowell, David C; Hoskins, Stephen; Pittson, Robin W; Hart, John P

    2005-11-15

    Screen-printed amperometric glucose biosensors have been fabricated using a water-based carbon ink. The enzyme glucose oxidase (GOD) and the electro-catalyst cobalt phthalocyanine were mixed with the carbon ink prior to the screen-printing process; therefore, biosensors are prepared in a one-step fabrication procedure. Optimisation of the biosensor performance was achieved by studying the effects of pH, buffer strength, and applied potential on the analytical response. Calibration studies were performed under optimum conditions, using amperometry in stirred solution, with an operating potential of +500 mV versus SCE. The sensitivity was found to be 1170 nA mM(-1), with a linear range of 0.025-2 mM; the former represents the detection limit. The disposable amperometric biosensor was evaluated by carrying out replicate determinations on a sample of bovine serum. This was achieved by the method of multiple standard additions and included a correction for background currents arising from oxidizable serum components. The mean serum concentration was calculated to be 8.63 mM and compared well with the supplier's value of 8.3 mM; the coefficient of variation was calculated to be 3.3% (n=6).

  18. Midbrain Gene Screening Identifies a New Mesoaccumbal Glutamatergic Pathway and a Marker for Dopamine Cells Neuroprotected in Parkinson's Disease.

    Science.gov (United States)

    Viereckel, Thomas; Dumas, Sylvie; Smith-Anttila, Casey J A; Vlcek, Bianca; Bimpisidis, Zisis; Lagerström, Malin C; Konradsson-Geuken, Åsa; Wallén-Mackenzie, Åsa

    2016-10-20

    The ventral tegmental area (VTA) and substantia nigra pars compacta (SNc) of the midbrain are associated with Parkinson's disease (PD), schizophrenia, mood disorders and addiction. Based on the recently unraveled heterogeneity within the VTA and SNc, where glutamate, GABA and co-releasing neurons have been found to co-exist with the classical dopamine neurons, there is a compelling need for identification of gene expression patterns that represent this heterogeneity and that are of value for development of human therapies. Here, several unique gene expression patterns were identified in the mouse midbrain of which NeuroD6 and Grp were expressed within different dopaminergic subpopulations of the VTA, and TrpV1 within a small heterogeneous population. Optogenetics-coupled in vivo amperometry revealed a previously unknown glutamatergic mesoaccumbal pathway characterized by TrpV1-Cre-expression. Human GRP was strongly detected in non-melanized dopaminergic neurons within the SNc of both control and PD brains, suggesting GRP as a marker for neuroprotected neurons in PD. This study thus unravels markers for distinct subpopulations of neurons within the mouse and human midbrain, defines unique anatomical subregions within the VTA and exposes an entirely new glutamatergic pathway. Finally, both TRPV1 and GRP are implied in midbrain physiology of importance to neurological and neuropsychiatric disorders.

  19. Midbrain Gene Screening Identifies a New Mesoaccumbal Glutamatergic Pathway and a Marker for Dopamine Cells Neuroprotected in Parkinson’s Disease

    Science.gov (United States)

    Viereckel, Thomas; Dumas, Sylvie; Smith-Anttila, Casey J. A.; Vlcek, Bianca; Bimpisidis, Zisis; Lagerström, Malin C.; Konradsson-Geuken, Åsa; Wallén-Mackenzie, Åsa

    2016-01-01

    The ventral tegmental area (VTA) and substantia nigra pars compacta (SNc) of the midbrain are associated with Parkinson’s disease (PD), schizophrenia, mood disorders and addiction. Based on the recently unraveled heterogeneity within the VTA and SNc, where glutamate, GABA and co-releasing neurons have been found to co-exist with the classical dopamine neurons, there is a compelling need for identification of gene expression patterns that represent this heterogeneity and that are of value for development of human therapies. Here, several unique gene expression patterns were identified in the mouse midbrain of which NeuroD6 and Grp were expressed within different dopaminergic subpopulations of the VTA, and TrpV1 within a small heterogeneous population. Optogenetics-coupled in vivo amperometry revealed a previously unknown glutamatergic mesoaccumbal pathway characterized by TrpV1-Cre-expression. Human GRP was strongly detected in non-melanized dopaminergic neurons within the SNc of both control and PD brains, suggesting GRP as a marker for neuroprotected neurons in PD. This study thus unravels markers for distinct subpopulations of neurons within the mouse and human midbrain, defines unique anatomical subregions within the VTA and exposes an entirely new glutamatergic pathway. Finally, both TRPV1 and GRP are implied in midbrain physiology of importance to neurological and neuropsychiatric disorders. PMID:27762319

  20. Cost-effective flow injection amperometric system with metal nanoparticle loaded carbon nanotube modified screen printed carbon electrode for sensitive determination of hydrogen peroxide.

    Science.gov (United States)

    Reanpang, Preeyaporn; Themsirimongkon, Suwaphid; Saipanya, Surin; Chailapakul, Orawon; Jakmunee, Jaroon

    2015-11-01

    Various metal nanoparticles (NPs) decorated on carbon nanotube (CNT) was modified on the home-made screen printed carbon electrode (SPCE) in order to enhances sensitivity of hydrogen peroxide (H2O2) determination. The simple casting method was used for the electrode modification. The monometallic and bimetallic NPs modified electrodes were investigated for their electrochemical properties for H2O2 reduction. The Pd-CNT/SPCE is appropriated to measure the H2O2 reduction at a potential of -0.3 V, then this modified electrode was incorporated with a home-made flow through cell and applied in a simple flow injection amperometry (FI-Amp). Some parameters influencing the resulted modified electrode and the FI-Amp system were studied. The proposed detection system was able to detect H2O2 in the range of 0.1-1.0 mM, with detection limit of 20 µM. Relative standard deviation for 100 replicated injections of 0.6 mM H2O2 was 2.3%. The reproducibility of 6 electrodes preparing in 3 different lots was 8.2%. It was demonstrated for determination of H2O2 in disinfectant, hair colorant and milk samples. Recoveries in the range of 90-109% were observed. The developed system provided high stability, good repeatability, high sample throughput and low reagent consumption. Copyright © 2015 Elsevier B.V. All rights reserved.

  1. Developing an electrochemical sensor based on a carbon paste electrode modified with nano-composite of reduced graphene oxide and CuFe2O4 nanoparticles for determination of hydrogen peroxide.

    Science.gov (United States)

    Benvidi, Ali; Nafar, Mohammad Taghi; Jahanbani, Shahriar; Tezerjani, Marzieh Dehghan; Rezaeinasab, Masoud; Dalirnasab, Sudabeh

    2017-06-01

    In this paper, a highly sensitive voltammetric sensor based on a carbon paste electrode with CuFe 2 O 4 nanoparticle (RGO/CuFe 2 O 4 /CPE) was designed for determination of hydrogen peroxide (H 2 O 2 ). The electrocatalytic reduction of H 2 O 2 was examined using various techniques such as cyclic voltammetry (CV), chronoamperometry, amperometry and differential pulse voltammetry (DPV). CuFe 2 O 4 nanoparticles were synthesized by co-precipitation method and characterized with scanning electron microscopy (SEM), Transmission electron microscopy (TEM), X-ray diffraction (XRD), and Fourier transform infrared (FTIR) techniques. Then, a high conductive platform based on a carbon paste electrode modified with RGO and CuFe 2 O 4 nanoparticles was prepared as a suitable platform for determination of hydrogen peroxide. Under the optimum conditions (pH5), the modified electrode indicated a fast amperometric response of determination of hydrogen peroxide. Also, the peak current of differential pulse voltammetry (DPV) of hydrogen peroxide is increased linearly with its concentration in the ranges of 2 to 10μM and 10 to 1000μM. The obtained detection limit for hydrogen peroxide was evaluated to be 0.064μM by DPV. The designed sensor was successfully applied for the assay of hydrogen peroxide in biological and pharmaceutical samples such as milk, green tea, and hair dye cream and mouthwash solution. Copyright © 2017. Published by Elsevier B.V.

  2. Fabrication of a novel electrochemical sensor for determination of hydrogen peroxide in different fruit juice samples

    Directory of Open Access Journals (Sweden)

    Navid Nasirizadeh

    2016-01-01

    Full Text Available A new hydrogen peroxide (H2O2 sensor is fabricated based on a multiwalled carbon nanotube-modified glassy carbon electrode (MWCNT-GCE and reactive blue 19 (RB. The charge transfer coefficient, α, and the charge transfer rate constant, ks, of RB adsorbed on MWCNT-GCE were calculated and found to be 0.44 ± 0.01 Hz and 1.9 ± 0.05 Hz, respectively. The catalysis of the electroreduction of H2O2 by RB-MWCNT-GCE is described. The RB-MWCNT-GCE shows a dramatic increase in the peak current and a decrease in the overvoltage of H2O2 electroreduction in comparison with that seen at an RB modified GCE, MWCNT modified GCE, and activated GCE. The kinetic parameters such as α and the heterogeneous rate constant, k', for the reduction of H2O2 at RB-MWCNT-GCE surface were determined using cyclic voltammetry. The detection limit of 0.27μM and three linear calibration ranges were obtained for H2O2 determination at the RB-MWCNT-GCE surface using an amperometry method. In addition, using the newly developed sensor, H2O2 was determined in real samples with satisfactory results.

  3. Novel amperometric sensor using metolcarb-imprinted film as the recognition element on a gold electrode and its application

    International Nuclear Information System (INIS)

    Pan Mingfei; Fang Guozhen; Liu Bing; Qian Kun; Wang Shuo

    2011-01-01

    A molecularly imprinted film is electrochemically synthesized on a gold electrode using cyclic voltammetry to electropolymerize o-aminothiophenol in the presence of metolcarb (MTMC). The mechanism of the imprinting process and a number of factors affecting the activity of the imprinted film are discussed and optimized. Scanning electron microscope observations and binding measurements have proved that an MTMC-imprinted film (with a thickness of nearly 100 nm) was formed on the surface of the gold electrode. The film exhibited high binding affinity and selectivity towards the template MTMC, as well as good penetrability, reproducibility and stability. A novel amperometry sensor using the imprinted film as recognition element was developed for MTMC determination in food samples. Under the experimental conditions, the MTMC standard is linear within the concentration range studied (r 2 = 0.9906). The limit of detection (S/N = 3) of the modified electrode was achieved to 1.34 x 10 -8 mol L -1 . Recoveries of MTMC from spiked apple juice, cabbage and cucumber samples for the developed electrochemical assay ranged from 94.80% to 102.43%, which was with great correlation coefficient (0.9929) with results from high-performance liquid chromatography. In practical application, the prepared amperometric sensor also showed good reproducibility and long lifetime for storage. The research in this study has offered a rapid, accurate and sensitive electrochemical method for quantitative determination of MTMC in food products.

  4. Sensitive endpoint detection for coulometric titration of microgram amounts of plutonium. Part II: Use of amperometric indication for the end point detection

    International Nuclear Information System (INIS)

    Chitnis, R.T.; Talnikar, S.G.; Thakur, V.A.

    1981-01-01

    Subsequent to the work on polarized indicator electrodes in the coulometric titration of PuO 2 2+ with electrolytically generated Fe 2+ , the possibility of applying amperometry for the endpoint detection in the same titration was explored. Earlier Moiseen et al used the amperometric indication in the coulometric titration of plutonium and have reported coefficient of variation of 0.4% for the titration of 1 mg of plutonium. The lowest amount of plutonium determined was in the range of 100 micrograms. In the present method, using similar analytical technique, the titrations of 25 micrograms and lower amounts of plutonium are reported. While titrating microgram amounts using amperometric indication, the residual currents due to the supporting electrolyte affect the titrations to a considerable extent. However, it is shown that by proper choice of the potential to be applied to the indicating electrode, the interference, due to the supporting electrolyte can be minimised. Using this technique, it is possible to titrate even a fraction of a microgram of plutonium. The precision at 0.5 microgram level is found to be about 6% and that for 5 micrograms, about 1%. (author)

  5. Analogs of N-cynnamoylphenylhydroxylamine as reagents for amperometric determination of scandium

    International Nuclear Information System (INIS)

    Shvedene, N.V.; Gallaj, Z.A.; Sheina, N.M.; Zujkova, N.V.

    1978-01-01

    To decrease the detection limit of scandium and increase selectivity of amperometric determination, oxidation of 2-furylacryloyl-N-p-chlorophenylhydroxylamine (FACPhHA) and 3-styrylacryloyl-N-phenylhydroxylamine (SAPhHA) on a graphite electrode has been studied by volt-amperometry. The possibility has been established of using the oxidation current of the reagent for plotting the titration curves. The solubility of scandium complexes with FACPhHA and SAPhHA under conditions of titration against the background with pH 6.0 has been determined and equals (2.1+-0.3)x10 -6 and (5.3+-0.3)x10 -7 , respectively. The methods have been developed of amperometric determination of scandium with the use of the considered reagents against backgrounds with pH 5.5-6.5. The use of SAPhHA has decreased the limit of scandium detection down to 0.1 mgk/ml. Besides, the amperometric method makes it possible to titrate in turbid and coloured media what is an advantage of this method. The developed method is used for determination of scandium in scandium silicide

  6. A lactate electrochemical biosensor with a titanate nanotube as direct electron transfer promoter

    International Nuclear Information System (INIS)

    Yang Mingli; Wang Jin; Li Huaqing; Wu Nianqiang Nick; Zheng Jianguo

    2008-01-01

    Hydrogen titanate (H 2 Ti 3 O 7 ) nanotubes (TNTs) have been synthesized by a one-step hydrothermal processing. Lactate oxidase (LOx) enzyme has been immobilized on the three-dimensional porous TNT network to make an electrochemical biosensor for lactate detection. Cyclic voltammetry and amperometry tests reveal that the LOx enzyme, which is supported on TNTs, maintains their substrate-specific catalytic activity. The nanotubes offer the pathway for direct electron transfer between the electrode surface and the active redox centers of LOx, which enables the biosensor to operate at a low working potential and to avoid the influence of the presence of O 2 on the amperometric current response. The biosensor exhibits a sensitivity of 0.24 μA cm -2 mM -1 , a 90% response time of 5 s, and a linear response in the range from 0.5 to 14 mM and the redox center of enzyme obviates the need of redox mediators for electrochemical enzymatic sensors, which is attractive for the development of reagentless biosensors

  7. Synthesis of PtNi Alloy Nanoparticles on Graphene-Based Polymer Nanohybrids for Electrocatalytic Oxidation of Methanol

    Directory of Open Access Journals (Sweden)

    Tung-Yuan Yung

    2016-12-01

    Full Text Available We have successfully produced bimetallic PtNi alloy nanoparticles on poly(diallyldimethylammonium chloride (PDDA-modified graphene nanosheets (PtNi/PDDA-G by the “one-pot” hydrothermal method. The size of PtNi alloy nanoparticles is approximately 2–5 nm. The PDDA-modified graphene nanosheets (PDDA-G provides an anchored site for metal precursors; hence, the PtNi nanoparticles could be easily bond on the PDDA-G substrate. PtNi alloy nanoparticles (2–5 nm display a homogenous alloy phase embedded on the PDDA-G substrate, evaluated by Raman, X-ray diffractometer (XRD, thermal gravity analysis (TGA, electron surface chemical analysis (ESCA, and electron energy loss spectroscopy (EELS. The Pt/Ni ratio of PtNi alloy nanoparticles is ~1.7, examined by the energy dispersive spectroscopy (EDS spectra of transmitting electron microscopy (EDS/TEM spectra and mapping technique. The methanol electro-oxidation of PtNi/PDDA-G was evaluated by cyclic voltammetry (CV in 0.5 M of H2SO4 and 0.5 M of CH3OH. Compared to Pt on carbon nanoparticles (Pt/C and Pt on Graphene (Pt/G, the PtNi/PDDA-G exhibits the optimal electrochemical surface area (ECSA, methanol oxidation reaction (MOR activity, and durability by chrono amperometry (CA test, which can be a candidate for MOR in the electro-catalysis of direct methanol fuel cells (DMFC.

  8. Bacteria-Templated NiO Nanoparticles/Microstructure for an Enzymeless Glucose Sensor

    Directory of Open Access Journals (Sweden)

    Settu Vaidyanathan

    2016-07-01

    Full Text Available The bacterial-induced hollow cylinder NiO (HCNiO nanomaterial was utilized for the enzymeless (without GOx detection of glucose in basic conditions. The determination of glucose in 0.05 M NaOH solution with high sensitivity was performed using cyclic voltammetry (CV and amperometry (i–t. The fundamental electrochemical parameters were analyzed and the obtained values of diffusion coefficient (D, heterogeneous rate constant (ks, electroactive surface coverage (Г, and transfer coefficient (alpha-α are 1.75 × 10−6 cm2/s, 57.65 M−1·s−1, 1.45 × 10−10 mol/cm2, and 0.52 respectively. The peak current of the i–t method shows two dynamic linear ranges of calibration curves 0.2 to 3.5 µM and 0.5 to 250 µM for the glucose electro-oxidation. The Ni2+/Ni3+ couple with the HCNiO electrode and the electrocatalytic properties were found to be sensitive to the glucose oxidation. The green chemistry of NiO preparation from bacteria and the high catalytic ability of the oxyhydroxide (NiOOH is the good choice for the development of a glucose sensor. The best obtained sensitivity and limit of detection (LOD for this sensor were 3978.9 µA mM−1·cm−2 and 0.9 µM, respectively.

  9. A Fast, Sensitive and Label Free Electrochemical DNA Sensor

    International Nuclear Information System (INIS)

    Chen Yu; Elling; Lee Yokeling; Chong Serchoong

    2006-01-01

    A label free and sensitive DNA/RNA silicon based electrochemical microsensor array was developed by using thin film of the conducting polymer polypyrrole doped with an oligonucleotide probe. The electrochemical potential pulse amperometry technique was used for a biowarfare pathogen target DNA detection. The electrical potential assistanted DNA hybridisation method was applied. The sensor signal was increased by increasing the electrical potential assistanted DNA hybridisation time. It was possible to detect 0.34pmol and 0.072fmol of complementary oligonucleotide target in 0.1ml in seconds by using unpolished and polished gold electrode respectively. The probe preparation was also in seconds time, comparing indirect electrochemical DNA sensor, it has a fast sensor preparation as well as sensor response and label free advantages. The silicon microfabrication technique was used for this sensor array fabrication, which holds the potential to integrate with sensor electrical circuits. The conducting polymer polypyrrole was electrochemically deposited on each electrode respectively which has a possibility to dope the different DNA probe into the individual electrode to form a sensor array

  10. Nonenzymatic glucose sensor based on disposable pencil graphite electrode modified by copper nanoparticles

    Directory of Open Access Journals (Sweden)

    Sima Pourbeyram

    2016-10-01

    Full Text Available A nonenzymatic glucose sensor based on a disposable pencil graphite electrode (PGE modified by copper nanoparticles [Cu(NP] was prepared for the first time. The prepared Cu(NP exhibited an absorption peak centered at ∼562 nm using UV-visible spectrophotometry and an almost homogenous spherical shape by scanning electron microscopy. Cyclic voltammetry of Cu(NP-PGE showed an adsorption controlled charge transfer process up to 90.0 mVs−1. The sensor was applied for the determination of glucose using an amperometry technique with a detection limit of [0.44 (±0.01 μM] and concentration sensitivity of [1467.5 (±1.3 μA/mMcm−2]. The preparation of the Cu(NP-PGE sensor was reproducible (relative standard deviation = 2.10%, n = 10, very simple, fast, and inexpensive, and the Cu(NP-PGE is suitable to be used as a disposable glucose sensor.

  11. Electrochemistry and electrocatalysis of polyoxometalate-ordered mesoporous carbon modified electrode

    International Nuclear Information System (INIS)

    Zhou Ming; Guo Liping; Lin Fanyun; Liu Haixia

    2007-01-01

    In this work, we have developed a convenient and efficient method for the functionalization of ordered mesoporous carbon (OMC) using polyoxometalate H 6 P 2 Mo 18 O 62 .xH 2 O (P 2 Mo 18 ). By the method, glassy carbon (GC) electrode modified with P 2 Mo 18 which was immobilized on the channel surface of OMC was prepared and characterized for the first time. The large specific surface area and porous structure of the modified OMC particles result in high heteropolyacid loading, and the P 2 Mo 18 entrapped in this order matrix is stable. Fourier transform infrared spectroscopy (FTIR), nitrogen adsorption-desorption isotherm and X-ray diffraction (XRD) were employed to give insight into the intermolecular interaction between OMC and P 2 Mo 18 . The electrochemical behavior of the modified electrode was studied in detail, including pH-dependence, stability and so on. The cyclic voltammetry (CV) and amperometry studies demonstrated that P 2 Mo 18 /OMC/GC electrode has high stability, fast response and good electrocatalytic activity for the reduction of nitrite, bromate, idonate, and hydrogen peroxide. The mechanism of catalysis on P 2 Mo 18 /OMC/GC electrode was discussed. Moreover, the development of our approach for OMC functionalization suggests the potential applications in catalysis, molecular electronics and sensors

  12. Sensitive and selective electrochemical detection of chromium(VI) based on gold nanoparticle-decorated titania nanotube arrays.

    Science.gov (United States)

    Jin, Wei; Wu, Guosheng; Chen, Aicheng

    2014-01-07

    Owing to the severe toxicity and mobility of Cr(VI) in biological and environmental systems, it is of great importance to develop convenient and reliable methods for its detection. Here we report on a facile and effective electrochemical technique for monitoring Cr(VI) concentrations based on the utilization of Au nanoparticle-decorated titania nanotubes (TiO2NTs) grown on a titanium substrate. It was found that the electrochemical reduction of Cr(VI) at the Ti/TiO2NT/Au electrode exhibited an almost 23 fold improvement in activity as compared to a polycrystalline gold electrode, due to its nanoparticle/nanotubular heterojunction infrastructure. As a result, the Ti/TiO2NT/Au electrode demonstrated a wide linear concentration range from 0.10 μM to 105 μM, a low detection limit of 0.03 μM, and a high sensitivity of 6.91 μA μM(-1) Cr(VI) via amperometry, satisfying the detection requirements of the World Health Organization (WHO). Moreover, the Ti/TiO2NT/Au electrode exhibited good resistance against interference from coexisting Cr(III) and other metal ions, and excellent recovery for Cr(VI) detection in both tap and lake water samples. These attributes suggest that this hybrid sensor has strong potential in applications for the selective detection of Cr(VI).

  13. Electro-oxidation of ethanol and ethylene glycol on carbon-supported nano-Pt and -PtRu catalyst in acid solution

    International Nuclear Information System (INIS)

    Chatterjee, Moitrayee; Chatterjee, Abhik; Ghosh, Susanta; Basumallick, I.

    2009-01-01

    Present paper reports kinetics of electro-oxidation of ethanol (EtOH) and ethylene glycol (EG) onto Pt and PtRu nanocatalysts of different compositions in the temperature range of 298-318 K. These catalysts have been characterized by SEM, EDX, XRD, CV and amperometry. It has been observed that apparent activation energies for oxidation of EtOH and EG pass through a minimum at about 15-20 at.% of Ru in the PtRu alloy catalysts. Anodic peak current vs. composition curve also shows a maximum around this composition. The results have been explained by a geometric model, which proposes requirement of an ensemble of three Pt atoms with an adjacent Ru atom onto PtRu surface for an efficient electro-oxidation of EtOH or EG. This is further supported from statistical data analysis of probability of occurrence of such ensembles onto PtRu alloy surface. Present results also suggest that electro-oxidation of EG onto nano-PtRu catalyst surfaces follows a different path from that of EtOH at alloy composition less than 15 at.% of Ru.

  14. Electro-oxidation of ethanol and ethylene glycol on carbon-supported nano-Pt and -PtRu catalyst in acid solution

    Energy Technology Data Exchange (ETDEWEB)

    Chatterjee, Moitrayee; Chatterjee, Abhik; Ghosh, Susanta [Electrochemical Laboratory, Department of Chemistry, Visva-Bharati University, Santiniketan 731235 (India); Basumallick, I., E-mail: ibasumallick@yahoo.co.u [Electrochemical Laboratory, Department of Chemistry, Visva-Bharati University, Santiniketan 731235 (India)

    2009-12-01

    Present paper reports kinetics of electro-oxidation of ethanol (EtOH) and ethylene glycol (EG) onto Pt and PtRu nanocatalysts of different compositions in the temperature range of 298-318 K. These catalysts have been characterized by SEM, EDX, XRD, CV and amperometry. It has been observed that apparent activation energies for oxidation of EtOH and EG pass through a minimum at about 15-20 at.% of Ru in the PtRu alloy catalysts. Anodic peak current vs. composition curve also shows a maximum around this composition. The results have been explained by a geometric model, which proposes requirement of an ensemble of three Pt atoms with an adjacent Ru atom onto PtRu surface for an efficient electro-oxidation of EtOH or EG. This is further supported from statistical data analysis of probability of occurrence of such ensembles onto PtRu alloy surface. Present results also suggest that electro-oxidation of EG onto nano-PtRu catalyst surfaces follows a different path from that of EtOH at alloy composition less than 15 at.% of Ru.

  15. Electrochemical determination of xanthine oxidase inhibitor drug in urate lowering therapy using graphene nanosheets modified electrode

    International Nuclear Information System (INIS)

    Raj, M. Amal; John, S. Abraham

    2014-01-01

    We report the electrochemical determination of urate lowering therapeutic drug, allopurinol (AP) using the electrochemically reduced graphene oxide (ERGO) modified glassy carbon electrode (GCE). The ERGO modified GCE was fabricated by self–assembling graphene oxide (GO) on 1,6-hexadiamine (HDA) modified GCE by the electrostatic interaction between the positively charged amine group and the negatively charged GO layers followed by the electrochemical reduction of GO layers at negative potential. XPS results confirmed the attachment of GO and its electrochemical reduction. The electrochemical behavior of AP was examined at ERGO modified electrode in the presence of ascorbic acid (AA) and uric acid (UA). It was found that ERGO modified electrode not only enhanced the oxidation currents of AP, AA and UA but also showed stable signals for them for repetitive potential cycles. The present modified electrode was successfully used to determine these analytes simultaneously in a mixture. Selective determination of AP in the presence of high concentrations of AA and UA was also demonstrated at ERGO modified GCE. Using amperometry, detections of 40 and 200 nM of UA and AP were achieved and the detection limits were found to be 9.0 × 10 −9 M and 1.1 × 10 −7 M, respectively (S/N = 3). Further, the practical application of the present modified electrode was demonstrated by simultaneously determining the concentrations of AA, UA and AP in human blood serum and urine samples

  16. Effect of the electrochemical passivation on the corrosion behaviour of austenitic stainless steel

    International Nuclear Information System (INIS)

    Barbucci, A.; Delucchi, M.; Panizza, M.; Farne, G.; Cerisola, G.

    2004-01-01

    Cold rolled SS is also fruitfully used in deep drawing however the presence of scales or oxides on the surface reduces the life of the tools and emphasises creep phenomena of the material. Then a cleaning of the SS surface from these impurities is necessary. Oxides can be formed during the hot rolling preceding the cold one, or during the annealing performed between the several steps of thickness reduction. The annealing helps to decrease the work hardening occurring during the process. Normally this heat treatment is performed in reducing atmosphere of pure hydrogen (bright annealing), but even in this conditions oxides are formed on the SS surface. To avoid this uncontrolled oxide growth one method recently applied is an electrochemical cleaning performed in an electrolytic solution containing chrome, generally called electrochemical passivation. The electrochemical passivation allows the dissolution of the contaminating hard particles on the strips. Few scientific contributions are available in literature, which explain in detail the process mechanism. The aim of this work is to investigate if the electrochemical passivated surface acts in a different way with regard to corrosion phenomena with respect to conventional SS. Electrochemical measurements like polarisation, chrono-amperometries and surface analysis were used to investigate the corrosion behaviour of electrochemically passivated AISI 304L and AISI 305. The effect of some process parameters were considered, too. (authors)

  17. Effect of the electrochemical passivation on the corrosion behaviour of austenitic stainless steel

    Energy Technology Data Exchange (ETDEWEB)

    Barbucci, A.; Delucchi, M.; Panizza, M.; Farne, G.; Cerisola, G. [DICheP, University of Genova, P.le Kennedy 1, 16129 Genova (Italy)

    2004-07-01

    Cold rolled SS is also fruitfully used in deep drawing however the presence of scales or oxides on the surface reduces the life of the tools and emphasises creep phenomena of the material. Then a cleaning of the SS surface from these impurities is necessary. Oxides can be formed during the hot rolling preceding the cold one, or during the annealing performed between the several steps of thickness reduction. The annealing helps to decrease the work hardening occurring during the process. Normally this heat treatment is performed in reducing atmosphere of pure hydrogen (bright annealing), but even in this conditions oxides are formed on the SS surface. To avoid this uncontrolled oxide growth one method recently applied is an electrochemical cleaning performed in an electrolytic solution containing chrome, generally called electrochemical passivation. The electrochemical passivation allows the dissolution of the contaminating hard particles on the strips. Few scientific contributions are available in literature, which explain in detail the process mechanism. The aim of this work is to investigate if the electrochemical passivated surface acts in a different way with regard to corrosion phenomena with respect to conventional SS. Electrochemical measurements like polarisation, chrono-amperometries and surface analysis were used to investigate the corrosion behaviour of electrochemically passivated AISI 304L and AISI 305. The effect of some process parameters were considered, too. (authors)

  18. Development and application of graphite-SiO2/Al2O3/Nb2O5-methylene blue (GRP-SiAlNb-MB composite for electrochemical determination of dopamine

    Directory of Open Access Journals (Sweden)

    Juliana de Fátima Giarola

    2017-03-01

    Full Text Available In the present paper an amperometric sensor based on graphite-SiO2/Al2O3/Nb2O5-methylene blue (GRP-SiAlNb-MB composite has been successfully prepared for dopamine (DA determination in real samples. The electrochemical behavior of DA at the GRP-SiAlNb-MB has been evaluated by employing cyclic voltammetry. The best ratio (m/m of GRP-SiAlNb-MB composite was found to be 1:0.54. Under optimized conditions (pH 7.5 in 0.15 mol L−1 phosphate buffer the amperometry method responds linearly to DA from 5.0 up to 500.0 μmol L−1 (r = 0.995 with limits of detection and quantification of 1.49 and 4.97 μmol L−1, respectively. The developed method was successfully applied for DA determination in real samples of pharmaceutical formulations and can be used for routine quality control analysis of pharmaceutical formulations containing DA. The use of inorganic matrix SiAlNb was found to be very useful to adsorb MB in the composite material with further improvement of the anodic peak current of DA.

  19. Direct electrodeposition of highly ordered gold nanotube arrays for use in non-enzymatic amperometric sensing of glucose

    International Nuclear Information System (INIS)

    Tian, Taolei; Dong, Junping; Xu, Jiaqiang

    2016-01-01

    The authors describe vertically aligned gold nanotube arrays (Au-NTAs) and gold nanowire arrays (Au-NWAs) that were directly grown in alumina oxide templates by galvanostatic deposition. The morphology of the gold arrays can be controlled by adjusting the pH value of the plating bath. Scanning electron microscopy shows the nanoarrays to be highly ordered (with an average length of around 2 μm), and the opening width of the gold nanotube arrays to be uniform (with diameters of around 50 nm). The electrocatalytic activities of the Au-NTAs and Au-NWAs deposited on a glassy carbon electrode toward glucose oxidation were compared by cyclic voltammetry and amperometry at pH 7.2. The Au-NTAs yield higher amperometric currents. The respective glucose sensor, when operated at a working potential of 0.25 V (vs. SCE), exhibits a linear range that extends from 5 μM to 16.4 mM concentrations of glucose, a sensitivity of 44.2 μA mM"−"1 cm"−"2, and a detection limit of 2.1 μM (at an S/N ratio of 3). The excellent sensing performance is attributed to the large surface area and the fast electron transfer rate for the one-dimensional gold nanoarrays (author)

  20. Novel amperometric sensor using metolcarb-imprinted film as the recognition element on a gold electrode and its application

    Energy Technology Data Exchange (ETDEWEB)

    Pan Mingfei; Fang Guozhen; Liu Bing; Qian Kun [Key Laboratory of Food Nutrition and Safety, Ministry of Education of China, Tianjin University of Science and Technology, Tianjin 300457 (China); Wang Shuo, E-mail: pmf2006@126.com [Key Laboratory of Food Nutrition and Safety, Ministry of Education of China, Tianjin University of Science and Technology, Tianjin 300457 (China)

    2011-04-01

    A molecularly imprinted film is electrochemically synthesized on a gold electrode using cyclic voltammetry to electropolymerize o-aminothiophenol in the presence of metolcarb (MTMC). The mechanism of the imprinting process and a number of factors affecting the activity of the imprinted film are discussed and optimized. Scanning electron microscope observations and binding measurements have proved that an MTMC-imprinted film (with a thickness of nearly 100 nm) was formed on the surface of the gold electrode. The film exhibited high binding affinity and selectivity towards the template MTMC, as well as good penetrability, reproducibility and stability. A novel amperometry sensor using the imprinted film as recognition element was developed for MTMC determination in food samples. Under the experimental conditions, the MTMC standard is linear within the concentration range studied (r{sup 2} = 0.9906). The limit of detection (S/N = 3) of the modified electrode was achieved to 1.34 x 10{sup -8} mol L{sup -1}. Recoveries of MTMC from spiked apple juice, cabbage and cucumber samples for the developed electrochemical assay ranged from 94.80% to 102.43%, which was with great correlation coefficient (0.9929) with results from high-performance liquid chromatography. In practical application, the prepared amperometric sensor also showed good reproducibility and long lifetime for storage. The research in this study has offered a rapid, accurate and sensitive electrochemical method for quantitative determination of MTMC in food products.

  1. Carbon Fiber Ultramicrodic Electrode Electrodeposited with Over-Oxidized Polypyrrole for Amperometric Detection of Vesicular Exocytosis from Pheochromocytoma Cell

    Directory of Open Access Journals (Sweden)

    Li Wang

    2015-01-01

    Full Text Available Vesicular exocytosis is ubiquitous, but it is difficult to detect within the cells’ communication mechanism. For this purpose, a 2 µm ultramicrodic carbon fiber electrode was fabricated in this work based on electrodeposition with over-oxidized polypyrrole nanoparticle (PPyox-CFE, which was applied successfully for real-time monitoring of quantal exocytosis from individual pheochromocytoma (PC12 cells. PPyox-CFE was evaluated by dopamine (DA solutions through cyclic voltammetry and amperometry electrochemical methods, and results revealed that PPyox-CFE improved the detection limit of DA. In particular, the sensitivity of DA was improved to 24.55 µA·µM−1·µm−2 using the PPyox-CFE. The ultramicrodic electrode combined with the patch-clamp system was used to detect vesicular exocytosis of DA from individual PC12 cells with 60 mM K+ stimulation. A total of 287 spikes released from 7 PC12 cells were statistically analyzed. The current amplitude (Imax and the released charge (Q of the amperometric spikes from the DA release by a stimulated PC12 cell is 45.1 ± 12.5 pA and 0.18 ± 0.04 pC, respectively. Furthermore, on average ~562,000 molecules were released in each vesicular exocytosis. PPyox-CFE, with its capability of detecting vesicular exocytosis, has potential application in neuron communication research.

  2. Ion chromatographic analysis of high specific activity 18FDG preparations and detection of the chemical impurity 2-deoxy-2-chloro-D-glucose

    International Nuclear Information System (INIS)

    Alexoff, D.L.; Casati, R.; Fowler, J.S.; Wolf, A.P.; Shea, C.; Schlyer, D.J.; Chyng-Yann Shiue

    1992-01-01

    Because of the widespread use of 2-deoxy-2-[ 18 F]fluoro-D-glucose(FDG) prepared by the ''Julich'' method or its variants it was decided necessary to determine the major chemical impurities present in the final product. An analytical system for quantifying FDG was developed using pulsed amperometry after separation by high-performance anion exchange chromotography. With this system a heretofore unidentified impurity, 2-deoxy-2-chloro-D-glucose(C1DG) was found in our preparation and in those from other laboratories using the ''Julich'' method. C1DG arises from C1 - ion displacement during the labeling procedure where C1 - ion comes from several sources, and C1 - ion displacement from the HC1 used in the hydrolysis step. FDG mass was present in the same preparations at a level of ca 1-40 μg. Other major chemical constituents were glucose (ca 1-6 mg) and mannose (ca 10-18 μg). Glycerol, arising from sterilizing filters, was also detected in most preparations. Although C1DG is a chemical impurity which has not been detected previously in nca FDG preparations, its biochemical and pharmacological properties are similar to FDG and 2-deoxy-D-glucose. Thus it is unlikely that the presence of small quantities of C1DG found in typical FDG preparations (ca 100 μg) would have adverse pharmacological or toxicological consequences that would limit continued application of this radiopharmaceutical in basic and clinical studies. (Author)

  3. Electrochemical quantification of the antioxidant capacity of medicinal plants using biosensors.

    Science.gov (United States)

    Rodríguez-Sevilla, Erika; Ramírez-Silva, María-Teresa; Romero-Romo, Mario; Ibarra-Escutia, Pedro; Palomar-Pardavé, Manuel

    2014-08-08

    The working area of a screen-printed electrode, SPE, was modified with the enzyme tyrosinase (Tyr) using different immobilization methods, namely entrapment with water-soluble polyvinyl alcohol (PVA), cross-linking using glutaraldehyde (GA), and cross-linking using GA and human serum albumin (HSA); the resulting electrodes were termed SPE/Tyr/PVA, SPE/Tyr/GA and SPE/Tyr/HSA/GA, respectively. These biosensors were characterized by means of amperometry and EIS techniques. From amperometric evaluations, the apparent Michaelis-Menten constant, Km', of each biosensor was evaluated while the respective charge transfer resistance, Rct, was assessed from impedance measurements. It was found that the SPE/Tyr/GA had the smallest Km' (57 ± 7) µM and Rct values. This electrode also displayed both the lowest detection and quantification limits for catechol quantification. Using the SPE/Tyr/GA, the Trolox Equivalent Antioxidant Capacity (TEAC) was determined from infusions prepared with "mirto" (Salvia microphylla), "hHierba dulce" (Lippia dulcis) and "salve real" (Lippia alba), medicinal plants commonly used in Mexico.

  4. Enterochromaffin cells of the human gut: sensors for spices and odorants.

    Science.gov (United States)

    Braun, Thomas; Voland, Petra; Kunz, Lars; Prinz, Christian; Gratzl, Manfred

    2007-05-01

    Release of serotonin from mucosal enterochromaffin cells triggered by luminal substances is the key event in the regulation of gut motility and secretion. We were interested to know whether nasal olfactory receptors are also expressed in the human gut mucosa by enterochromaffin cells and whether their ligands and odorants present in spices, fragrances, detergents, and cosmetics cause serotonin release. Receptor expression was studied by the reverse-transcription polymerase chain reaction method in human mucosal enterochromaffin cells isolated by laser microdissection and in a cell line derived from human enterochromaffin cells. Activation of the cells by odorants was investigated by digital fluorescence imaging using the fluorescent Ca(2+) indicator Fluo-4. Serotonin release was measured in culture supernatants by a serotonin enzyme immunoassay and amperometry using carbon fiber microelectrodes placed on single cells. We found expression of 4 olfactory receptors in microdissected human mucosal enterochromaffin cells and in a cell line derived from human enterochromaffin cells. Ca(2+) imaging studies revealed that odorant ligands of the identified olfactory receptors cause Ca(2+) influx, elevation of intracellular free Ca(2+) levels, and, consequently, serotonin release. Our results show that odorants present in the luminal environment of the gut may stimulate serotonin release via olfactory receptors present in human enterochromaffin cells. Serotonin controls both gut motility and secretion and is implicated in pathologic conditions such as vomiting, diarrhea, and irritable bowel syndrome. Thus, olfactory receptors are potential novel targets for the treatment of gastrointestinal diseases and motility disorders.

  5. Cerebellar modulation of frontal cortex dopamine efflux in mice: relevance to autism and schizophrenia.

    Science.gov (United States)

    Mittleman, Guy; Goldowitz, Daniel; Heck, Detlef H; Blaha, Charles D

    2008-07-01

    Cerebellar and frontal cortical pathologies have been commonly reported in schizophrenia, autism, and other developmental disorders. Whether there is a relationship between prefrontal and cerebellar pathologies is unknown. Using fixed potential amperometry, dopamine (DA) efflux evoked by cerebellar or, dentate nucleus electrical stimulation (50 Hz, 200 muA) was recorded in prefrontal cortex of urethane anesthetized lurcher (Lc/+) mice with 100% loss of cerebellar Purkinje cells and wildtype (+/+) control mice. Cerebellar stimulation with 25 and 100 pulses evoked prefrontal cortex DA efflux in +/+ mice that persisted for 12 and 25 s poststimulation, respectively. In contrast, 25 pulse cerebellar stimulation failed to evoke prefrontal cortex DA efflux in Lc/+ mice indicating a dependency on cerebellar Purkinje cell outputs. Dentate nucleus stimulation (25 pulses) evoked a comparable but briefer (baseline recovery within 7 s) increase in prefrontal cortex DA efflux compared to similar cerebellar stimulation in +/+ mice. However, in Lc/+ mice 25 pulse dentate nucleus evoked prefrontal cortex DA efflux was attenuated by 60% with baseline recovery within 4 s suggesting that dentate nucleus outputs to prefrontal cortex remain partially functional. DA reuptake blockade enhanced 100 pulse stimulation evoked prefrontal cortex responses, while serotonin or norepinephrine reuptake blockade were without effect indicating the specificity of the amperometric recordings to DA. Results provide neurochemical evidence that the cerebellum can modulate DA efflux in the prefrontal cortex. Together, these findings may explain why cerebellar and frontal cortical pathologies co-occur, and may provide a mechanism that accounts for the diversity of symptoms common to multiple developmental disorders.

  6. Characterization of electrogenerated polypyrrole-benzophenone films coated on poly(pyrrole-methyl metacrylate) optic-conductive fibers.

    Science.gov (United States)

    Abu-Rabeah, Khalil; Atias, Danit; Herrmann, Sebastien; Frenkel, Julia; Tavor, Dorith; Cosnier, Serge; Marks, Robert S

    2009-09-01

    A conductive surface was created for the development of a biosensing platform via chemical polymerization of pyrrole onto the surface of poly(methyl methacrylate) (PMMA) fibers, with a subsequent electrogeneration of a photoactive linker pyrrole-benzophenone (PyBz) monomer on the fiber surface. Irradiation of the benzophenone groups embedded in the polypyrrole (Ppy) films by UV (350 nm) formed active radicals, allowing covalent attachment of the desired biomaterials. Characterization and optimization of this platform were carried out, with the platform showing conductive, stable, thin, controllable, and light-transmissible film features. Various parameters such as time deposition, process temperature, and activator plus pyrrole monomer concentrations were examined in the study. The morphology and permeability of the optic-fiber PMMA fibers were investigated to examine mass transfer ability. Cyclic voltammetry and amperometry techniques were applied to characterize the electrical features of the surface and charge transfer. The platform potential was then demonstrated by the construction of both amperometric and optical biosensors.

  7. Preparation and characterization of AuNPs/CNTs-ErGO electrochemical sensors for highly sensitive detection of hydrazine.

    Science.gov (United States)

    Zhao, Zhenting; Sun, Yongjiao; Li, Pengwei; Zhang, Wendong; Lian, Kun; Hu, Jie; Chen, Yong

    2016-09-01

    A highly sensitive electrochemical sensor of hydrazine has been fabricated by Au nanoparticles (AuNPs) coating of carbon nanotubes-electrochemical reduced graphene oxide composite film (CNTs-ErGO) on glassy carbon electrode (GCE). Cyclic voltammetry and potential amperometry have been used to investigate the electrochemical properties of the fabricated sensors for hydrazine detection. The performances of the sensors were optimized by varying the CNTs to ErGO ratio and the quantity of Au nanoparticles. The results show that under optimal conditions, a sensitivity of 9.73μAμM(-1)cm(-2), a short response time of 3s, and a low detection limit of 0.065μM could be achieved with a linear concentration response range from 0.3μM to 319μM. The enhanced electrochemical performances could be attributed to the synergistic effect between AuNPs and CNTs-ErGO film and the outstanding catalytic effect of the Au nanoparticles. Finally, the sensor was successfully used to analyse the tap water, showing high potential for practical applications. Copyright © 2016 Elsevier B.V. All rights reserved.

  8. A nano-structured Ni(II)-chelidamic acid modified gold nanoparticle self-assembled electrode for electrocatalytic oxidation and determination of methanol

    Energy Technology Data Exchange (ETDEWEB)

    Gholivand, Mohammad Bagher, E-mail: mbgholivand@yahoo.com [Department of Analytical Chemistry, Faculty of Chemistry, Razi University, Kermanshah (Iran, Islamic Republic of); Azadbakht, Azadeh [Department of Chemistry, Faculty of Basic Science, Khorramabad Branch, Islamic Azad University, Khorramabad (Iran, Islamic Republic of)

    2012-10-01

    A nano-structured Ni(II)-chelidamic acid (2,6-dicarboxy-4-hydroxypyridine) film was electrodeposited on a gold nanoparticle-cysteine-gold electrode. The morphology of Ni(II)-chelidamic acid gold nanoparticle self-assembled electrode was investigated by scanning electron microscopy (SEM). Electrocatalytic oxidation of methanol on the surface of modified electrode was studied by cyclic voltammetry and chronoamperometry methods. The hydrodynamic amperometry at a rotating modified electrode at constant potential versus reference electrode was used for detection of methanol. Under optimized conditions the calibration plots are linear in the concentration range 0-50 mM with a detection limit of 15 {mu}M. The formed matrix in our work possessed a 3D porous network structure with a large effective surface area, high catalytic activity and behaved like microelectrode ensembles. The modified electrode indicated reproducible behavior and a high level stability during the experiments, making it particularly suitable for analytical purposes. - Highlights: Black-Right-Pointing-Pointer The Au electrode modified with thin Ni(II)/CHE-AuNP film shows stable and reproducible behavior. Black-Right-Pointing-Pointer Long stability and excellent electrochemical reversibility were observed. Black-Right-Pointing-Pointer This modified electrode shows excellent catalytic activity for methanol oxidation. Black-Right-Pointing-Pointer Combination of unique properties of AuNP and Ni(II)/CHE resulted in improvement of current responses.

  9. A 200-Channel Area-Power-Efficient Chemical and Electrical Dual-Mode Acquisition IC for the Study of Neurodegenerative Diseases.

    Science.gov (United States)

    Guo, Jing; Ng, Waichiu; Yuan, Jie; Li, Suwen; Chan, Mansun

    2016-06-01

    Microelectrode array (MEA) can be used in the study of neurodegenerative diseases by monitoring the chemical neurotransmitter release and the electrical potential simultaneously at the cellular level. Currently, the MEA technology is migrating to more electrodes and higher electrode density, which raises power and area constraints on the design of acquisition IC. In this paper, we report the design of a 200-channel dual-mode acquisition IC with highly efficient usage of power and area. Under the constraints of target noise and fast settling, the current channel design saves power by including a novel current buffer biased in discrete time (DT) before the TIA (transimpedance amplifier). The 200 channels are sampled at 20 kS/s and quantized by column-wise SAR ADCs. The prototype IC was fabricated in a 0.18 μm CMOS process. Silicon measurements show the current channel has 21.6 pArms noise with cyclic voltammetry (CV) and 0.48 pArms noise with constant amperometry (CA) while consuming 12.1 μW . The voltage channel has 4.07 μVrms noise in the bandwidth of 100 kHz and 0.2% nonlinearity while consuming 9.1 μW. Each channel occupies 0.03 mm(2) area, which is among the smallest.

  10. Wireless Instantaneous Neurotransmitter Concentration Sensing System (WINCS) for intraoperative neurochemical monitoring.

    Science.gov (United States)

    Kimble, Christopher J; Johnson, David M; Winter, Bruce A; Whitlock, Sidney V; Kressin, Kenneth R; Horne, April E; Robinson, Justin C; Bledsoe, Jonathan M; Tye, Susannah J; Chang, Su-Youne; Agnesi, Filippo; Griessenauer, Christoph J; Covey, Daniel; Shon, Young-Min; Bennet, Kevin E; Garris, Paul A; Lee, Kendall H

    2009-01-01

    The Wireless Instantaneous Neurotransmitter Concentration Sensing System (WINCS) measures extracellular neurotransmitter concentration in vivo and displays the data graphically in nearly real time. WINCS implements two electroanalytical methods, fast-scan cyclic voltammetry (FSCV) and fixed-potential amperometry (FPA), to measure neurotransmitter concentrations at an electrochemical sensor, typically a carbon-fiber microelectrode. WINCS comprises a battery-powered patient module and a custom software application (WINCSware) running on a nearby personal computer. The patient module impresses upon the electrochemical sensor either a constant potential (for FPA) or a time-varying waveform (for FSCV). A transimpedance amplifier converts the resulting current to a signal that is digitized and transmitted to the base station via a Bluetooth radio link. WINCSware controls the operational parameters for FPA or FSCV, and records the transmitted data stream. Filtered data is displayed in various formats, including a background-subtracted plot of sequential FSCV scans - a representation that enables users to distinguish the signatures of various analytes with considerable specificity. Dopamine, glutamate, adenosine and serotonin were selected as analytes for test trials. Proof-of-principle tests included in vitro flow-injection measurements and in vivo measurements in rat and pig. Further testing demonstrated basic functionality in a 3-Tesla MRI unit. WINCS was designed in compliance with consensus standards for medical electrical device safety, and it is anticipated that its capability for real-time intraoperative monitoring of neurotransmitter release at an implanted sensor will prove useful for advancing functional neurosurgery.

  11. Design of a new hypoxanthine biosensor: xanthine oxidase modified carbon film and multi-walled carbon nanotube/carbon film electrodes.

    Science.gov (United States)

    Torres, A Carolina; Ghica, M Emilia; Brett, Christopher M A

    2013-04-01

    A new and simple-to-prepare hypoxanthine biosensor has been developed using xanthine oxidase (XOD) immobilised on carbon electrode surfaces. XOD was immobilised by glutaraldehyde cross-linking on carbon film (CF) electrodes and on carbon nanotube (CNT) modified CF (CNT/CF). A comparison of the performance of the two configurations was carried out by the current response using amperometry at fixed potential; the best characteristics being exhibited by XOD/CNT/CF modified electrodes. The effects of electrolyte pH and applied potential were evaluated, and a proposal is made for the enzyme mechanism of action involving competition between regeneration of flavin adenine dinucleotide and reduction of hydrogen peroxide. Under optimised conditions, the determination of hypoxanthine was carried out at -0.2 V vs. a saturated calomel electrode (SCE) with a detection limit of 0.75 μM on electrodes with CNT and at -0.3 V vs. SCE with a detection limit of 0.77 μM on electrodes without CNT. The applicability of the biosensor was verified by performing an interference study, reproducibility and stability were investigated, and hypoxanthine was successfully determined in sardine and shrimp samples.

  12. Characterization of palladium nanoparticles anchored on graphene oxide obtained by electron beam

    Energy Technology Data Exchange (ETDEWEB)

    Sobrinho, Luiza F.; Garcia, Rafael H.L.; Silva, Flávia R.O.; Neto, Almir O.; Sakata, Solange K., E-mail: lunnaquimica@usp.br, E-mail: sksakata@ipen.br [Instituto de Pesquisas Energéticas e Nucleares (IPEN/CNEN-SP), São Paulo, SP (Brazil)

    2017-07-01

    Fuel Cells (FCs) are devices that convert chemical energy directly in electrical and thermal energy. There are two disadvantages in the process that difficult the implementation of these new power supply. The fuel, hydrogen, is highly flammable and it is difficult to transport and the catalyst is costly. FCs have been attracting worldwide attention because they are environmental friendly and potential as clean and efficient power source. However, their durability and cost have being identified as important issues in this power supply. The objective of this work is to provide a new material based on incorporation of palladium graphene oxide as catalyst. Graphene Oxide (GO) was synthesized from graphite by the modified Hummers method, in water/alcohol medium. The one-step method to incorporate nanoparticles on this nanomaterial was developed using by electron beam (EB). Additionally, this method also reduces the Graphene Oxide (GO). This nanocomposite were characterized by thermogravimetry (TG), Fourier transform infrared (FT-IR), transmission electron microscopy (TEM), x-rays diffraction (XRD) and its potential for electro catalysis were performed by cyclic voltammetry (CV) and amperometry (CA). The results showed that the incorporation of Pd on reduced GO (rGO) by electron beam was 20-40 % in mass. The process using EB and Pd nanoparticles supported on graphene oxide as a support are an alternative, in substitution of conventional methods to the production of electrodes for fuel cells. (author)

  13. Characterization of palladium nanoparticles anchored on graphene oxide obtained by electron beam

    International Nuclear Information System (INIS)

    Sobrinho, Luiza F.; Garcia, Rafael H.L.; Silva, Flávia R.O.; Neto, Almir O.; Sakata, Solange K.

    2017-01-01

    Fuel Cells (FCs) are devices that convert chemical energy directly in electrical and thermal energy. There are two disadvantages in the process that difficult the implementation of these new power supply. The fuel, hydrogen, is highly flammable and it is difficult to transport and the catalyst is costly. FCs have been attracting worldwide attention because they are environmental friendly and potential as clean and efficient power source. However, their durability and cost have being identified as important issues in this power supply. The objective of this work is to provide a new material based on incorporation of palladium graphene oxide as catalyst. Graphene Oxide (GO) was synthesized from graphite by the modified Hummers method, in water/alcohol medium. The one-step method to incorporate nanoparticles on this nanomaterial was developed using by electron beam (EB). Additionally, this method also reduces the Graphene Oxide (GO). This nanocomposite were characterized by thermogravimetry (TG), Fourier transform infrared (FT-IR), transmission electron microscopy (TEM), x-rays diffraction (XRD) and its potential for electro catalysis were performed by cyclic voltammetry (CV) and amperometry (CA). The results showed that the incorporation of Pd on reduced GO (rGO) by electron beam was 20-40 % in mass. The process using EB and Pd nanoparticles supported on graphene oxide as a support are an alternative, in substitution of conventional methods to the production of electrodes for fuel cells. (author)

  14. Investigation of reaction mechanisms during electroreduction of carbon dioxide on lead electrode for the production of organic compounds

    International Nuclear Information System (INIS)

    Innocent, B.

    2008-09-01

    The aim of this work was to promote the reduction of CO 2 through its electrochemical conversion (electro-synthesis) on a lead electrode into high added value products. Depending on the nature of electrolyte, the electro-reduction of carbon dioxide leads to different products. Various electrolytes (aqueous or organic, protic or aprotic) were used to study two mechanisms: hydrogenation (formation of formate) and electro-dimerization (synthesis of oxalate). Cyclic voltammetry studies have been carried out for electrochemically characterizing CO 2 reduction on Pb. The electrochemical investigation of the electrode electrolyte interface has shown that the process of CO 2 electro-reduction is a mass transfer control both in the organic and aqueous media. Electrochemical experiments (cyclic voltammetry, chrono-amperometry) coupled with in situ infrared reflectance spectroscopic techniques (SPAIRS, SNIFTIRS) have also shown that in aqueous medium (7 ≤pH≤9) hydrogeno-carbonate ions were reduced to formate. The modification of solvent (propylene carbonate) leads selectively to oxalate as the main reaction product. Long-term electrolyses were performed in a filter-press cell to deal large volumes. In aqueous medium, the reduction of HCO 3 - to HCOO - (R F = 89% at -2.5 mA cm -2 and 4 C) is always accompanied by the production of H 2 . (author)

  15. Amperometric Determination of Sulfite by Gas Diffusion- Sequential Injection with Boron-Doped Diamond Electrode

    Directory of Open Access Journals (Sweden)

    Orawon Chailapakul

    2008-03-01

    Full Text Available A gas diffusion sequential injection system with amperometric detection using aboron-doped diamond electrode was developed for the determination of sulfite. A gasdiffusion unit (GDU was used to prevent interference from sample matrices for theelectrochemical measurement. The sample was mixed with an acid solution to generategaseous sulfur dioxide prior to its passage through the donor channel of the GDU. Thesulfur dioxide diffused through the PTFE hydrophobic membrane into a carrier solution of 0.1 M phosphate buffer (pH 8/0.1% sodium dodecyl sulfate in the acceptor channel of theGDU and turned to sulfite. Then the sulfite was carried to the electrochemical flow cell anddetected directly by amperometry using the boron-doped diamond electrode at 0.95 V(versus Ag/AgCl. Sodium dodecyl sulfate was added to the carrier solution to preventelectrode fouling. This method was applicable in the concentration range of 0.2-20 mgSO32−/L and a detection limit (S/N = 3 of 0.05 mg SO32−/L was achieved. This method wassuccessfully applied to the determination of sulfite in wines and the analytical resultsagreed well with those obtained by iodimetric titration. The relative standard deviations forthe analysis of sulfite in wines were in the range of 1.0-4.1 %. The sampling frequency was65 h−1.

  16. Direct detection of ammonium ion by means of oxygen electrocatalysis at a copper-polyaniline composite on a screen-printed electrode

    International Nuclear Information System (INIS)

    Zhybak, Mykhailo T.; Vagin, Mikhail Yu.; Beni, Valerio; Liu, Xianjie; Turner, Anthony P. F.; Dempsey, Eithne; Korpan, Yaroslav I.

    2016-01-01

    We describe a composite material for use in electrochemical oxygen reduction. A screen-printed electrode (SPE) was consecutively modified with electrodeposited copper, a Nafion membrane and electropolymerized polyaniline (PANi) to give an electrocatalytic composite of type PANi/Nafion/Cu_2O/SPE that displays good electrical conductivity at neutral pH values. It is found that the presence of ammonia causes complex formation with Cu(I), and this causes electroreduction of oxygen to result in an increased cathodic current. The finding was applied to the quantification of ammonium ions in the 1 to 1000 μM concentration range by amperometry at −0.45 V (vs. Ag/AgCl). This Faradaic phenomenon offers the advantage of direct voltammetric detection, one of the lowest known limits of detection (0.5 μM), and high sensitivity (250 mA∙M"−"1∙cm"−"2). It was applied to the determination of ammonium ion in human serum where it compared well with the photometric routine approach for clinical analysis using glutamate dehydrogenase. (author)

  17. A Micro-Platinum Wire Biosensor for Fast and Selective Detection of Alanine Aminotransferase

    Directory of Open Access Journals (Sweden)

    Tran Nguyen Thanh Thuy

    2016-05-01

    Full Text Available In this study, a miniaturized biosensor based on permselective polymer layers (overoxidized polypyrrole (Ppy and Nafion® modified and enzyme (glutamate oxidase (GlutOx immobilized micro-platinum wire electrode for the detection of alanine aminotransferase (ALT was fabricated. The proposed ALT biosensor was measured electrochemically by constant potential amperometry at +0.7 V vs. Ag/AgCl. The ALT biosensor provides fast response time (~5 s and superior selectivity towards ALT against both negatively and positively charged species (e.g., ascorbic acid (AA and dopamine (DA, respectively. The detection range of the ALT biosensor is found to be 10–900 U/L which covers the range of normal ALT levels presented in the serum and the detection limit and sensitivity are found to be 8.48 U/L and 0.059 nA/(U/L·mm2 (N = 10, respectively. We also found that one-day storage of the ALT biosensor at −20 °C right after the sensor being fabricated can enhance the sensor sensitivity (1.74 times higher than that of the sensor stored at 4 °C. The ALT biosensor is stable after eight weeks of storage at −20 °C. The sensor was tested in spiked ALT samples (ALT activities: 20, 200, 400, and 900 U/L and reasonable recoveries (70%~107% were obtained.

  18. A highly sensitive NADH sensor based on a mycelium-like nanocomposite using graphene oxide and multi-walled carbon nanotubes to co-immobilize poly(luminol) and poly(neutral red) hybrid films.

    Science.gov (United States)

    Chiang Lin, Kuo; Yu Lai, Szu; Ming Chen, Shen

    2014-08-21

    Hybridization of poly(luminol) (PLM) and poly(neutral red) (PNR) has been successfully performed and further enhanced by a conductive and steric hybrid nanotemplate using graphene oxide (GO) and multi-walled carbon nanotubes (MWCNTs). The morphology of the PLM-PNR-MWCNT-GO mycelium-like nanocomposite is studied by SEM and AFM and it is found to be electroactive, pH-dependent, and stable in the electrochemical system. It shows electrocatalytic activity towards NADH with a high current response and low overpotential. Using amperometry, it has been shown to have a high sensitivity of 288.9 μA mM(-1) cm(-2) to NADH (Eapp. = +0.1 V). Linearity is estimated in a concentration range of 1.33 × 10(-8) to 1.95 × 10(-4) M with a detection limit of 1.33 × 10(-8) M (S/N = 3). Particularly, it also shows another linear range of 2.08 × 10(-4) to 5.81 × 10(-4) M with a sensitivity of 151.3 μA mM(-1) cm(-2). The hybridization and activity of PLM and PNR can be effectively enhanced by MWCNTs and GO, resulting in an active hybrid nanocomposite for determination of NADH.

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

    Science.gov (United States)

    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. © 2013 Elsevier B.V. All rights reserved.

  20. Electrochemistry and biosensing reactivity of heme proteins adsorbed on the structure-tailored mesoporous Nb2O5 matrix

    International Nuclear Information System (INIS)

    Xu Xin; Tian Bozhi; Zhang Song; Kong Jilie; Zhao Dongyuan; Liu Baohong

    2004-01-01

    The highly ordered mesoporous niobium oxides fabricated by self-adjusted synthesis have been used as immobilization matrices of heme proteins including Cytochrome c (Cyt C) and horseradish peroxidase (HRP) for their large surface areas, narrow pore size distributions and good biocompatibility. The assembling process was investigated by cyclic voltammetry, amperometry and potential step chronoamperometry in details. Niobium oxide matrices with different structural features were templated with the surfactants and the selectivity of these hosts to specific protein characteristics was determined. It was observed that proteins could be readily assembled onto the mesoporous films with detectable retention of bioactivity. The Nb 2 O 5 matrix with a tailored pore size and counterpoised surface charge to that of hemes allowed for a maximum adsorption capacity of biomolecules. The adsorbed redox molecules exhibited direct electrochemical behavior and gave a pair of well-defined quasi-reversible cyclic voltammetric peaks, indicating that the mesoporous niobium oxide matrix could effectively promote the direct electron transfer between the protein redox site adsorbed and the electrode surface. The midpoint redox potentials of adsorbed Cyt-c and HRP were 14 and -122 mV versus SCE, respectively. Furthermore, the immobilized HRP onto Nb 2 O 5 derived electrode presented good bioactivity and thus was fabricated as an amperometric biosensor for the response of hydrogen peroxide in the range from 0.1 μM to 0.1 mM

  1. Direct electrochemistry of hemoglobin and biosensing for hydrogen peroxide using a film containing silver nanoparticles and poly(amidoamine) dendrimer

    Energy Technology Data Exchange (ETDEWEB)

    Baccarin, Marina [Nanomedicine and Nanotoxicology Group, Instituto de Física de São Carlos, Universidade de São Paulo, 13566-390 São Carlos, SP (Brazil); Departamento de Química, Universidade Federal de São Carlos, 13565-970 São Carlos, SP (Brazil); Janegitz, Bruno C., E-mail: brunocj@ymail.com [Departamento de Química, Universidade Federal de São Carlos, 13565-970 São Carlos, SP (Brazil); Departamento de Ciências da Natureza, Matemática e Educação, Universidade Federal de São Carlos, 13600-970 Araras, SP (Brazil); Berté, Rodrigo [Nanomedicine and Nanotoxicology Group, Instituto de Física de São Carlos, Universidade de São Paulo, 13566-390 São Carlos, SP (Brazil); Vicentini, Fernando Campanhã [Departamento de Química, Universidade Federal de São Carlos, 13565-970 São Carlos, SP (Brazil); Banks, Craig E. [Faculty of Science and Engineering, School of Chemistry and the Environment, Division of Chemistry and Environmental Science, Manchester Metropolitan University, Chester Street, Manchester M15GD (United Kingdom); Fatibello-Filho, Orlando [Departamento de Química, Universidade Federal de São Carlos, 13565-970 São Carlos, SP (Brazil); and others

    2016-01-01

    A new architecture for a biosensor is proposed using a glassy carbon electrode (GCE) modified with hemoglobin (Hb) and silver nanoparticles (AgNPs) encapsulated in poly(amidoamine) dendrimer (PAMAM). The biosensors were characterized using ultraviolet–visible spectroscopy, ζ-potential and cyclic voltammetry to investigate the interactions between Hb, AgNPs and the PAMAM film. The biosensor exhibited a well-defined cathodic peak attributed to reduction of the Fe{sup 3+} present in the heme group in Hb, as revealed by cyclic voltammetry in the presence of O{sub 2}. An apparent heterogeneous electron transfer rate of 4.1 s{sup −1} was obtained. The Hb–AgNPs-PAMAM/GCE third generation biosensor was applied in the amperometric determination of hydrogen peroxide over the linear range from 6.0 × 10{sup −6} to 9.1 × 10{sup −5} mol L{sup −1} with a detection limit of 4.9 × 10{sup −6} mol L{sup −1}. The proposed method can be extended to immobilize and evaluate the direct electron transfer of other redox enzymes. - Highlights: • A new architecture for biosensor using Hb, AgNPs and PAMAM is proposed. • H{sub 2}O{sub 2} is determined by amperometry using the proposed third generation biosensor. • The direct electron transfer was obtained from Hb using Hb–AgNPs–PAMAM.

  2. The electrocatalytic activity of a supramolecular assembly of CoTsPc/FeT4MPyP on multi-walled carbon nanotubes towards L-glutathione, and its determination in human erythrocytes

    International Nuclear Information System (INIS)

    Luz, R.C.S.; Maroneze, C.M.; Tanaka, A.A.; Kubota, L.T.; Gushikem, Y.; Damos, F.S.

    2010-01-01

    The electrocatalytic activity of a supramolecular complex based on cobalt(II) phthalocyanine tetrasulfonate and iron(III) tetra-(N-methyl-4-pyridyl)-porphyrin adsorbed on multi-walled carbon nanotubes for the oxidation of L-glutathione (GSH) was investigated at pH 7.4. Scanning electron microscopy and energy dispersive X-ray spectrometry were used to characterize the morphologies and composition of the materials. The modified electrode displayed efficient electrocatalytic activity in terms of oxidation of GSH at an oxidation potential of 0 V (versus Ag/AgCl). Cyclic voltammetry and amperometry indicated that the oxidation involves 2-electrons, with a heterogeneous rate constant of 4.9 x 10 5 mol -1 L s -1 . The response is linear from 2 to 210 μmol L -1 , the sensitivity is 1570 μA L mmol -1 , the detection limit is 0.03 μmol L -1 , and the relative standard deviation of 110 μmol L -1 GSH was 2.6% (n=10). The modified electrode was applied to the determination of GSH in erythrocytes and the results were in agreement with those obtained by a method reported in the literature. (author)

  3. Electrochemical Selective and Simultaneous Detection of Diclofenac and Ibuprofen in Aqueous Solution Using HKUST-1 Metal-Organic Framework-Carbon Nanofiber Composite Electrode

    Directory of Open Access Journals (Sweden)

    Sorina Motoc

    2016-10-01

    Full Text Available In this study, the detection protocols for the individual, selective, and simultaneous determination of ibuprofen (IBP and diclofenac (DCF in aqueous solutions have been developed using HKUST-1 metal-organic framework-carbon nanofiber composite (HKUST-CNF electrode. The morphological and electrical characterization of modified composite electrode prepared by film casting was studied by scanning electronic microscopy and four-point-probe methods. The electrochemical characterization of the electrode by cyclic voltammetry (CV was considered the reference basis for the optimization of the operating conditions for chronoamperometry (CA and multiple-pulsed amperometry (MPA. This electrode exhibited the possibility to selectively detect IBP and DCF by simple switching the detection potential using CA. However, the MPA operated under optimum working conditions of four potential levels selected based on CV shape in relation to the potential value, pulse time, and potential level number, and order allowed the selective/simultaneous detection of IBP and DCF characterized by the enhanced detection performance. For this application, the HKUST-CNF electrode exhibited a good stability and reproducibility of the results was achieved.

  4. Electrochemical Selective and Simultaneous Detection of Diclofenac and Ibuprofen in Aqueous Solution Using HKUST-1 Metal-Organic Framework-Carbon Nanofiber Composite Electrode.

    Science.gov (United States)

    Motoc, Sorina; Manea, Florica; Iacob, Adriana; Martinez-Joaristi, Alberto; Gascon, Jorge; Pop, Aniela; Schoonman, Joop

    2016-10-17

    In this study, the detection protocols for the individual, selective, and simultaneous determination of ibuprofen (IBP) and diclofenac (DCF) in aqueous solutions have been developed using HKUST-1 metal-organic framework-carbon nanofiber composite (HKUST-CNF) electrode. The morphological and electrical characterization of modified composite electrode prepared by film casting was studied by scanning electronic microscopy and four-point-probe methods. The electrochemical characterization of the electrode by cyclic voltammetry (CV) was considered the reference basis for the optimization of the operating conditions for chronoamperometry (CA) and multiple-pulsed amperometry (MPA). This electrode exhibited the possibility to selectively detect IBP and DCF by simple switching the detection potential using CA. However, the MPA operated under optimum working conditions of four potential levels selected based on CV shape in relation to the potential value, pulse time, and potential level number, and order allowed the selective/simultaneous detection of IBP and DCF characterized by the enhanced detection performance. For this application, the HKUST-CNF electrode exhibited a good stability and reproducibility of the results was achieved.

  5. Effect of sampling site, repeated sampling, pH, and PCO2 on plasma lactate concentration in healthy dogs.

    Science.gov (United States)

    Hughes, D; Rozanski, E R; Shofer, F S; Laster, L L; Drobatz, K J

    1999-04-01

    To characterize the variation in plasma lactate concentration among samples from commonly used blood sampling sites in conscious, healthy dogs. 60 healthy dogs. Cross-sectional study using a replicated Latin square design. Each dog was assigned to 1 of 6 groups (n = 10) representing all possible orders for 3 sites (cephalic vein, jugular vein, and femoral artery) used to obtain blood. Samples were analyzed immediately, by use of direct amperometry for pH, PO2, Pco2, glucose, and lactate concentration. Significant differences in plasma lactate concentrations were detected among blood samples from the cephalic vein (highest), femoral artery, and jugular vein (lowest). Mean plasma lactate concentration in the first sample obtained, irrespective of sampling site, was lower than in subsequent samples. Covariation was identified among plasma lactate concentration, pH, and PCO2, but correlation coefficients were low. Plasma lactate concentrations differed among blood samples from various sites. A reference range for plasma lactate concentration was 0.3 to 2.5 mmol/L. Differences in plasma lactate concentrations among samples from various sites and with repeated sampling, in healthy dogs, are small. Use of the reference range may facilitate the clinical use of plasma lactate concentration in dogs.

  6. Amperometric L-glutamate biosensor based on bacterial cell-surface displayed glutamate dehydrogenase.

    Science.gov (United States)

    Liang, Bo; Zhang, Shu; Lang, Qiaolin; Song, Jianxia; Han, Lihui; Liu, Aihua

    2015-07-16

    A novel L-glutamate biosensor was fabricated using bacteria surface-displayed glutamate dehydrogenase (Gldh-bacteria). Here the cofactor NADP(+)-specific dependent Gldh was expressed on the surface of Escherichia coli using N-terminal region of ice nucleation protein (INP) as the anchoring motif. The cell fractionation assay and SDS-PAGE analysis indicated that the majority of INP-Gldh fusion proteins were located on the surface of cells. The biosensor was fabricated by successively casting polyethyleneimine (PEI)-dispersed multi-walled carbon nanotubes (MWNTs), Gldh-bacteria and Nafion onto the glassy carbon electrode (Nafion/Gldh-bacteria/PEI-MWNTs/GCE). The MWNTs could not only significantly lower the oxidation overpotential towards NAPDH, which was the product of NADP(+) involving in the oxidation of glutamate by Gldh, but also enhanced the current response. Under the optimized experimental conditions, the current-time curve of the Nafion/Gldh-bacteria/PEI-MWNTs/GCE was performed at +0.52 V (vs. SCE) by amperometry varying glutamate concentration. The current response was linear with glutamate concentration in two ranges (10 μM-1 mM and 2-10 mM). The low limit of detection was estimated to be 2 μM glutamate (S/N=3). Moreover, the proposed biosensor is stable, specific, reproducible and simple, which can be applied to real samples detection. Copyright © 2015 Elsevier B.V. All rights reserved.

  7. Highly sensitive and wide-range nonenzymatic disposable glucose sensor based on a screen printed carbon electrode modified with reduced graphene oxide and Pd-CuO nanoparticles

    International Nuclear Information System (INIS)

    Dhara, Keerthy; Thiagarajan, Ramachandran; Thekkedath, Gopalakrishnan Satheesh Babu; Nair, Bipin G.

    2015-01-01

    A nanocomposite consisting of reduced graphene oxide decorated with palladium-copper oxide nanoparticles (Pd-CuO/rGO) was synthesized by single-step chemical reduction. The morphology and crystal structure of the nanocomposite were characterized by field-emission scanning electron microscopy, high resolution transmission electron microscopy and X-ray diffraction analysis. A 3-electrode system was fabricated by screen printing technology and the Pd-CuO/rGO nanocomposite was drop cast on the carbon working electrode. The catalytic activity towards glucose in 0.2 M NaOH solutions was analyzed by linear sweep voltammetry and amperometry. The steady state current obtained at a constant potential of +0.6 V (vs. Ag/AgCl) showed the modified electrode to possess a wide analytical range (6 μM to 22 mM), a rather low limit of detection (30 nM), excellent sensitivity (3355 μA∙mM −1 ∙cm −2 ) and good selectivity over commonly interfering species and other sugars including fructose, sucrose and lactose. The sensor was successfully employed to the determination of glucose in blood serum. (author)

  8. A lactate electrochemical biosensor with a titanate nanotube as direct electron transfer promoter

    Science.gov (United States)

    Yang, Mingli; Wang, Jin; Li, Huaqing; Zheng, Jian-Guo; Wu, Nianqiang Nick

    2008-02-01

    Hydrogen titanate (H2Ti3O7) nanotubes (TNTs) have been synthesized by a one-step hydrothermal processing. Lactate oxidase (LOx) enzyme has been immobilized on the three-dimensional porous TNT network to make an electrochemical biosensor for lactate detection. Cyclic voltammetry and amperometry tests reveal that the LOx enzyme, which is supported on TNTs, maintains their substrate-specific catalytic activity. The nanotubes offer the pathway for direct electron transfer between the electrode surface and the active redox centers of LOx, which enables the biosensor to operate at a low working potential and to avoid the influence of the presence of O2 on the amperometric current response. The biosensor exhibits a sensitivity of 0.24 µA cm-2 mM-1, a 90% response time of 5 s, and a linear response in the range from 0.5 to 14 mM and the redox center of enzyme obviates the need of redox mediators for electrochemical enzymatic sensors, which is attractive for the development of reagentless biosensors.

  9. Co-immobilization of gold nanoparticles with glucose oxidase to improve bioelectrocatalytic glucose oxidation

    Science.gov (United States)

    Aquino Neto, Sidney; Milton, Ross D.; Crepaldi, Laís B.; Hickey, David P.; de Andrade, Adalgisa R.; Minteer, Shelley D.

    2015-07-01

    Recently, there has been much effort in developing metal nanoparticle catalysts for fuel oxidation, as well as the development of enzymatic bioelectrocatalysts for fuel oxidation. However, there has been little study of the synergy of hybrid electrocatalytic systems. We report the preparation of hybrid bioanodes based on Au nanoparticles supported on multi-walled carbon nanotubes (MWCNTs) co-immobilized with glucose oxidase (GOx). Mediated electron transfer was achieved by two strategies: ferrocene entrapped within polypyrrole and a ferrocene-modified linear poly(ethylenimine) (Fc-LPEI) redox polymer. Electrochemical characterization of the Au nanoparticles supported on MWCNTs indicate that this catalyst exhibits an electrocatalytic response for glucose even in acidic conditions. Using the redox polymer Fc-LPEI as the mediator, voltammetric and amperometric data demonstrated that these bioanodes can efficiently achieve mediated electron transfer and also indicated higher catalytic currents with the hybrid bioelectrode. From the amperometry, the maximum current density (Jmax) achieved with the hybrid bioelectrode was 615 ± 39 μA cm-2, whereas the bioanode employing GOx only achieved a Jmax of 409 ± 26 μA cm-2. Biofuel cell tests are consistent with the electrochemical characterization, thus confirming that the addition of the metallic species into the bioanode structure can improve fuel oxidation and consequently, improve the power generated by the system.

  10. Graphene: The Missing Piece for Cancer Diagnosis?

    Directory of Open Access Journals (Sweden)

    Sandra M. A. Cruz

    2016-01-01

    Full Text Available This paper reviews recent advances in graphene-based biosensors development in order to obtain smaller and more portable devices with better performance for earlier cancer detection. In fact, the potential of Graphene for sensitive detection and chemical/biological free-label applications results from its exceptional physicochemical properties such as high electrical and thermal conductivity, aspect-ratio, optical transparency and remarkable mechanical and chemical stability. Herein we start by providing a general overview of the types of graphene and its derivatives, briefly describing the synthesis procedure and main properties. It follows the reference to different routes to engineer the graphene surface for sensing applications with organic biomolecules and nanoparticles for the development of advanced biosensing platforms able to detect/quantify the characteristic cancer biomolecules in biological fluids or overexpressed on cancerous cells surface with elevated sensitivity, selectivity and stability. We then describe the application of graphene in optical imaging methods such as photoluminescence and Raman imaging, electrochemical sensors for enzymatic biosensing, DNA sensing, and immunosensing. The bioquantification of cancer biomarkers and cells is finally discussed, particularly electrochemical methods such as voltammetry and amperometry which are generally adopted transducing techniques for the development of graphene based sensors for biosensing due to their simplicity, high sensitivity and low-cost. To close, we discuss the major challenges that graphene based biosensors must overcome in order to reach the necessary standards for the early detection of cancer biomarkers by providing reliable information about the patient disease stage.

  11. Study of the corrosion of nickel base alloys in molten fluorides medium

    International Nuclear Information System (INIS)

    Fabre, St.; Finne, J.; Noel, D.; Catalette, H.; Cabet, C.; Chamelot, P.; Taxil, P.; Cassayre, L.

    2007-01-01

    The aim of this work is to study the corrosion mechanisms of nickel and its alloys in molten fluoride media. In a first part, the behaviour of the pure alloy metals has been studied (Ni, Mo, W, Fe and Cr) in three different salts mixtures: LiF-NaF, LiF-CaF 2 and LiF-AlF 3 in a temperature range of 700-1000 C. An experimental assembly allowing the implementation of electrochemical methods has been fabricated and validated. Linear scanning volt-amperometry has been used for studying the corrosion reactions of metals. It has then been possible to obtain intensity-potential curves and to determine the currents and corrosion potentials by the plotting of Tafel straight lines. These experimental results have finely been interpreted in considering the thermodynamic data accessible in literature (potential-oxo-acidity diagrams of metals in salts built from HSC Chemistry 5.1) and the influence of temperature and the nature of the bath have been estimated. (O.M.)

  12. Study of the corrosion of nickel base alloys in molten fluorides medium; Etude de la corrosion des alliages base nickel en milieu de fluorures fondus

    Energy Technology Data Exchange (ETDEWEB)

    Fabre, St.; Finne, J.; Noel, D.; Catalette, H. [Electricite de France (EDF/RD), Dept. Materiaux et Mecanique des Composants, Groupe Chimie et Corrosion, 77 - Ecuelles (France); Cabet, C. [CEA Saclay, Dept. de Physico-Chimie (DEN/DANS/DPC/SCCME), 91 - Gif sur Yvette (France); Chamelot, P.; Taxil, P.; Cassayre, L. [Universite Paul Sabatier, Lab. de Genie Chimique UMR 5503, Dept. Procedes Electrochimiques, 31 - Toulouse (France)

    2007-07-01

    The aim of this work is to study the corrosion mechanisms of nickel and its alloys in molten fluoride media. In a first part, the behaviour of the pure alloy metals has been studied (Ni, Mo, W, Fe and Cr) in three different salts mixtures: LiF-NaF, LiF-CaF{sub 2} and LiF-AlF{sub 3} in a temperature range of 700-1000 C. An experimental assembly allowing the implementation of electrochemical methods has been fabricated and validated. Linear scanning volt-amperometry has been used for studying the corrosion reactions of metals. It has then been possible to obtain intensity-potential curves and to determine the currents and corrosion potentials by the plotting of Tafel straight lines. These experimental results have finely been interpreted in considering the thermodynamic data accessible in literature (potential-oxo-acidity diagrams of metals in salts built from HSC Chemistry 5.1) and the influence of temperature and the nature of the bath have been estimated. (O.M.)

  13. Direct electrochemistry of hemoglobin and biosensing for hydrogen peroxide using a film containing silver nanoparticles and poly(amidoamine) dendrimer

    International Nuclear Information System (INIS)

    Baccarin, Marina; Janegitz, Bruno C.; Berté, Rodrigo; Vicentini, Fernando Campanhã; Banks, Craig E.; Fatibello-Filho, Orlando

    2016-01-01

    A new architecture for a biosensor is proposed using a glassy carbon electrode (GCE) modified with hemoglobin (Hb) and silver nanoparticles (AgNPs) encapsulated in poly(amidoamine) dendrimer (PAMAM). The biosensors were characterized using ultraviolet–visible spectroscopy, ζ-potential and cyclic voltammetry to investigate the interactions between Hb, AgNPs and the PAMAM film. The biosensor exhibited a well-defined cathodic peak attributed to reduction of the Fe"3"+ present in the heme group in Hb, as revealed by cyclic voltammetry in the presence of O_2. An apparent heterogeneous electron transfer rate of 4.1 s"−"1 was obtained. The Hb–AgNPs-PAMAM/GCE third generation biosensor was applied in the amperometric determination of hydrogen peroxide over the linear range from 6.0 × 10"−"6 to 9.1 × 10"−"5 mol L"−"1 with a detection limit of 4.9 × 10"−"6 mol L"−"1. The proposed method can be extended to immobilize and evaluate the direct electron transfer of other redox enzymes. - Highlights: • A new architecture for biosensor using Hb, AgNPs and PAMAM is proposed. • H_2O_2 is determined by amperometry using the proposed third generation biosensor. • The direct electron transfer was obtained from Hb using Hb–AgNPs–PAMAM.

  14. Electrooxidation and amperometric determination of vorinostat on hierarchical leaf-like gold nanolayers.

    Science.gov (United States)

    Vais, R Dehdari; Karimian, K; Heli, H

    2018-02-01

    Hierarchical leaf-like gold nanolayers were electrodeposited using choline chloride as a shape directing agent and characterized using field emission scanning electron microscopy. The electrooxidation behavior of vorinostat was then studied on the nanolayers and the kinetic parameters of the electrodic process were obtained by voltammetric measurements in a phosphate buffer solution at pH 7.40. Vorinostat was electrooxidized on the nanolayers' surface at a lower potential and with a higher rate, compared to a polycrystalline smooth gold surface, through an irreversible process. Based on the results, an amperometric sensor was designed using the hierarchical leaf-like gold nanolayers for the determination of vorinostat. A linear dynamic range of 4.0-52μmol L -1 with a calibration sensitivity of 7.7mAmol -1 L, and a detection limit of 1.40μmolL -1 were obtained. The amperometry method was also applied to the analysis of vorinostat capsules. Copyright © 2017 Elsevier B.V. All rights reserved.

  15. A new electrochemical sensor for highly sensitive and selective detection of nitrite in food samples based on sonochemical synthesized Calcium Ferrite (CaFe2O4) clusters modified screen printed carbon electrode.

    Science.gov (United States)

    Balasubramanian, Paramasivam; Settu, Ramki; Chen, Shen-Ming; Chen, Tse-Wei; Sharmila, Ganapathi

    2018-08-15

    Herein, we report a novel, disposable electrochemical sensor for the detection of nitrite ions in food samples based on the sonochemical synthesized orthorhombic CaFe 2 O 4 (CFO) clusters modified screen printed electrode. As synthesized CFO clusters were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), Fourier transformer infrared spectroscopy (FT-IR), Thermogravimetric analysis (TGA), X-ray photoelectron spectroscopy (XPS), electrochemical impedance spectroscopy (EIS), cyclic voltammetry (CV) and amperometry (i-t). Under optimal condition, the CFO modified electrode displayed a rapid current response to nitrite, a linear response range from 0.016 to 1921 µM associated with a low detection limit 6.6 nM. The suggested sensor also showed the excellent sensitivity of 3.712 μA μM -1  cm -2 . Furthermore, a good reproducibility, long-term stability and excellent selectivity were also attained on the proposed sensor. In addition, the practical applicability of the sensor was investigated via meat samples, tap water and drinking water, and showed desirable recovery rate, representing its possibilities for practical application. Copyright © 2018 Elsevier Inc. All rights reserved.

  16. Lipase immobilized on nanostructured cerium oxide thin film coated on transparent conducting oxide electrode for butyrin sensing

    International Nuclear Information System (INIS)

    Panky, Sreedevi; Thandavan, Kavitha; Sivalingam, Durgajanani; Sethuraman, Swaminathan; Krishnan, Uma Maheswari; Jeyaprakash, Beri Gopalakrishnan; Rayappan, John Bosco Balaguru

    2013-01-01

    Nanostructured cerium oxide (CeO 2 ) thin films were deposited on transparent conducting oxide (TCO) substrate using spray pyrolysis technique with cerium nitrate salt, Ce(NO 3 ) 3 ·6H 2 O as precursor. Fluorine doped cadmium oxide (CdO:F) thin film prepared using spray pyrolysis technique acts as the TCO film and hence the bare electrode. The structural, morphological and elemental characterizations of the films were carried out using X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM) and energy dispersive X-ray analysis (EDX) respectively. The diffraction peak positions in XRD confirmed the formation of highly crystalline ceria with cubic structure and FE-SEM images showed uniform adherent films with granular morphology. The band gaps of CeO 2 and TCO were found to be 3.2 eV and 2.6 eV respectively. Lipase enzyme was physisorbed on the surface of CeO 2 /TCO film to form the lipase/nano-CeO 2 /TCO bioelectrode. Sensing studies were carried out using cyclic voltammetry and amperometry, with lipase/nano-CeO 2 /TCO as working electrode and tributyrin as substrate. The mediator-free biosensor with nanointerface exhibited excellent linearity (0.33–1.98 mM) with a lowest detection limit of 2 μM with sharp response time of 5 s and a shelf life of about 6 weeks. -- Graphical abstract: Nanostructured cerium oxide thin films were deposited on transparent conducting oxide (TCO) substrate using spray pyrolysis technique. Fluorine doped cadmium oxide (CdO:F) thin film acts as the TCO film and hence the working electrode. Lipase enzyme was physisorbed on the surface of CeO 2 /TCO film and hence the lipase/nano-CeO 2 /TCO bioelectrode has been fabricated. Sensing studies were carried out using cyclic voltammetry and amperometry with tributyrin as substrate. The mediator-free biosensor with nanointerface exhibited excellent linearity (0.33–1.98 mM) with a lowest detection limit of 2 μM with sharp response time of 5 s and a shelf life of about 6

  17. Lipase immobilized on nanostructured cerium oxide thin film coated on transparent conducting oxide electrode for butyrin sensing

    Energy Technology Data Exchange (ETDEWEB)

    Panky, Sreedevi; Thandavan, Kavitha [Centre for Nanotechnology and Advanced Biomaterials (CeNTAB), SASTRA University, Thanjavur 613 401, Tamil Nadu (India); School of Chemical and Biotechnology, SASTRA University, Thanjavur 613 401, Tamil Nadu (India); Sivalingam, Durgajanani [Centre for Nanotechnology and Advanced Biomaterials (CeNTAB), SASTRA University, Thanjavur 613 401, Tamil Nadu (India); School of Electrical and Electronics Engineering, SASTRA University, Thanjavur 613 401, Tamil Nadu (India); Sethuraman, Swaminathan; Krishnan, Uma Maheswari [Centre for Nanotechnology and Advanced Biomaterials (CeNTAB), SASTRA University, Thanjavur 613 401, Tamil Nadu (India); School of Chemical and Biotechnology, SASTRA University, Thanjavur 613 401, Tamil Nadu (India); Jeyaprakash, Beri Gopalakrishnan [Centre for Nanotechnology and Advanced Biomaterials (CeNTAB), SASTRA University, Thanjavur 613 401, Tamil Nadu (India); School of Electrical and Electronics Engineering, SASTRA University, Thanjavur 613 401, Tamil Nadu (India); Rayappan, John Bosco Balaguru, E-mail: rjbosco@ece.sastra.edu [Centre for Nanotechnology and Advanced Biomaterials (CeNTAB), SASTRA University, Thanjavur 613 401, Tamil Nadu (India); School of Electrical and Electronics Engineering, SASTRA University, Thanjavur 613 401, Tamil Nadu (India)

    2013-01-15

    Nanostructured cerium oxide (CeO{sub 2}) thin films were deposited on transparent conducting oxide (TCO) substrate using spray pyrolysis technique with cerium nitrate salt, Ce(NO{sub 3}){sub 3}{center_dot}6H{sub 2}O as precursor. Fluorine doped cadmium oxide (CdO:F) thin film prepared using spray pyrolysis technique acts as the TCO film and hence the bare electrode. The structural, morphological and elemental characterizations of the films were carried out using X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM) and energy dispersive X-ray analysis (EDX) respectively. The diffraction peak positions in XRD confirmed the formation of highly crystalline ceria with cubic structure and FE-SEM images showed uniform adherent films with granular morphology. The band gaps of CeO{sub 2} and TCO were found to be 3.2 eV and 2.6 eV respectively. Lipase enzyme was physisorbed on the surface of CeO{sub 2}/TCO film to form the lipase/nano-CeO{sub 2}/TCO bioelectrode. Sensing studies were carried out using cyclic voltammetry and amperometry, with lipase/nano-CeO{sub 2}/TCO as working electrode and tributyrin as substrate. The mediator-free biosensor with nanointerface exhibited excellent linearity (0.33-1.98 mM) with a lowest detection limit of 2 {mu}M with sharp response time of 5 s and a shelf life of about 6 weeks. -- Graphical abstract: Nanostructured cerium oxide thin films were deposited on transparent conducting oxide (TCO) substrate using spray pyrolysis technique. Fluorine doped cadmium oxide (CdO:F) thin film acts as the TCO film and hence the working electrode. Lipase enzyme was physisorbed on the surface of CeO{sub 2}/TCO film and hence the lipase/nano-CeO{sub 2}/TCO bioelectrode has been fabricated. Sensing studies were carried out using cyclic voltammetry and amperometry with tributyrin as substrate. The mediator-free biosensor with nanointerface exhibited excellent linearity (0.33-1.98 mM) with a lowest detection limit of 2 {mu}M with sharp

  18. Electrooxidation of borohydride on platinum and gold electrodes: implications for direct borohydride fuel cells

    Energy Technology Data Exchange (ETDEWEB)

    Gyenge, E. [University of British Columbia, Vancouver (Canada). Dept. of Chemical and Biological Engineering

    2004-03-01

    The electrochemical oxidation of BH{sub 4}{sup -} in 2M NaOH on Pt and Au (i.e. catalytic and non-catalytic electrodes, respectively, for BH{sub 4}{sup -} hydrolysis accompanied by H{sub 2} evolution) has been studied by cyclic voltammetry, chrono-techniques (i.e., potentiometry, amperometry, coulometry) and electrochemical impedance spectroscopy. In the case of Pt the cyclic voltammetry behaviour of BH{sub 4}{sup -} is influenced by both, the catalytic hydrolysis of BH{sub 4}{sup -} yielding H{sub 2} followed by electrooxidation of the latter at peak potentials between -0.7 and -0.9 V versus Ag/AgCl, KCl{sub std} and direct oxidation of BH{sub 4}{sup -} at more positive potentials, i.e., between -0.15 and -0.05 V. Thiourea (TU, 1.5 x 10{sup -3} M) was an effective inhibitor of the catalytic hydrolysis associated with BH{sub 4}{sup -} electrooxidation on Pt. Therefore, in the presence of TU, only the direct oxidation of BH{sub 4}{sup -} has been detected, with peak potentials between -0.2 and 0 V. It is proposed that TU could improve the BH{sub 4}{sup -} utilization efficiency and the coulombic efficiency of direct borohydride fuel cells using catalytic anodes. The electrooxidation of BH{sub 4}{sup -} on Pt/TU is an overall four-electron process, instead of the maximum eight electrons reported for Au, and it is affected by adsorbed species such as BH{sub 4}{sup -} (fractional surface coverage {approx}0.3), TU and possibly reaction intermediates. (author)

  19. One dimensional CdS nanowire@TiO2 nanoparticles core-shell as high performance photocatalyst for fast degradation of dye pollutants under visible and sunlight irradiation.

    Science.gov (United States)

    Arabzadeh, Abbas; Salimi, Abdollah

    2016-10-01

    In this study, one-dimensional CdS nanowires@TiO2 nanoparticles core-shell structures (1D CdS NWs@TiO2 NPs) were synthesized by a facile wet chemical-solvothermal method. The different aspects of the properties of CdS NWs@TiO2 NPs were surveyed by using a comprehensive range of characterization techniques including X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), UV-vis spectroscopy, scanning electron microscopy (SEM), fluorescence spectroscopy, energy dispersive X-ray spectroscopy (EDX), Cyclic Voltammetry (CV) and amperometry. The as-prepared nanostructure was applied as an effective photocatalyst for degradation of methyl orange (MO), methylene blue (MB) and rhodamine B (Rh B) under visible and sunlight irradiation. The results indicated significantly enhanced photocatalytic activity of CdS NWs@TiO2 NPs for degradation of MO, MB and Rh B compared to CdS NWs. The enhanced photocatalytic activity could be attributed to the enhanced sunlight absorbance and the efficient charge separation of the formed heterostructure between CdS NWs and TiO2. The results showed that MO, Rh B and MB were almost completely degraded after 2, 2 and 3min of exposure to sunlight, respectively; while under visible light irradiation (3W blue LED lamp) the dyes were decomposed with less half degradation rate. The catalytic activity was retained even after three degradation cycles of organic dyes, demonstrating that the proposed nanocomposite can be effectively used as efficient photocatalyst for removal of environmental pollutions caused by organic dyes under sunlight irradiation and it could be an important addition to the field of wastewater treatment. We hope the present study may open a new window of such 1-D semiconductor nanocomposites to be used as visible light photocatalysts in the promising field of organic dyes degradation. Copyright © 2016 Elsevier Inc. All rights reserved.

  20. SnO(2) quantum dots-reduced graphene oxide composite for enzyme-free ultrasensitive electrochemical detection of urea.

    Science.gov (United States)

    Dutta, Dipa; Chandra, Sudeshna; Swain, Akshaya K; Bahadur, Dhirendra

    2014-06-17

    Most of the urea sensors are biosensors and utilize urease, which limit their use in harsh environments. Recently, because of their exceptional ability to endorse faster electron transfer, carbonaceous material composites and quantum dots are being used for fabrication of a sensitive transducer surface for urea biosensors. We demonstrate an enzyme free ultrasensitive urea sensor fabricated using a SnO2 quantum dots (QDs)/reduced graphene oxide (RGO) composite. Due to the synergistic effect of the constituents, the SnO2 QDs/RGO (SRGO) composite proved to be an excellent probe for electrochemical sensing. The morphology and structure of the composite was characterized by various techniques, and it was observed that SnO2 QDs are decorated on RGO layers. Electrochemical studies were performed to evaluate the characteristics of the sensor toward detection of urea. Amperometry studies show that the SRGO/GCE electrode is sensitive to urea in the concentration range of 1.6 × 10(-14)-3.9 × 10(-12) M, with a detection limit of as low as 11.7 fM. However, this is an indirect measurement for urea wherein the analytical signal is recorded as a decrease in the amperommetric and/or voltammetric current from the solution redox species ferrocyanide. The porous structure of the SRGO matrix offers a very low transport barrier and thus promotes rapid diffusion of the ionic species from the solution to the electrode, leading to a rapid response time (∼5 s) and ultrahigh sensitivity (1.38 μA/fM). Good analytical performance in the presence of interfering agents, low cost, and easy synthesis methodology suggest that SRGO can be quite promising as an electroactive material for effective urea sensing.

  1. Amperometric L-glutamate biosensor based on bacterial cell-surface displayed glutamate dehydrogenase

    Energy Technology Data Exchange (ETDEWEB)

    Liang, Bo [Laboratory for Biosensing, Key Laboratory of Biofuels, and Shandong Provinicial Key Laboratory of Energy Genetics, Qingdao Institute of Bioenergy & Bioprocess Technology, Chinese Academy of Sciences, 189 Songling Road, Qingdao 266101 (China); University of Chinese Academy of Sciences, 19A Yuquan Road, Beijing 100049 (China); Zhang, Shu [Laboratory for Biosensing, Key Laboratory of Biofuels, and Shandong Provinicial Key Laboratory of Energy Genetics, Qingdao Institute of Bioenergy & Bioprocess Technology, Chinese Academy of Sciences, 189 Songling Road, Qingdao 266101 (China); Key Laboratory of Marine Chemistry Theory and Technology of Ministry of Education, Ocean University of China, 238 Songling Road, Qingdao 266100 (China); Lang, Qiaolin [Laboratory for Biosensing, Key Laboratory of Biofuels, and Shandong Provinicial Key Laboratory of Energy Genetics, Qingdao Institute of Bioenergy & Bioprocess Technology, Chinese Academy of Sciences, 189 Songling Road, Qingdao 266101 (China); Song, Jianxia; Han, Lihui [Key Laboratory of Marine Chemistry Theory and Technology of Ministry of Education, Ocean University of China, 238 Songling Road, Qingdao 266100 (China); Liu, Aihua, E-mail: liuah@qibebt.ac.cn [Laboratory for Biosensing, Key Laboratory of Biofuels, and Shandong Provinicial Key Laboratory of Energy Genetics, Qingdao Institute of Bioenergy & Bioprocess Technology, Chinese Academy of Sciences, 189 Songling Road, Qingdao 266101 (China); University of Chinese Academy of Sciences, 19A Yuquan Road, Beijing 100049 (China)

    2015-07-16

    Highlights: • E. coli surface-dispalyed Gldh exhibiting excellent enzyme activity and stability. • Sensitive amperometric biosensor for glutamate using Gldh-bacteria and MWNTs. • The glutamate biosensor exhibited high specificity and stability. - Abstract: A novel L-glutamate biosensor was fabricated using bacteria surface-displayed glutamate dehydrogenase (Gldh-bacteria). Here the cofactor NADP{sup +}-specific dependent Gldh was expressed on the surface of Escherichia coli using N-terminal region of ice nucleation protein (INP) as the anchoring motif. The cell fractionation assay and SDS-PAGE analysis indicated that the majority of INP-Gldh fusion proteins were located on the surface of cells. The biosensor was fabricated by successively casting polyethyleneimine (PEI)-dispersed multi-walled carbon nanotubes (MWNTs), Gldh-bacteria and Nafion onto the glassy carbon electrode (Nafion/Gldh-bacteria/PEI-MWNTs/GCE). The MWNTs could not only significantly lower the oxidation overpotential towards NAPDH, which was the product of NADP{sup +} involving in the oxidation of glutamate by Gldh, but also enhanced the current response. Under the optimized experimental conditions, the current–time curve of the Nafion/Gldh-bacteria/PEI-MWNTs/GCE was performed at +0.52 V (vs. SCE) by amperometry varying glutamate concentration. The current response was linear with glutamate concentration in two ranges (10 μM–1 mM and 2–10 mM). The low limit of detection was estimated to be 2 μM glutamate (S/N = 3). Moreover, the proposed biosensor is stable, specific, reproducible and simple, which can be applied to real samples detection.

  2. PdNi- and Pd-coated electrodes prepared by electrodeposition from ionic liquid for nonenzymatic electrochemical determination of ethanol and glucose in alkaline media.

    Science.gov (United States)

    Huang, Hsin-Yi; Chen, Po-Yu

    2010-12-15

    Nonenzymatic electrochemical determination of ethanol and glucose was respectively achieved using PdNi- and Pd-coated electrodes prepared by electrodeposition from the novel metal-free ionic liquid (IL); N-butyl-N-methylpyrrolidinium dicyanamide (BMP-DCA). BMP-DCA provided an excellent environment and wide cathodic limit for electrodeposition of metals and alloys because many metal chlorides could dissolve in this IL where the reduction potentials of Pd(II) and Ni(II) indeed overlapped, leading to the convenience of potentiostatic codeposition. In aqueous solutions, the reduction potentials of Pd(II) and Ni(II) are considerably separated. The bimetallic PdNi coatings with atomic ratios of ∼ 80/20 showed the highest current for ethanol oxidation reaction (EOR). Ethanol was detected by either cyclic voltammetry (CV) or hydrodynamic amperometry (HA). Using CV, the dependence of EOR peak current on concentration was linear from 4.92 to 962 μM with a detection limit of 2.26 μM (σ=3), and a linearity was observed from 4.92 to 988 μM using HA (detection limit 0.83 μM (σ=3)). The Pd-coated electrodes prepared by electrodeposition from BMP-DCA showed electrocatalytic activity to glucose oxidation and CV, HA, and square-wave voltammetry (SWV) were employed to determine glucose. SWV showed the best sensitivity and linearity was observed from 2.86 μM to 107 μM, and from 2.99 mM to 10.88 mM with detection limits of 0.78 μM and 25.9 μM (σ=3), respectively. For glucose detection, the interference produced from ascorbic acid, uric acid, and acetaminophen was significantly suppressed, compared with a regular Pt disk electrode. Copyright © 2010 Elsevier B.V. All rights reserved.

  3. Pituitary adenylate cyclase activating polypeptide modulates catecholamine storage and exocytosis in PC12 cells.

    Directory of Open Access Journals (Sweden)

    Yan Dong

    Full Text Available A number of efforts have been made to understand how pituitary adenylate cyclase activating polypeptide (PACAP functions as a neurotrophic and neuroprotective factor in Parkinson's disease (PD. Recently its effects on neurotransmission and underlying mechanisms have generated interest. In the present study, we investigate the effects of PACAP on catecholamine storage and secretion in PC12 cells with amperometry and transmission electron microscopy (TEM. PACAP increases quantal release induced by high K+ without significantly regulating the frequency of vesicle fusion events. TEM data indicate that the increased volume of the vesicle is mainly the result of enlargement of the fluidic space around the dense core. Moreover, the number of docked vesicles isn't modulated by PACAP. When cells are acutely treated with L-DOPA, the vesicular volume and quantal release both increase dramatically. It is likely that the characteristics of amperometric spikes from L-DOPA treated cells are associated with increased volume of individual vesicles rather than a direct effect on the mechanics of exocytosis. Treatment with PACAP versus L-DOPA results in different profiles of the dynamics of exocytosis. Release via the fusion pore prior to full exocytosis was observed with the same frequency following treatment with PACAP and L-DOPA. However, release events have a shorter duration and higher average current after PACAP treatment compared to L-DOPA. Furthermore, PACAP reduced the proportion of spikes having rapid decay time and shortened the decay time of both fast and slow spikes. In contrast, the distributions of the amperometric spike decay for both fast and slow spikes were shifted to longer time following L-DOPA treatment. Compared to L-DOPA, PACAP may produce multiple favorable effects on dopaminergic neurons, including protecting dopaminergic neurons against neurodegeneration and potentially regulating dopamine storage and release, making it a promising

  4. Novel, reagentless, amperometric biosensor for uric acid based on a chemically modified screen-printed carbon electrode coated with cellulose acetate and uricase.

    Science.gov (United States)

    Gilmartin, M A; Hart, J P

    1994-05-01

    Amperometry in stirred solution has been used for the systematic evaluation of modified screen-printed carbon electrodes (SPCEs) with a view to developing a reagentless biosensor for uric acid. The developed system consists of a base cobalt phthalocyanine (CoPC) electrode tailored to the electrocatalytic oxidation of H2O2 by means of a cellulose acetate (CA)-uricase bilayer. Uricase was immobilized by drop-coating the enzyme onto the CA membrane covering the CoPC-SPCE. The device exploits the near-universal H2O2-generating propensity of oxidases, the permselectivity of the CA film towards H2O2 and the electrocatalytic oxidation of this product at the CoPC-SPCE. The electrochemical oxidation of the resulting Co+ species was used as the analytical signal, facilitating the application of a greatly reduced operating potential when compared with that required for direct oxidation of H2O2 at unmodified electrodes. The time required to achieve 95% of the steady-state current (t95i(ss)) was 44 s [relative standard deviation = 7.5% (n = 10)]. Amperometric calibrations were linear over the range from 13 x 10(-6) to 1 x 10(-3) mol dm-3, with the former representing the limit of detection. The CA membrane extended the linear range of the biosensor by over two orders of magnitude, when apparent Michaelis-Menten constants (Km') of immobilized and free enzymes are compared. This suggests that the process is diffusion-controlled and not governed by the kinetics of the enzyme. The precision of electrode fabrication was determined by cyclic voltammetry to be 4.9% (n = 6).(ABSTRACT TRUNCATED AT 250 WORDS)

  5. Rapid fluctuations in extracellular brain glucose levels induced by natural arousing stimuli and intravenous cocaine: fueling the brain during neural activation

    Science.gov (United States)

    Lenoir, Magalie

    2012-01-01

    Glucose, a primary energetic substrate for neural activity, is continuously influenced by two opposing forces that tend to either decrease its extracellular levels due to enhanced utilization in neural cells or increase its levels due to entry from peripheral circulation via enhanced cerebral blood flow. How this balance is maintained under physiological conditions and changed during neural activation remains unclear. To clarify this issue, enzyme-based glucose sensors coupled with high-speed amperometry were used in freely moving rats to evaluate fluctuations in extracellular glucose levels induced by brief audio stimulus, tail pinch (TP), social interaction with another rat (SI), and intravenous cocaine (1 mg/kg). Measurements were performed in nucleus accumbens (NAcc) and substantia nigra pars reticulata (SNr), which drastically differ in neuronal activity. In NAcc, where most cells are powerfully excited after salient stimulation, glucose levels rapidly (latency 2–6 s) increased (30–70 μM or 6–14% over baseline) by all stimuli; the increase differed in magnitude and duration for each stimulus. In SNr, where most cells are transiently inhibited by salient stimuli, TP, SI, and cocaine induced a biphasic glucose response, with the initial decrease (−20–40 μM or 5–10% below baseline) followed by a reboundlike increase. The critical role of neuronal activity in mediating the initial glucose response was confirmed by monitoring glucose currents after local microinjections of glutamate (GLU) or procaine (PRO). While intra-NAcc injection of GLU transiently increased glucose levels in this structure, intra-SNr PRO injection resulted in rapid, transient decreases in SNr glucose. Therefore, extracellular glucose levels in the brain change very rapidly after physiological and pharmacological stimulation, the response is structure specific, and the pattern of neuronal activity appears to be a critical factor determining direction and magnitude of physiological

  6. Synthesis of palladium nanoparticle modified reduced graphene oxide and multi-walled carbon nanotube hybrid structures for electrochemical applications

    Energy Technology Data Exchange (ETDEWEB)

    Hu, Jie, E-mail: hujie@tyut.edu.cn [Micro and Nano System Research Center, Key Lab of Advanced Transducers and Intelligent Control System (Ministry of Education) & College of Information Engineering, Taiyuan University of Technology, Taiyuan, 030024, Shanxi (China); Zhao, Zhenting; Zhang, Jun; Li, Gang; Li, Pengwei; Zhang, Wendong [Micro and Nano System Research Center, Key Lab of Advanced Transducers and Intelligent Control System (Ministry of Education) & College of Information Engineering, Taiyuan University of Technology, Taiyuan, 030024, Shanxi (China); Lian, Kun, E-mail: liankun@tyut.edu.cn [Micro and Nano System Research Center, Key Lab of Advanced Transducers and Intelligent Control System (Ministry of Education) & College of Information Engineering, Taiyuan University of Technology, Taiyuan, 030024, Shanxi (China); School of Nano-Science and Nano-Engineering, Suzhou & Collaborative Innovation Center of Suzhou Nano Science and Technology, Xi' an Jiaotong University, Xi' an, 710049 (China); Center for Advanced Microstructures and Devices, Louisiana State University, LA, 70806 (United States)

    2017-02-28

    Graphical abstract: A sensitive hydrazine electrochemical sensor was fabricated by using palladium (Pd) nanoparticle functionalized reduced graphene oxide (rGO) and multi-walled carbon nanotube (MWCNTs) hybrid structures (Pd/rGO-MWCNTs). - Highlights: • rGO-MWCNTs hybrid structures and Pd nanoparticles are prepared using electrochemical methods. • rGO-MWCNTs hybrid films are used as supports and co-catalysts for Pd nanoparticles. • The Pd/rGO-MWCNTs hybrid structure based sensor shows an ultra-high sensitivity of 7.09 μA μM{sup −1} cm{sup −2} and a low detection limit of 0.15 μM. • The proposed electrochemical sensor exhibits excellent selectivity. - Abstract: In this work, palladium (Pd) nanoparticles functionalized reduced graphene oxide (rGO) and multi-walled carbon nanotubes (MWCNTs) hybrid structures (Pd/rGO-MWCNTs) were successfully prepared by a combination of electrochemical reduction with electrodeposition method. The morphology, structure, and composition of the Pd/rGO-MWCNTs hybrid were characterized by scanning electron microscopy, transmission electron microscopy and energy dispersive spectroscopy. The as-synthesized hybrid structures were modified on the glassy carbon electrode (GCE) and further utilized for hydrazine sensing. Electrochemical impedance spectroscopic, cyclic voltammetry and single-potential amperometry experiments were carried out on Pd/rGO-MWCNTs hybrid structures to investigate the interface properties and sensing performance. The measured results demonstrate that the fabricated Pd/rGO-MWCNTs/GCE sensor show a high sensitivity of 7.09 μA μM{sup −1} cm{sup −2} in a large concentration range of 1.0 to 1100 μM and a low detection limit of 0.15 μM. Moreover, the as-prepared sensor exhibits good selectivity and stability for the determination of hydrazine under interference conditions.

  7. Electrochemical fabrication of a novel conducting metallopolymer nanoparticles and its electrocatalytic application

    International Nuclear Information System (INIS)

    Kazemi, Sayed Habib; Mohamadi, Rahim

    2013-01-01

    Graphical abstract: Nanoparticles of nickel-curcumin conducting polymer (Ni-Curc-NPs) were fabricated by a two steps electrochemical method. In the first step, nickel source was immobilized at the electrode surface in the form of nickel nanoparticles (NiNPs). Then, electropolymerization of Ni-curcumin was performed at the NiNPs modified electrode. These nanostructures were successfully employed for electrooxidative determination of glucose and significant increase in the electrochemical sensitivity and lower limit of detection were observed. -- Highlights: • A novel two steps method for fabrication of nickel-curcumin conducting polymer was described. • Nickel-curcumine nanoparticles were easily prepared instead of thin film. • Ni-Curc-NPs modified electrode was successfully employed for electrooxidation of glucose. • Significant improvement in the sensitivity and limit of detection was observed. -- Abstract: Present article is the first example of a novel two step electrochemical route for fabrication of nanoparticles of conducting metallopolymer of Ni-curcumin (Ni-Curc-NPs). Firstly, nickel nanoparticles (Ni-NPs) were electrochemically deposited on the electrode surface. Then, electropolymerization of Ni-Curc-NPs were performed at the electrode modified with Ni-NPs. These nanostructures were characterized using electrochemical methods including cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS) and hydrodynamic amperometry, also surface analysis methods and electron microscopy including energy dispersive analysis of X-ray (EDAX), X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM). Additionally, application of the Ni-Curc-NPs modified electrode toward glucose electrooxidation was examined. A lower limit of detection and enhanced dynamic linear range for determination of glucose were observed at Ni-Curc-NPs modified electrode compared to Ni-NPs modified electrode

  8. Electrocatalytic reduction of H2O2 by Pt nanoparticles covalently bonded to thiolated carbon nanostructures

    International Nuclear Information System (INIS)

    You, Jung-Min; Kim, Daekun; Jeon, Seungwon

    2012-01-01

    Highlights: ► Novel thiolated carbon nanostructures – platinum nanoparticles [t-GO-C(O)-pt and t-MWCNT-C(O)-S-pt] have been synthesized, and [t-GO-C(O)-pt and t-MWCNT-C(O)-S-pt] denotes as t-GO-pt and t-MWCNT-Pt in manuscript, respectively. ► The modified electrode denoted as PDDA/t-GO-pt/GCE was used for the electrochemical determination of H 2 O 2 for the first time. ► The results show that PDDA/t-GO-pt nanoparticles have the promising potential as the basic unit of the electrochemical biosensors for the detection of H 2 O 2 . ► The proposed H 2 O 2 biosensors exhibited wide linear ranges and low detection limits, giving fast responses within 10 s. - Abstract: Glassy carbon electrodes were coated with thiolated carbon nanostructures – multi-walled carbon nanotubes and graphene oxide. The subsequent covalent addition of platinum nanoparticles and coating with poly(diallydimethylammonium chloride) resulted in biosensors that detected hydrogen peroxide through its electrocatalytic reduction. The sensors were easily and quickly prepared and showed improved sensitivity to the electrocatalytic reduction of H 2 O 2 . The Pt nanoparticles covalently bonded to the thiolated carbon nanostructures were characterized by transmission electron microscopy, X-ray photoelectron spectroscopy, and energy dispersive X-ray spectroscopy. Cyclic voltammetry and amperometry were used to characterize the biosensors’ performances. The sensors exhibited wide linear ranges and low detection limits, giving fast responses within 10 s, thus demonstrating their potential for use in H 2 O 2 analysis.

  9. Electrocatalytic reduction of H{sub 2}O{sub 2} by Pt nanoparticles covalently bonded to thiolated carbon nanostructures

    Energy Technology Data Exchange (ETDEWEB)

    You, Jung-Min; Kim, Daekun [Department of Chemistry and Institute of Basic Science, Chonnam National University, Gwangju 500-757 (Korea, Republic of); Jeon, Seungwon [Department of Chemistry and Institute of Basic Science, Chonnam National University, Gwangju 500-757 (Korea, Republic of)

    2012-03-30

    Highlights: Black-Right-Pointing-Pointer Novel thiolated carbon nanostructures - platinum nanoparticles [t-GO-C(O)-pt and t-MWCNT-C(O)-S-pt] have been synthesized, and [t-GO-C(O)-pt and t-MWCNT-C(O)-S-pt] denotes as t-GO-pt and t-MWCNT-Pt in manuscript, respectively. Black-Right-Pointing-Pointer The modified electrode denoted as PDDA/t-GO-pt/GCE was used for the electrochemical determination of H{sub 2}O{sub 2} for the first time. Black-Right-Pointing-Pointer The results show that PDDA/t-GO-pt nanoparticles have the promising potential as the basic unit of the electrochemical biosensors for the detection of H{sub 2}O{sub 2}. Black-Right-Pointing-Pointer The proposed H{sub 2}O{sub 2} biosensors exhibited wide linear ranges and low detection limits, giving fast responses within 10 s. - Abstract: Glassy carbon electrodes were coated with thiolated carbon nanostructures - multi-walled carbon nanotubes and graphene oxide. The subsequent covalent addition of platinum nanoparticles and coating with poly(diallydimethylammonium chloride) resulted in biosensors that detected hydrogen peroxide through its electrocatalytic reduction. The sensors were easily and quickly prepared and showed improved sensitivity to the electrocatalytic reduction of H{sub 2}O{sub 2}. The Pt nanoparticles covalently bonded to the thiolated carbon nanostructures were characterized by transmission electron microscopy, X-ray photoelectron spectroscopy, and energy dispersive X-ray spectroscopy. Cyclic voltammetry and amperometry were used to characterize the biosensors' performances. The sensors exhibited wide linear ranges and low detection limits, giving fast responses within 10 s, thus demonstrating their potential for use in H{sub 2}O{sub 2} analysis.

  10. A DNA biosensor for molecular diagnosis of Aeromonas hydrophila using zinc sulfide nanospheres

    Directory of Open Access Journals (Sweden)

    M. Negahdary

    2017-07-01

    Full Text Available Today, identification of pathogenic bacteria using modern and accurate methods is inevitable. Integration in electrochemical measurements with nanotechnology has led to the design of efficient and sensitive DNA biosensors against bacterial agents. Here, efforts were made to detect Aeromonas hydrophila using aptamers as probes and zinc sulfide (ZnS nanospheres as signal enhancers and electron transfer facilitators. After modification of the working electrode area (in a screen-printed electrode with ZnS nanospheres through electrodeposition, the coated surface of a modified electrode with ZnS nanospheres was investigated through scanning electron microscopy (SEM. The size of synthesized ZnS nanospheres was estimated at about 20–50 nm and their shape was in the form of porous plates in microscopic observations. All electrochemical measurements were performed using cyclic voltammetry (CV, electrochemical impedance spectroscopy (EIS, and constant potential amperometry (CPA techniques. The designed DNA biosensor was able to detect deoxyribonucleic acid (DNA of Aeromonas hydrophila in the range 1.0  ×  10−4 to 1.0  ×  10−9 mol L−1; the limit of detection (LOD in this study was 1  ×  10−13 mol L−1. This DNA biosensor showed satisfactory thermal and pH stability. Reproducibility for this DNA biosensor was measured and the relative standard deviation (RSD of the performance of this DNA biosensor was calculated as 5 % during 42 days.

  11. Effect of anode polarization on biofilm formation and electron transfer in Shewanella oneidensis/graphite felt microbial fuel cells.

    Science.gov (United States)

    Pinto, David; Coradin, Thibaud; Laberty-Robert, Christel

    2018-04-01

    In microbial fuel cells, electricity generation is assumed by bacterial degradation of low-grade organics generating electrons that are transferred to an electrode. The nature and efficiency of the electron transfer from the bacteria to the electrodes are determined by several chemical, physical and biological parameters. Specifically, the application of a specific potential at the bioanode has been shown to stimulate the formation of an electro-active biofilm, but the underlying mechanisms remain poorly understood. In this study, we have investigated the effect of an applied potential on the formation and electroactivity of biofilms established by Shewanella oneidensis bacteria on graphite felt electrodes in single- and double-chamber reactor configurations in oxic conditions. Using amperometry, cyclic voltammetry, and OCP/Power/Polarization curves techniques, we showed that a potential ranging between -0.3V and +0.5V (vs. Ag/AgCl/KCl sat.) and its converse application to a couple of electrodes leads to different electrochemical behaviors, anodic currents and biofilm architectures. For example, when the bacteria were confined in the anodic compartment of a double-chamber cell, a negative applied potential (-0.3V) at the bioanode favors a mediated electron transfer correlated with the progressive formation of a biofilm that fills the felt porosity and bridges the graphite fibers. In contrast, a positive applied potential (+0.3V) at the bioanode stimulates a direct electron transfer resulting in the fast-bacterial colonization of the fibers only. These results provide significant insight for the understanding of the complex bacteria-electrode interactions in microbial fuel cells. Copyright © 2017 Elsevier B.V. All rights reserved.

  12. Biosensing hydrogen peroxide utilizing carbon paste electrodes containing peroxidases naturally immobilized on coconut (Cocus nucifera L.) fibers.

    Science.gov (United States)

    Kozan, J V B; Silva, R P; Serrano, S H P; Lima, A W O; Angnes, L

    2007-05-22

    A novel unmediated hydrogen peroxide biosensor based on the incorporation of fibrous tissue of coconut fruit in carbon paste matrix is presented. Cyclic voltammetry and amperometry were utilized to characterize the main electrochemical parameters and the performance of this new biosensor under different preparation and operation conditions. The resulting H2O2-sensitive biosensors respond rapidly (7 s to attain 90% of the signal), was operated at -0.15 V, presented linear response between 2.0x10(-4) and 3.4x10(-3) mol L(-1), the detection limit was estimated as 4.0x10(-5) mol L(-1). Its operation potential was situated between -0.2 and 0.1 V and the best pH was determined as 5.2. Electrodes containing 5% (w/w) of coconut fiber presented the best signal and their lifetime was extended to 3 months. The apparent Michaelis-Menten constant KM(app) and Vmax were estimated to be 8.90 mmol L(-1) and 6.92 mmol L(-1) microA(-1), respectively. The results obtained for determination of hydrogen peroxide in four pharmaceutical products (antiseptic solution, contact lenses cleaning solution, hair coloring cream and antiseptic dental rinse solution) were in agreement with those obtained by the spectrophotometric method. An additional advantage of these biosensors is the capacity to measure hydrogen peroxide even in samples with relatively low pH. To demonstrate the enzymatic activity of the coconut tissue, a very simple way was created during this work. Coconut fibers were immersed in H2O2 solution between two glass slides. Sequential images were taken to show the rapid generation of O2, attesting the high activity of the enzymes.

  13. Highly sensitive interference-free electrochemical determination of pyridoxine at graphene modified electrode: Importance in Parkinson and Asthma treatments.

    Science.gov (United States)

    Raj, M Amal; Gowthaman, N S K; John, S Abraham

    2016-07-15

    To reduce the side effects in the medication of Parkinson and Asthma, pyridoxine (PY) is administered along with l-3,4-dihydroxyphenyl alanine (l-dopa) and theophylline (TP), respectively. However, excessive dosage of PY leads to nervous disorder. Thus, a sensitive and selective electrochemical method was developed for the determination of PY in the presence of major interferences including TP, l-dopa, ascorbic acid (AA) and riboflavin (RB) using electrochemically reduced graphene oxide (ERGO) film modified glassy carbon electrode (GCE) in this paper. The ERGO fabrication process involves the nucleophilic substitution of graphene oxide at basic pH on amine terminal of 1,6-hexadiamine which was pre-assembled on GCE followed by electrochemical reduction. The electrocatalytic activity of the ERGO modified electrode was examined towards the oxidation of PY. It greatly enhanced the oxidation current of PY in contrast to bare and GO modified GCEs due to facile electron transfer besides π-π interaction between ERGO film and PY. Since TP and l-dopa drugs antagonize the drug action of PY, ERGO modified GCE was also used for the simultaneous determination of PY and l-dopa and PY and TP. Further, the selective determination of PY in the presence of other water soluble vitamins such as ascorbic acid and riboflavin was also demonstrated. Using amperometry, detection of 100nM PY was achieved and the detection limit was found to be 5.6×10(-8)M (S/N=3). The practical application of the present method was demonstrated by determining the concentration of PY in human blood serum and commercial drugs. Copyright © 2016 Elsevier Inc. All rights reserved.

  14. Dispersion of multi-wall carbon nanotubes in polyhistidine: Characterization and analytical applications

    International Nuclear Information System (INIS)

    Dalmasso, Pablo R.; Pedano, María L.; Rivas, Gustavo A.

    2012-01-01

    Highlights: ► Polyhistidine (Polyhis) is an efficient dispersing agent of MWCNT. ► MWCNT/Polyhis ratio and sonication time are critical variables when dispersing MWCNT. ► MWCNT–Polyhis deposited at GCE largely catalyzes the oxidation of ascorbic acid. ► GCE/MWCNT–Polyhis allows the selective and sensitive quantification of UA and Do. - Abstract: We report for the first time the use of polyhistidine (Polyhis) to efficiently disperse multiwall carbon nanotubes (MWCNTs). The optimum dispersion MWCNT–Polyhis was obtained by sonicating for 30 min 1.0 mg mL −1 MWCNTs in 0.25 mg mL −1 Polyhis solution prepared in 75:25 (v/v) ethanol/0.200 M acetate buffer solution pH 5.00. The dispersion was characterized by scanning electron microscopy, and by cyclic voltammetry and amperometry using ascorbic acid as redox marker. The modification of glassy carbon electrodes with MWCNT–Polyhis produces a drastic decrease in the overvoltage for the oxidation of ascorbic acid (580 mV) at variance with the response observed at glassy carbon electrodes modified just with Polyhis, where the charge transfer is more difficult due to the blocking effect of the polymer. The reproducibility for the sensitivities obtained after 10 successive calibration plots using the same surface was 6.3%. The MWCNT-modified glassy carbon electrode demonstrated to be highly stable since after 45 days storage at room temperature the response was 94.0% of the original. The glassy carbon electrode modified with MWCNT–Polyhis dispersion was successfully used to quantify dopamine or uric acid at nanomolar levels, even in the presence of large excess of ascorbic acid. Determinations of uric acid in human blood serum samples demonstrated a very good correlation with the value reported by Wienner laboratory.

  15. Central and peripheral contributions to dynamic changes in nucleus accumbens glucose induced by intravenous cocaine

    Directory of Open Access Journals (Sweden)

    Ken Taro Wakabayashi

    2015-02-01

    Full Text Available The pattern of neural, physiological and behavioral effects induced by cocaine is consistent with metabolic neural activation, yet direct attempts to evaluate central metabolic effects of this drug have produced controversial results. Here, we used enzyme-based glucose sensors coupled with high-speed amperometry in freely moving rats to examine how intravenous cocaine at a behaviorally active dose affects extracellular glucose levels in the nucleus accumbens (NAc, a critical structure within the motivation-reinforcement circuit. In drug-naive rats, cocaine induced a bimodal increase in glucose, with the first, ultra-fast phasic rise appearing during the injection (latency 6-8 s; ~50 µM or ~5% of baseline followed by a larger, more prolonged tonic elevation (~100 µM or 10% of baseline, peak ~15 min. While the rapid, phasic component of the glucose response remained stable following subsequent cocaine injections, the tonic component progressively decreased. Cocaine-methiodide, cocaine’s peripherally acting analog, induced an equally rapid and strong initial glucose rise, indicating cocaine’s action on peripheral neural substrates as its cause. However, this analog did not induce increases in either locomotion or tonic glucose, suggesting direct central mediation of these cocaine effects. Under systemic pharmacological blockade of dopamine transmission, both phasic and tonic components of the cocaine-induced glucose response were only slightly reduced, suggesting a significant role of non-dopamine mechanisms in cocaine-induced accumbal glucose influx. Hence, intravenous cocaine induces rapid, strong inflow of glucose into NAc extracellular space by involving both peripheral and central, non-dopamine drug actions, thus preventing a possible deficit resulting from enhanced glucose use by brain cells.

  16. Development of sensitive amperometric hydrogen peroxide sensor using a CuNPs/MB/MWCNT-C_6_0-Cs-IL nanocomposite modified glassy carbon electrode

    International Nuclear Information System (INIS)

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

    2016-01-01

    A sensitive hydrogen peroxide (H_2O_2) sensor was constructed based on copper nanoparticles/methylene blue/multiwall carbon nanotubes–fullerene–chitosan–ionic liquid (CuNPs/MB/MWCNTs–C_6_0–Cs–IL) nanocomposites. The MB/MWCNTs–C_6_0–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–C_6_0–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 H_2O_2 in the range of 0.2 μM to 2.0 mM, and the detection limit is 55.0 nM (S/N = 3). In addition, the modified electrode was used to determine H_2O_2 concentration in human blood serum sample with satisfactory results. - Highlights: • CuNPs/MB/MWCNT-C_6_0-Cs-IL/GC electrode was constructed by layer-by-layer method. • The catalytic performance of the sensor was studied with the use of amperometric technique. • The constructed sensor showed enhanced electrocatalytic activity toward the reduction of H_2O_2. • The CuNPs/MB/MWCNT-C_6_0-Cs-IL/GC electrode demonstrated high stability for the detection of H_2O_2.

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

    International Nuclear Information System (INIS)

    Kurd, Masoumeh; Salimi, Abdollah; Hallaj, Rahman

    2013-01-01

    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 (k s ) 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 CCl 3 COOH to CH 3 COOH have been clearly seen. The observed chronoamperometric currents are linearly increased with the concentration of TCA at concentration range up to 20 mM. 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. Highlights: ► Phthalocyanine (PC) and Fe(II) immobilized onto MWCNTs modified GC electrode. ► A pair of well-defined redox couple correspondent to (Fe(III)Pc/Fe(II)Pc) observed. ► Modified electrode shows excellent catalytic activity to electroreduction of CCl 3 COOH. ► Amperometry and cyclic voltammetry techniques were used for detection of CCl 3 COOH. ► Detection limit and sensitivity were 2.0 μM and 0.10 μA μM −1 cm −2 , respectively

  18. Development of an on-line electrochemical analyser for trace level aluminium

    International Nuclear Information System (INIS)

    Chow, Christopher W.K.; Thomas, Shaun D.; Davey, David E.; Mulcahy, Dennis E.; Drikas, Mary

    2003-01-01

    An in-house designed computerised flow injection (FI) system for low-level aluminium analysis is examined. A simple, low cost electrochemical detection system has been implemented with computerised control and data acquisition system. The system consists of a commercial electrochemical analyser, FI components (manifold, pumps and valves) and an in-house designed control system to perform automated analysis. This system was developed to study aluminium speciation in water, particularly for drinking water. The analytical technique was based upon the complexation reaction between aluminium and a ligand--DASA (1,2-dihydroxy-anthraquinone-3-sulphonic acid). 'Labile' and total aluminium concentrations, Al labile and Al total , respectively, were determined by measuring the sample before and after UV irradiation by amperometry at +0.6 V. The limit of detection for this technique was 10 μg/l (0.37 μM) and the linear calibration range was up to 1.6 mg/l (60 μM) with r 2 value of 0.999. The Al labile /Al total ratios of the water treated by 40, 80 and 100 mg/l of alum using a laboratory scale pilot plant to simulate conventional drinking water treatment processes were found to be 0.4, 0.5 and 0.8, respectively. These results indicated that when higher alum dose was employed, the residual aluminium was present mostly as the 'labile' species. Whereas, if the treatment process was not running at its optimum condition (underdosing), a large portion of aluminium was present as natural organic matter (NOM) - aluminium complexes in the treated water. The system offers a practical and effective means of providing extended knowledge of residual aluminium in drinking water

  19. An electrochemical approach: Switching Structures of rare earth metal Praseodymium hexacyanoferrate and its application to sulfite sensor in Red Wine

    International Nuclear Information System (INIS)

    Devadas, Balamurugan; Sivakumar, Mani; Chen, Shen Ming; Cheemalapati, Srikanth

    2015-01-01

    Graphical abstract: Nucleation and growth of PrHCF and its application to sulfite oxidation in wine samples. - Highlights: • Electrochemical synthesis of PrHCF. • Switching structures of PrHCF. • Sulfite electrochemical sensor. • Wide linear range and low limit of detection. • Real sample application. - Abstract: Herein, we report a shape-controlled preparation of Praseodymium hexacyanoferrate (PrHCF) using a simple electrochemical technique. The electrochemically fabricated PrHCF modified glassy carbon electrodes (GCE) shows an excellent electrocatalytic activity towards sulfite oxidation. The morphology of PrHCF particles were controlled by carefully changing various synthesis conditions including electrochemical technique (cyclic voltammetry, amperometry and chemical), cations in the supporting electrolyte (K + , Na + , Li + and H + ), deposition cycles, molar ratio of precursors, and applied potential (-.2,0 and 0.2 V). The morphologies of the PrHCF was elucidated using scanning electron microscopy (SEM). The as-synthesized PrHCF was characterized using X-ray diffraction pattern (XRD), Infra-red (IR) and energy dispersive X-ray spectroscopy (EDX). The electrochemical oxidation of sulfite on PrHCF modified GCE was investigated using cyclic voltammetry (CV) and linear sweep voltammetry (LSV). The sensitivity of the as-developed sulfite sensor was determined to be 0.036 μA μM −1 cm −2 . The low limit of detection was determined to be 2.15 μM. The real time application of PrHCF modified GCE was confirmed through the determination of sulfite from red wine and tap water samples

  20. Electrochemical estimation of the polyphenol index in wines using a laccase biosensor.

    Science.gov (United States)

    Gamella, M; Campuzano, S; Reviejo, A J; Pingarrón, J M

    2006-10-18

    The use of a laccase biosensor, under both batch and flow injection (FI) conditions, for a rapid and reliable amperometric estimation of the total content of polyphenolic compounds in wines is reported. The enzyme was immobilized by cross-linking with glutaraldehyde onto a glassy carbon electrode. Caffeic acid and gallic acid were selected as standard compounds to carry out such estimation. Experimental variables such as the enzyme loading, the applied potential, and the pH value were optimized, and different aspects regarding the operational stability of the laccase biosensor were evaluated. Using batch amperometry at -200 mV, the detection limits obtained were 2.6 x 10(-3) and 7.2 x 10(-4) mg L(-1) gallic acid and caffeic acid, respectively, which compares advantageously with previous biosensor designs. An extremely simple sample treatment consisting only of an appropriate dilution of wine sample with the supporting electrolyte solution (0.1 mol L(-1) citrate buffer of pH 5.0) was needed for the amperometric analysis of red, rosé, and white wines. Good correlations were found when the polyphenol indices obtained with the biosensor (in both the batch and FI modes) for different wine samples were plotted versus the results achieved with the classic Folin-Ciocalteu method. Application of the calibration transfer chemometric model (multiplicative fitting) allowed that the confidence intervals (for a significance level of 0.05) for the slope and intercept values of the amperometric index versus Folin-Ciocalteu index plots (r = 0.997) included the unit and zero values, respectively. This indicates that the laccase biosensor can be successfully used for the estimation of the polyphenol index in wines when compared with the Folin-Ciocalteu reference method.

  1. Dispersion of multi-wall carbon nanotubes in polyhistidine: Characterization and analytical applications

    Energy Technology Data Exchange (ETDEWEB)

    Dalmasso, Pablo R. [INFIQC, Departamento de Fisicoquimica, Facultad de Ciencias Quimicas, Universidad Nacional de Cordoba, Ciudad Universitaria, 5000 Cordoba (Argentina); Pedano, Maria L., E-mail: mlpedano@fcq.unc.edu.ar [INFIQC, Departamento de Fisicoquimica, Facultad de Ciencias Quimicas, Universidad Nacional de Cordoba, Ciudad Universitaria, 5000 Cordoba (Argentina); Rivas, Gustavo A., E-mail: grivas@mail.fcq.unc.edu.ar [INFIQC, Departamento de Fisicoquimica, Facultad de Ciencias Quimicas, Universidad Nacional de Cordoba, Ciudad Universitaria, 5000 Cordoba (Argentina)

    2012-01-13

    Highlights: Black-Right-Pointing-Pointer Polyhistidine (Polyhis) is an efficient dispersing agent of MWCNT. Black-Right-Pointing-Pointer MWCNT/Polyhis ratio and sonication time are critical variables when dispersing MWCNT. Black-Right-Pointing-Pointer MWCNT-Polyhis deposited at GCE largely catalyzes the oxidation of ascorbic acid. Black-Right-Pointing-Pointer GCE/MWCNT-Polyhis allows the selective and sensitive quantification of UA and Do. - Abstract: We report for the first time the use of polyhistidine (Polyhis) to efficiently disperse multiwall carbon nanotubes (MWCNTs). The optimum dispersion MWCNT-Polyhis was obtained by sonicating for 30 min 1.0 mg mL{sup -1} MWCNTs in 0.25 mg mL{sup -1} Polyhis solution prepared in 75:25 (v/v) ethanol/0.200 M acetate buffer solution pH 5.00. The dispersion was characterized by scanning electron microscopy, and by cyclic voltammetry and amperometry using ascorbic acid as redox marker. The modification of glassy carbon electrodes with MWCNT-Polyhis produces a drastic decrease in the overvoltage for the oxidation of ascorbic acid (580 mV) at variance with the response observed at glassy carbon electrodes modified just with Polyhis, where the charge transfer is more difficult due to the blocking effect of the polymer. The reproducibility for the sensitivities obtained after 10 successive calibration plots using the same surface was 6.3%. The MWCNT-modified glassy carbon electrode demonstrated to be highly stable since after 45 days storage at room temperature the response was 94.0% of the original. The glassy carbon electrode modified with MWCNT-Polyhis dispersion was successfully used to quantify dopamine or uric acid at nanomolar levels, even in the presence of large excess of ascorbic acid. Determinations of uric acid in human blood serum samples demonstrated a very good correlation with the value reported by Wienner laboratory.

  2. CO{sub 2} electroreduction: conversion into formic acid and mechanistic aspect in aqueous medium; Electroreduction du CO{sub 2}: conversion en acide formique et aspect mecanistique en milieu aqueux

    Energy Technology Data Exchange (ETDEWEB)

    Innocent, B.; Pasquier, D.; Ropital, F. [Institut Francais du Petrole (IFP), 92 - Rueil-Malmaison (France); Hahn, F.; Leger, J.M.; Kokoh, B. [Poitiers Univ., LaCCO, Equipe Electrocatalyse, UMR 6503 CNRS, 86 (France)

    2007-07-01

    The CO{sub 2} release reduction is nowadays considered as a necessity to limit the climatic change phenomena due to the greenhouse effect. For that, a part of CO{sub 2} could be transformed by its electrochemical reduction on a hydrogen overvoltage electrode as lead. According to the nature of the electrode material and of the electrolyte, CO{sub 2} can be electro catalytically hydrogenated or dimerized. In the conditions presented here (basic aqueous medium, lead electrode), the reagent is in majority reduced into formate, the parasite faradic reaction being the solvent transformation into dihydrogen. The studies carried out by cyclic voltametry have shown that the reducible form of CO{sub 2} is the hydrogeno-carbonate ion; its reduction begins at -1.2 V and reaches a maximum for an electrode potential of -1.6 V vs. ECS. Long intentiostatic electrolyses have then been carried out in an electrolytic circulation cell of 'filter-press' type. The cathode is a lead sheet of 20 cm{sup 2} and a current intensity of -100 mA has been imposed. The chromatographic analyses of the electrolytic solution have allowed to show that the formate selectivity is of 90%. The electroreduction process induces an acido-basic disequilibrium which induces a decrease of the reaction yield. A pH correction is then necessary to obtain great conversions of CO{sub 2} in alkaline medium (pH{>=}7) as follows: HCO{sub 3}{sup -} + H{sub 2}O + 2e{sup -} {yields} HCOO{sup -} + 2 HO{sup -}. In situ reflexion infrared spectroscopy studies, carried out in deuterated aqueous medium and by chrono-amperometry, have shown characteristic bands due to the hydrogeno-carbonate ion (weakly adsorbed) and to the formate produced, required for the understanding of the reactional mechanism. (O.M.)

  3. Reorganization of circuits underlying cerebellar modulation of prefrontal cortical dopamine in mouse models of autism spectrum disorder.

    Science.gov (United States)

    Rogers, Tiffany D; Dickson, Price E; McKimm, Eric; Heck, Detlef H; Goldowitz, Dan; Blaha, Charles D; Mittleman, Guy

    2013-08-01

    Imaging, clinical, and pre-clinical studies have provided ample evidence for a cerebellar involvement in cognitive brain function including cognitive brain disorders, such as autism and schizophrenia. We previously reported that cerebellar activity modulates dopamine release in the mouse medial prefrontal cortex (mPFC) via two distinct pathways: (1) cerebellum to mPFC via dopaminergic projections from the ventral tegmental area (VTA) and (2) cerebellum to mPFC via glutamatergic projections from the mediodorsal and ventrolateral thalamus (ThN md and vl). The present study compared functional adaptations of cerebello-cortical circuitry following developmental cerebellar pathology in a mouse model of developmental loss of Purkinje cells (Lurcher) and a mouse model of fragile X syndrome (Fmr1 KO mice). Fixed potential amperometry was used to measure mPFC dopamine release in response to cerebellar electrical stimulation. Mutant mice of both strains showed an attenuation in cerebellar-evoked mPFC dopamine release compared to respective wildtype mice. This was accompanied by a functional reorganization of the VTA and thalamic pathways mediating cerebellar modulation of mPFC dopamine release. Inactivation of the VTA pathway by intra-VTA lidocaine or kynurenate infusions decreased dopamine release by 50 % in wildtype and 20-30 % in mutant mice of both strains. Intra-ThN vl infusions of either drug decreased dopamine release by 15 % in wildtype and 40 % in mutant mice of both strains, while dopamine release remained relatively unchanged following intra-ThN md drug infusions. These results indicate a shift in strength towards the thalamic vl projection, away from the VTA. Thus, cerebellar neuropathologies associated with autism spectrum disorders may cause a reduction in cerebellar modulation of mPFC dopamine release that is related to a reorganization of the mediating neuronal pathways.

  4. Extracellular levels of lactate, but not oxygen, reflect sleep homeostasis in the rat cerebral cortex.

    Science.gov (United States)

    Dash, Michael B; Tononi, Giulio; Cirelli, Chiara

    2012-07-01

    It is well established that brain metabolism is higher during wake and rapid eye movement (REM) sleep than in nonrapid eye movement (NREM) sleep. Most of the brain's energy is used to maintain neuronal firing and glutamatergic transmission. Recent evidence shows that cortical firing rates, extracellular glutamate levels, and markers of excitatory synaptic strength increase with time spent awake and decline throughout NREM sleep. These data imply that the metabolic cost of each behavioral state is not fixed but may reflect sleep-wake history, a possibility that is investigated in the current report. Chronic (4d) electroencephalographic (EEG) recordings in the rat cerebral cortex were coupled with fixed-potential amperometry to monitor the extracellular concentration of oxygen ([oxy]) and lactate ([lac]) on a second-by-second basis across the spontaneous sleep-wake cycle and in response to sleep deprivation. Basic sleep research laboratory. Wistar Kyoto (WKY) adult male rats. N/A. Within 30-60 sec [lac] and [oxy] progressively increased during wake and REM sleep and declined during NREM sleep (n = 10 rats/metabolite), but with several differences. [Oxy], but not [lac], increased more during wake with high motor activity and/or elevated EEG high-frequency power. Meanwhile, only the NREM decline of [lac] reflected sleep pressure as measured by slow-wave activity, mirroring previous results for cortical glutamate. The observed state-dependent changes in cortical [lac] and [oxy] are consistent with higher brain metabolism during waking and REM sleep in comparison with NREM sleep. Moreover, these data suggest that glycolytic activity, most likely through its link with glutamatergic transmission, reflects sleep homeostasis.

  5. Simultaneous determination of paracetamol and ascorbic acid using tetraoctylammonium bromide capped gold nanoparticles immobilized on 1,6-hexanedithiol modified Au electrode

    International Nuclear Information System (INIS)

    Nair, Santhosh S.; John, S. Abraham; Sagara, Takamasa

    2009-01-01

    Tetraoctylammonium bromide stabilized gold nanoparticles (TOAB-AuNPs) attached to 1,6-hexanedithiol (HDT) modified Au electrode was used for the simultaneous determination of paracetamol (PA) and ascorbic acid (AA) at physiological pH. The attachment of TOAB-AuNPs on HDT modified Au surface was confirmed by attenuated total reflectance (ATR)-FT-IR spectroscopy and atomic force microscope (AFM). The ATR-FT-IR spectrum of TOAB-AuNPs attached to the HDT monolayer showed a characteristic stretching modes corresponding to -CH 2 and -CH 3 of TOAB, confirming the immobilization of AuNPs with surface-protecting TOAB ions on the surface of the AuNPs after being attached to HDT modified Au electrode. AFM image showed that the immobilized AuNPs were spherical in shape and densely packed to a film of ca. 7 nm thickness. Interestingly, TOAB-AuNPs modified electrode shifted the oxidation potential of PA towards less positive potential by 70 mV and enhanced its oxidation current twice when compared to bare Au electrode. In addition, the AuNPs modified electrode separated the oxidation potentials of AA and PA by 210 mV, whereas bare Au electrode failed to resolve them. The amperometry current of PA was increased linearly from 1.50 x 10 -7 to 1.34 x 10 -5 M with a correlation coefficient of 0.9981 and the lowest detection limit was found to be 2.6 nM (S/N = 3). The present method was successfully used to determine the concentration of PA in human blood plasma and commercial drugs.

  6. Simultaneous determination of paracetamol and ascorbic acid using tetraoctylammonium bromide capped gold nanoparticles immobilized on 1,6-hexanedithiol modified Au electrode

    Energy Technology Data Exchange (ETDEWEB)

    Nair, Santhosh S. [Department of Chemistry, Gandhigram Rural University, Gandhigram 624302, Dindigul (India); John, S. Abraham [Department of Chemistry, Gandhigram Rural University, Gandhigram 624302, Dindigul (India)], E-mail: abrajohn@yahoo.co.in; Sagara, Takamasa [Department of Chemistry, Gandhigram Rural University, Gandhigram 624302, Dindigul (India)], E-mail: sagara@nagasaki-u.ac.jp

    2009-11-30

    Tetraoctylammonium bromide stabilized gold nanoparticles (TOAB-AuNPs) attached to 1,6-hexanedithiol (HDT) modified Au electrode was used for the simultaneous determination of paracetamol (PA) and ascorbic acid (AA) at physiological pH. The attachment of TOAB-AuNPs on HDT modified Au surface was confirmed by attenuated total reflectance (ATR)-FT-IR spectroscopy and atomic force microscope (AFM). The ATR-FT-IR spectrum of TOAB-AuNPs attached to the HDT monolayer showed a characteristic stretching modes corresponding to -CH{sub 2} and -CH{sub 3} of TOAB, confirming the immobilization of AuNPs with surface-protecting TOAB ions on the surface of the AuNPs after being attached to HDT modified Au electrode. AFM image showed that the immobilized AuNPs were spherical in shape and densely packed to a film of ca. 7 nm thickness. Interestingly, TOAB-AuNPs modified electrode shifted the oxidation potential of PA towards less positive potential by 70 mV and enhanced its oxidation current twice when compared to bare Au electrode. In addition, the AuNPs modified electrode separated the oxidation potentials of AA and PA by 210 mV, whereas bare Au electrode failed to resolve them. The amperometry current of PA was increased linearly from 1.50 x 10{sup -7} to 1.34 x 10{sup -5} M with a correlation coefficient of 0.9981 and the lowest detection limit was found to be 2.6 nM (S/N = 3). The present method was successfully used to determine the concentration of PA in human blood plasma and commercial drugs.

  7. Flow-based method for epinephrine determination using a solid reactor based on molecularly imprinted poly(FePP-MAA-EGDMA)

    International Nuclear Information System (INIS)

    Sartori, Lucas Rossi; Santos, Wilney de Jesus Rodrigues; Kubota, Lauro Tatsuo; Segatelli, Mariana Gava; Tarley, Cesar Ricardo Teixeira

    2011-01-01

    A solid phase reactor based on molecularly imprinted poly(iron (III) protoporphyrin-methacrylic acid-ethylene glycol dimethacrylate) (MIP-MAA) has been synthesized by bulk method and applied as an selective material for the epinephrine determination in the presence of hydrogen peroxide. In order to prove the selective behaviour of MIP, two blank polymers named non-imprinted polymer (NIP1), non-imprinted polymer in the absence of hemin (NIP2) as well as a poly(iron (III) protoporphyrin-4-vynilpyridine-ethylene glycol dimethacrylate) (MIP-4VPy) were synthesized. The epinephrine-selective MIP-MAA reactor was used in a flow injection system, in which an epinephrine solution (120 μL) at pH 8.0 percolates in the presence of hydrogen peroxide (300 μmol L -1 ) through MIP-MAA. The oxidation of epinephrine by hydrogen peroxide is increased by using MIP-MAA, being the product formed monitored by amperometry at 0.0 V vs. Ag/AgCl. The MIP-MAA showed better selective behaviour than NIP1, NIP2 and MIP-4VPy, demonstrating the effectiveness of molecular imprinting effect. Highly improved response was observed for epinephrine in detriment of similar substances (phenol, ascorbic acid, methyl-L-DOPA, p-aminophenol, catechol, L-DOPA and guaiacol). The method provided a calibration curve ranging from 10 to 500 μmol L -1 and a limit of detection of 5.2 μmol L -1 . Kinetic data indicated a value of maximum rate V max (0.993 μA) and apparent Michaelis-Menten constant of K m app (725.6 μmol L -1 ). The feasibility of biomimetic solid reactor was attested by its successful application for epinephrine determination in pharmaceutical formulation.

  8. The Effect of Multilayer Gold Nanoparticles on the Electrochemical Response of Ammonium Ion Biosensor Based on Alanine Dehydrogenase Enzyme

    Directory of Open Access Journals (Sweden)

    Tan Ling Ling

    2011-01-01

    Full Text Available The use of multilayer of gold nanoparticles (AuNPs attached on gold electrode surface via thiol chemistry to fabricate an ammonium (NH4+ ion biosensor based on alanine dehydrogenase (AlaDH was investigated. The approach of the study was based on construction of biosensor by direct deposition of AuNPs and 1,8-octanedithiol (C8-DT onto the gold electrode surface. For the immobilisation of enzyme, 2-mercaptoethanol (2BME was first covalently attached to AlaDH via esther bonding and then followed by chemically attached the 2BME-modified AlaDH (2BME-AlaDH moiety onto the AuNPs electrode via the exposed thiol group of 2BME. The resulting biosensor response was examined by means of amperometry for the quantification of NH4+ ion. In the absence of enzyme attachment, the use of three layers of AuNPs was found to improve the electrochemistry of the gold electrode when compared with no AuNPs was coated. However, when more than three layers of AuNPs were coated, the electrode response deteriorated due to excessive deposition of C8-DT. When AlaDH was incoporated into the AuNPs modified electrode, a linear response to NH4+ ion over the concentration range of 0.1–0.5 mM with a detection limit of 0.01 mM was obtained. In the absence of AuNPs, the NH4+ ion biosensor did not exhibit any good linear response range although the current response was observed to be higher. This work demonstrated that the incorporation of AuNPs could lead to the detection of higher NH4+ ion concentration without the need of dilution for high NH4+ ion concentration samples with a rapid response time of <1 min.

  9. Synthesis of palladium nanoparticle modified reduced graphene oxide and multi-walled carbon nanotube hybrid structures for electrochemical applications

    International Nuclear Information System (INIS)

    Hu, Jie; Zhao, Zhenting; Zhang, Jun; Li, Gang; Li, Pengwei; Zhang, Wendong; Lian, Kun

    2017-01-01

    Graphical abstract: A sensitive hydrazine electrochemical sensor was fabricated by using palladium (Pd) nanoparticle functionalized reduced graphene oxide (rGO) and multi-walled carbon nanotube (MWCNTs) hybrid structures (Pd/rGO-MWCNTs). - Highlights: • rGO-MWCNTs hybrid structures and Pd nanoparticles are prepared using electrochemical methods. • rGO-MWCNTs hybrid films are used as supports and co-catalysts for Pd nanoparticles. • The Pd/rGO-MWCNTs hybrid structure based sensor shows an ultra-high sensitivity of 7.09 μA μM"−"1 cm"−"2 and a low detection limit of 0.15 μM. • The proposed electrochemical sensor exhibits excellent selectivity. - Abstract: In this work, palladium (Pd) nanoparticles functionalized reduced graphene oxide (rGO) and multi-walled carbon nanotubes (MWCNTs) hybrid structures (Pd/rGO-MWCNTs) were successfully prepared by a combination of electrochemical reduction with electrodeposition method. The morphology, structure, and composition of the Pd/rGO-MWCNTs hybrid were characterized by scanning electron microscopy, transmission electron microscopy and energy dispersive spectroscopy. The as-synthesized hybrid structures were modified on the glassy carbon electrode (GCE) and further utilized for hydrazine sensing. Electrochemical impedance spectroscopic, cyclic voltammetry and single-potential amperometry experiments were carried out on Pd/rGO-MWCNTs hybrid structures to investigate the interface properties and sensing performance. The measured results demonstrate that the fabricated Pd/rGO-MWCNTs/GCE sensor show a high sensitivity of 7.09 μA μM"−"1 cm"−"2 in a large concentration range of 1.0 to 1100 μM and a low detection limit of 0.15 μM. Moreover, the as-prepared sensor exhibits good selectivity and stability for the determination of hydrazine under interference conditions.

  10. Molecularly imprinted polyaniline-ferrocene-sulfonic acid-Carbon dots modified pencil graphite electrodes for chiral selective sensing of D-Ascorbic acid and L-Ascorbic acid: A clinical biomarker for preeclampsia

    International Nuclear Information System (INIS)

    Pandey, Indu; Jha, Shashank Shekhar

    2015-01-01

    Highlights: • Pencil graphite electrode was non-covalently functionalized by C-dots. • Electrochemically synthesized ferrocene-sulfonic acid doped PANI film was used as chiral recognition element. • Electrochemical chiral sensing of L-ascorbic acid and D-ascorbic acid was carried out. • L-ascorbic acid determination was done in aqueous, biological and pharmaceutical samples at nM level. - Abstract: A simple and novel method is proposed for chiral separation of L-ascorbic acid and D-ascorbic acid in human cerebrospinal fluids and blood plasma samples. Electro-polymerized molecularly imprinted poly-aniline ferrocenesulfonic acid-C-dots modified pencil graphite electrodes was successfully applied for separation and quantification of D-/L-ascorbic acid in aqueous and some biological samples. Parameters, important to control the performance of the electrochemical sensor were investigated and optimized, including the effects of pH, monomer- template ratios, electropolymerization cycles and scan rates. The molecularly imprinted film exhibited a high chiral selectivity and sensitivity towards D-ascorbic acid and L-ascorbic acid respectively. The surface morphologies and electrochemical properties of the proposed sensor were characterized by scanning electron microscopy, cyclic voltammetry, difference pulse voltammetry, chrono-amperometry and electrochemical impedance spectroscopy. L-ascorbic acid selective sensor shows excellent selectivity towards the L-ascorbic acid in comparison to D- ascorbic acid vice versa for D- ascorbic acid selective sensor. Under optimal conditions the linear range of the calibration curve for L- ascorbic acid and D- ascorbic acid was 6.0–165.0 nM and 6.0–155.0 nM, with the detection limit of 0.001 nM and 0.002 nM. Chiral detection of L-ascorbic acid was successfully carried out in pharmaceuticals and human plasma samples (pregnant women and non pregnant women) via proposed sensor with good selectivity and sensitivity.

  11. Non-enzymatic hydrogen peroxide detection at NiO nanoporous thin film- electrodes prepared by physical vapor deposition at oblique angles

    International Nuclear Information System (INIS)

    Salazar, Pedro; Rico, Victor; González-Elipe, Agustín R.

    2017-01-01

    Highlights: • A non-enzymatic sensor for H 2 O 2 detection based on nickel thin film is reported. • Nanostructured nickel thin films are prepared by physical vapor deposition at oblique angles. • Main analytical parameters were obtained under optimal operation conditions. • Sensors depict an outstanding selectivity and a high stability. • Sensors are successfully used to determine H 2 O 2 in antiseptic solutions. - Abstract: In this work we report a non-enzymatic sensor for hydrogen peroxide (H 2 O 2 ) detection based on nanostructured nickel thin films prepared by physical vapor deposition at oblique angles. Porous thin films deposited on ITO substrates were characterized by X-ray diffraction analysis, scanning electron microcopy (SEMs), X-ray photoelectron spectroscopy (XPS) and electrochemical techniques such as Cyclic Voltammetry (CV) and Constant Potential Amperometry (CPA). The microstructure of the thin films consisted of inclined and separated Ni nanocolumns forming a porous thin layer of about 500 nm thickness. Prior to their use, the films surface was electrochemically modified and the chemical state studied by CV and XPS analysis. These techniques also showed that Ni 2+ /Ni 3+ species were involved in the electrochemical oxidation and detection of H 2 O 2 in alkaline medium. Main analytical parameters such as sensitivity (807 mA M −1 cm −2 ), limit of detection (3.22 μM) and linear range (0.011–2.4 mM) were obtained under optimal operation conditions. Sensors depicted an outstanding selectivity and a high stability and they were successfully used to determine H 2 O 2 concentration in commercial antiseptic solutions.

  12. Fluctuations in nucleus accumbens extracellular glutamate and glucose during motivated glucose-drinking behavior: dissecting the neurochemistry of reward.

    Science.gov (United States)

    Wakabayashi, Ken T; Myal, Stephanie E; Kiyatkin, Eugene A

    2015-02-01

    While motivated behavior involves multiple neurochemical systems, few studies have focused on the role of glutamate, the brain's excitatory neurotransmitter, and glucose, the energetic substrate of neural activity in reward-related neural processes. Here, we used high-speed amperometry with enzyme-based substrate-sensitive and control, enzyme-free biosensors to examine second-scale fluctuations in the extracellular levels of these substances in the nucleus accumbens shell during glucose-drinking behavior in trained rats. Glutamate rose rapidly after the presentation of a glucose-containing cup and before the initiation of drinking (reward seeking), decreased more slowly to levels below baseline during consumption (sensory reward), and returned to baseline when the ingested glucose reached the brain (metabolic reward). When water was substituted for glucose, glutamate rapidly increased with cup presentation and in contrast to glucose drinking, increased above baseline after rats tasted the water and refused to drink further. Therefore, extracellular glutamate show distinct changes associated with key events of motivated drinking behavior and opposite dynamics during sensory and metabolic components of reward. In contrast to glutamate, glucose increased at each stimulus and behavioral event, showing a sustained elevation during the entire behavior and a robust post-ingestion rise that correlated with the gradual return of glutamate levels to their baseline. By comparing active drinking with passive intra-gastric glucose delivery, we revealed that fluctuations in extracellular glucose are highly dynamic, reflecting a balance between rapid delivery because of neural activity, intense metabolism, and the influence of ingested glucose reaching the brain. Published 2014. This article is a U.S. Government work and is in the public domain in the USA.

  13. Determination of ascorbic acid in pharmaceutical preparation and fruit juice using modified carbon paste electrode

    Directory of Open Access Journals (Sweden)

    Simona Žabčíková

    2016-06-01

    Full Text Available Acrobic acid is key substance in the human metabolism and the rapid and accurate determination in food is of a great interest. Ascorbic acid is an electroactive compound, however poorly responded on the bare carbon paste electrodes. In this paper, brilliant cresyl blue and multi-walled carbon nanotubes were used for the modification of carbon paste electrode. Brilliant cresyl blue acts as a mediator improving the transition of electrons, whereas multiwalled carbon nanotubes increased the surface of the electrode. Both brilliant cresyl blue and multiwalled carbon nanotubes were added directly to the composite material. The electrochemical behavior of modified electode was determined in electrolyte at various pH, and the effect of the scan rate was also performed. It was shown that the electrochemical process on the surface of the modified carbon paste electrode was diffusion-controlled. The resulted modified carbon paste electrode showed a good electrocatalytic activity towards the oxidation of ascorbic acid at a reduced overpotential of +100 mV descreasing the risk of interferences. A linear response of the ascorbic acid oxidation current measured by the amperometry in the range of 0.1 - 350 µmol.L-1 was obtained applying the sensor for the standard solution. The limit of detection and limit of quantification was found to be 0.05 and 0.15 µmol.L-1, respectively. The novel method was applied for the determination of ascorbic acid in pharmaceutical vitamin preparation and fruit juice, and the results were in good agreement with the standard HPLC method. The presented modification of carbon paste electrode is suitable for the fast, sensitive and very accurate determination of ascorbic acid in fruit juices and pharmaceutical preparation.

  14. Synthesis and characterization of cobalt-nichel oxides for the oxygen formation reaction

    International Nuclear Information System (INIS)

    Morales G, P.

    2001-01-01

    In this work the compounds of cobalt and nickel oxides and the mixtures of cobalt-nickel were prepared which were characterized and evaluated as electrocatalysts in the oxygen release reaction in alkaline media. The compounds were synthesised by the sol-gel method: heated at 400 and 500 Centigrade. The compounds characterization was realized by thermogravimetry, X-ray diffraction and Scanning electron microscopy. As the Co 3 O 4 and the Ni O as the mixtures Ni O/Co 3 O 4 were obtained as a porous material with a small particle size, characteristics which are presented by cause of the low temperature of synthesis. The electrocatalytic evaluation for the synthesised compounds for the oxygen release reaction was realized by cyclic volt amperometry in a 0.5M KOH solution. The oxides mixtures presented a well electrocatalytic activity to be used in the electrochemical release of oxygen. The current density and the electrochemically active area, in all the cases of mixtures is very higher to the Co 3 O 4 and Ni O ones. Observing with greater clearness the synergic effects, in the obtained mixture at 400 C. The oxides mixtures heated at 400 C were stables for the oxygen formation reaction. Therefore it is be able to say that the Ni O/Co 3 O 4 mixture counts on a great reactive area: electrocatalytic characteristic desirable to be a material used as anode in the electrolysis of water, which increases the oxygen release in the anode and so the hydrogen release in the cathode. (Author)

  15. Li ion transport in sputter deposited LiCoO{sub 2} thin films and glassy borate membranes

    Energy Technology Data Exchange (ETDEWEB)

    Stockhoff, Tobias; Gallasch, Tobias; Schmitz, Guido [Westfaelische Wilhelms-Universitaet Muenster, Institut fuer Materialphysik, Muenster (Germany)

    2010-07-01

    LiCoO{sub 2} membranes are key components of current battery technology. We investigate sputter-deposited thin films of these materials aiming at the application in all-solid-state thin film batteries. For this, LiCoO{sub 2} films (10-200 nm) were deposited onto ITO-coated glass substrates by ion beam sputtering. In addition, a part of these films are coated by an ion-conductive membrane of Li{sub 2}O-B{sub 2}O{sub 3} glasses in the thickness range of 50 to 300 nm. Structural, chemical and electrical properties of the layers are studied by means of TEM(EELS) and various electrical methods (cyclic voltammetry, chrono-amperometry/-potentiometry). Since the color of the LiCoO{sub 2} films changes from red-brown to grey during de-intercalation of Li and the substrate as well as the glassy membrane deposited on top are optical transparent, reversible Li de- and intercalation can be directly demonstrated and quantified by a measurement of light transmission through the layered system. Samples coated with an ion-conductive membrane reveal a characteristic delay in switching optical transparency which is due to the slower transport across the membrane. Varying the thickness of the glassy membrane, the d.c. ion-conductivity and permeation through the membrane is determined quantitatively. Using thin membranes in the range of a few tens of nanometers the critical current densities are way sufficient for battery applications.

  16. Dual mode antimony electrode for simultaneous measurements of PO2 and pH.

    Science.gov (United States)

    Sjöberg, F; Nilsson, G

    2000-01-01

    In biomedical research and clinical medicine there is a demand for potent sensors to measure the components that make up blood gas analyses. Today, as when the electrochemical PO2, PCO2 and pH electrodes were first introduced, these measurements are usually made with the same type of sensor technology. The aims of the present study were, firstly, to find out whether the platinum cathode in the Clark electrode can be replaced by antimony for oxygen measurements (amperometry (A)); secondly, whether, during oxygen measurements, the inherent corrosion potential of the antimony metal can be used for measurement of pH in the same measurement area (potentiometry (P)). An electrode of purified, crystallographically orientated monocrystalline antimony (COMA) connected to a reference electrode (silver-silver chloride) was used for the P measurements. Measurements of A (at -900 mV) and P were made in an aqueous environment regulated for oxygen, pH, and temperature. Reproducible oxygen sensitivities of 0.925 nA/% oxygen (2% CV (coefficient of variation)) (A), 10.7 mV/% (P), and 0.7 mV/% (P) were found in the oxygen range: 0-21%, <5%, and above 5%, respectively. The pH sensitivity was 57 mV/pH unit (P). Oxygen and pH measurements were less accurate at oxygen concentrations close to 0%. Both the oxygen and pH part of the composite electrode signal can be identified by this dual mode technique (A and P). The sensor seems to be promising as it provides measurements of two separate variables (oxygen and pH) and also has the desirable characteristics of a solid state sensor.

  17. New approach for monitoring fish stress: A novel enzyme-functionalized label-free immunosensor system for detecting cortisol levels in fish.

    Science.gov (United States)

    Wu, Haiyun; Ohnuki, Hitoshi; Ota, Shirei; Murata, Masataka; Yoshiura, Yasutoshi; Endo, Hideaki

    2017-07-15

    Fishes display a wide variation in their physiological responses to stress, which is clearly evident in the plasma corticosteroid changes, chiefly cortisol levels in fish. As a well-known indicator of fish stress, a simple and rapid method for detecting cortisol changes especially sudden increases is desired. In this study, we describe an enzyme-functionalized label-free immunosensor system for detecting fish cortisol levels. Detection of cortisol using amperometry was achieved by immobilizing both anti-cortisol antibody (selective detection of cortisol) and glucose oxidase (signal amplification and non-toxic measurement) on an Au electrode surface with a self-assembled monolayer. This system is based on the maximum glucose oxidation output current change induced by the generation of a non-conductive antigen-antibody complex, which depends on the levels of cortisol in the sample. The immunosensor responded to cortisol levels with a linear decrease in the current in the range of 1.25-200ngml -1 (R=0.964). Since the dynamic range of the sensor can cover the normal range of plasma cortisol in fish, the samples obtained from the fish did not need to be diluted. Further, electrochemical measurement of one sample required only ~30min. The sensor system was applied to determine the cortisol levels in plasma sampled from Nile tilapia (Oreochromis niloticus), which were then compared with levels of the same samples determined using the conventional method (ELISA). Values determined using both methods were well correlated. These findings suggest that the proposed label-free immunosensor could be useful for rapid and convenient analysis of cortisol levels in fish without sample dilution. We also believe that the proposed system could be integrated in a miniaturized potentiostat for point-of-care cortisol detection and useful as a portable diagnostic in fish farms in the future. Copyright © 2016 Elsevier B.V. All rights reserved.

  18. High-performance glucose biosensor based on chitosan-glucose oxidase immobilized polypyrrole/Nafion/functionalized multi-walled carbon nanotubes bio-nanohybrid film.

    Science.gov (United States)

    Shrestha, Bishnu Kumar; Ahmad, Rafiq; Mousa, Hamouda M; Kim, In-Gi; Kim, Jeong In; Neupane, Madhav Prasad; Park, Chan Hee; Kim, Cheol Sang

    2016-11-15

    A highly electroactive bio-nanohybrid film of polypyrrole (PPy)-Nafion (Nf)-functionalized multi-walled carbon nanotubes (fMWCNTs) nanocomposite was prepared on the glassy carbon electrode (GCE) by a facile one-step electrochemical polymerization technique followed by chitosan-glucose oxidase (CH-GOx) immobilization on its surface to achieve a high-performance glucose biosensor. The as-fabricated nanohybrid composite provides high surface area for GOx immobilization and thus enhances the enzyme-loading efficiency. The structural characterization revealed that the PPy-Nf-fMWCNTs nanocomposite films were uniformly formed on GCE and after GOx immobilization, the surface porosities of the film were decreased due to enzyme encapsulation inside the bio-nanohybrid composite materials. The electrochemical behavior of the fabricated biosensor was investigated by cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS), and amperometry measurements. The results indicated an excellent catalytic property of bio-nanohybrid film for glucose detection with improved sensitivity of 2860.3μAmM(-1)cm(-2), the linear range up to 4.7mM (R(2)=0.9992), and a low detection limit of 5μM under a signal/noise (S/N) ratio of 3. Furthermore, the resulting biosensor presented reliable selectivity, better long-term stability, good repeatability, reproducibility, and acceptable measurement of glucose concentration in real serum samples. Thus, this fabricated biosensor provides an efficient and highly sensitive platform for glucose sensing and can open up new avenues for clinical applications. Copyright © 2016 Elsevier Inc. All rights reserved.

  19. Kinetics modelling of the concentrated nitric acid reduction on 304L stainless steel

    International Nuclear Information System (INIS)

    Benoit, Marie

    2016-01-01

    In France, the spent nuclear fuel reprocessing involves the use of nitric acid at various concentrations and temperatures. The corrosiveness of these nitric mixtures leads to the use of corrosion resistant materials such as austenitic stainless steels (SS), which naturally forms a protective oxide layer under those conditions. The goal of this work is to study the influence of the passive layer on the mechanism and kinetics of concentrated nitric acid reduction reaction (NRR). We firstly focused on a single step in the reduction reaction (Fe(III)/Fe(II) couple in acidic solution) on passivated zirconium with different oxide layer thicknesses. The electrochemical impedance spectroscopy can lead to estimate the semiconducting properties of the film: the space charge capacitance (from the Mott-Schottky equation) allowed to estimate the number of charge carriers in the oxide. We experimentally compare the NRR on gold (on which no passive layer is formed) and SS, respectively. The chemical composition (chromium enrichment) and thickness of the SS passive layer are characterized by electrochemical impedance spectroscopy (EIS) and X-ray photoelectron spectroscopy (XPS), and the mechanism and kinetics of NRR are studied by chrono-amperometry and EIS. On gold electrode, two mechanisms occur successively as a function of cathodic overpotential. at lower over potentials (0.85≤E/SHE≤1.15 V) we propose that NRR follows the Vetter's mechanism, whereas at higher over potentials (0.65≤E/ESH≤ 0.85 V), Schmid's mechanism may occur. On SS, the presence of the passive layer slows down the NRR by a factor 10"4. Moreover, depending on the experimental conditions (4 M to 8 M, 40 C to 100 C) Schmid's mechanism may occur or not in the potential range investigated. Finally, based on the EIS results, we propose a quantitative modelling of the NRR mechanism on stainless steel electrodes. (author) [fr

  20. Adenoviral vectors for highly selective gene expression in central serotonergic neurons reveal quantal characteristics of serotonin release in the rat brain

    Directory of Open Access Journals (Sweden)

    Teschemacher Anja G

    2009-03-01

    Full Text Available Abstract Background 5-hydroxytryptamine (5 HT, serotonin is one of the key neuromodulators in mammalian brain, but many fundamental properties of serotonergic neurones and 5 HT release remain unknown. The objective of this study was to generate an adenoviral vector system for selective targeting of serotonergic neurones and apply it to study quantal characteristics of 5 HT release in the rat brain. Results We have generated adenoviral vectors which incorporate a 3.6 kb fragment of the rat tryptophan hydroxylase-2 (TPH-2 gene which selectively (97% co-localisation with TPH-2 target raphe serotonergic neurones. In order to enhance the level of expression a two-step transcriptional amplification strategy was employed. This allowed direct visualization of serotonergic neurones by EGFP fluorescence. Using these vectors we have performed initial characterization of EGFP-expressing serotonergic neurones in rat organotypic brain slice cultures. Fluorescent serotonergic neurones were identified and studied using patch clamp and confocal Ca2+ imaging and had features consistent with those previously reported using post-hoc identification approaches. Fine processes of serotonergic neurones could also be visualized in un-fixed tissue and morphometric analysis suggested two putative types of axonal varicosities. We used micro-amperometry to analyse the quantal characteristics of 5 HT release and found that central 5 HT exocytosis occurs predominantly in quanta of ~28000 molecules from varicosities and ~34000 molecules from cell bodies. In addition, in somata, we observed a minority of large release events discharging on average ~800000 molecules. Conclusion For the first time quantal release of 5 HT from somato-dendritic compartments and axonal varicosities in mammalian brain has been demonstrated directly and characterised. Release from somato-dendritic and axonal compartments might have different physiological functions. Novel vectors generated in this

  1. Development of sensitive amperometric hydrogen peroxide sensor using a CuNPs/MB/MWCNT-C{sub 60}-Cs-IL nanocomposite modified glassy carbon electrode

    Energy Technology Data Exchange (ETDEWEB)

    Roushani, Mahmoud, E-mail: mahmoudroushani@yahoo.com; Bakyas, Kobra; Zare Dizajdizi, Behruz

    2016-07-01

    A sensitive hydrogen peroxide (H{sub 2}O{sub 2}) sensor was constructed based on copper nanoparticles/methylene blue/multiwall carbon nanotubes–fullerene–chitosan–ionic liquid (CuNPs/MB/MWCNTs–C{sub 60}–Cs–IL) nanocomposites. The MB/MWCNTs–C{sub 60}–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–C{sub 60}–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 H{sub 2}O{sub 2} in the range of 0.2 μM to 2.0 mM, and the detection limit is 55.0 nM (S/N = 3). In addition, the modified electrode was used to determine H{sub 2}O{sub 2} concentration in human blood serum sample with satisfactory results. - Highlights: • CuNPs/MB/MWCNT-C{sub 60}-Cs-IL/GC electrode was constructed by layer-by-layer method. • The catalytic performance of the sensor was studied with the use of amperometric technique. • The constructed sensor showed enhanced electrocatalytic activity toward the reduction of H{sub 2}O{sub 2}. • The CuNPs/MB/MWCNT-C{sub 60}-Cs-IL/GC electrode demonstrated high stability for the detection of H{sub 2}O{sub 2}.

  2. Signal enhancement in amperometric peroxide detection by using graphene materials with low number of defects

    International Nuclear Information System (INIS)

    Zöpfl, Alexander; Matysik, Frank-Michael; Hirsch, Thomas; Sisakthi, Masoumeh; Eroms, Jonathan; Strunk, Christoph

    2016-01-01

    Two-dimensional carbon nanomaterials ranging from single-layer graphene to defective structures such as chemically reduced graphene oxide were studied with respect to their use in electrodes and sensors. Their electrochemical properties and utility in terms of fabrication of sensing devices are compared. Specifically, the electrodes have been applied to reductive amperometric determination of hydrogen peroxide. Low-defect graphene (SG) was obtained through mechanical exfoliation of natural graphite, while higher-defect graphenes were produced by chemical vapor deposition (CVDG) and by chemical oxidation of graphite and subsequent reduction (rGO). The carbonaceous materials were mainly characterized by Raman microscopy. They were applied as electrode material and the electrochemical behavior was investigated by chronocoulometry, cyclic voltammetry, electrochemical impedance spectroscopy and amperometry and compared to a carbon disc electrode. It is shown that the quality of the graphene has an enormous impact on the amperometric performance. The use of carbon materials with many defects (like rGO) does not result in a significant improvement in signal compared to a plain carbon disc electrode. The sensitivity is 173 mA · M −1  · cm −2 in case of using CVDG which is about 50 times better than that of a plain carbon disc electrode and about 7 times better than that of rGO. The limit of detection for hydrogen peroxide is 15.1 μM (at a working potential of −0.3 V vs SCE) for CVDG. It is concluded that the application of two-dimensional carbon nanomaterials offers large perspectives in amperometric detection systems due to electrocatalytic effects that result in highly sensitive detection. (author)

  3. Characterizing Enzymatic Deposition for Microelectrode Neurotransmitter Detection

    Energy Technology Data Exchange (ETDEWEB)

    Hosein, W. K. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Yorita, A. M. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Tolosa, V. M. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States)

    2016-08-12

    The enzyme immobilization process, one step in creating an enzymatic biosensor, was characterized and analyzed as a function of its physical properties. The neural glutamic biosensor is a flexible device, effectively minimizing trauma to the area of implantation. The Multielectrode Array (MEA) is composed primarily of a proprietary polymer which has been successfully implanted into human subjects in recent years. This polymer allows the device the pliability that other devices normally lack, though this poses some challenges to implantation. The electrodes are made of Platinum (Pt), and can range in number from eight to thirty two electrodes per device. These electrodes are electroplated with a semipermeable polymer layer to improve selectivity of the electrode to the neurotransmitter of interest, in this case glutamate. A signal is created from the interaction of glutamate in the brain with the glutamate oxidase (GluOx) which is immobilized on the surface of the electrode by using crosslinking chemistry in conjunction with glutaraldehyde and Bovine Serum Albumin (BSA). The glutamate is oxidized by glutamate oxidase, producing α-ketoglutarate and hydrogen peroxide (H2O2) as a by-product. The production of H2O2 is crucial for detection of the presence of the glutamate within the enzymatic coating, as it diffuses through the enzyme layer and oxidizes at the surface of the electrode. This oxidation is detectable by measurable change in the current using amperometry. Hence, the MEA allows for in vivo monitoring of neurotransmitter activity in real time. The sensitivity of the sensor to these neurotransmitters is dependent on the thickness of the layer, which is investigated in these experiments in order to optimize the efficacy of the device to detecting the substrate, once implanted.

  4. Synthesis and characterization of cobalt-nichel oxides for the oxygen formation reaction; Sintesis y caracterizacion de oxidos de cobalto-niquel para la reaccion de formacion de oxigeno

    Energy Technology Data Exchange (ETDEWEB)

    Morales G, P

    2001-07-01

    In this work the compounds of cobalt and nickel oxides and the mixtures of cobalt-nickel were prepared which were characterized and evaluated as electrocatalysts in the oxygen release reaction in alkaline media. The compounds were synthesised by the sol-gel method: heated at 400 and 500 Centigrade. The compounds characterization was realized by thermogravimetry, X-ray diffraction and Scanning electron microscopy. As the Co{sub 3}O{sub 4} and the Ni O as the mixtures Ni O/Co{sub 3}O{sub 4} were obtained as a porous material with a small particle size, characteristics which are presented by cause of the low temperature of synthesis. The electrocatalytic evaluation for the synthesised compounds for the oxygen release reaction was realized by cyclic volt amperometry in a 0.5M KOH solution. The oxides mixtures presented a well electrocatalytic activity to be used in the electrochemical release of oxygen. The current density and the electrochemically active area, in all the cases of mixtures is very higher to the Co{sub 3}O{sub 4} and Ni O ones. Observing with greater clearness the synergic effects, in the obtained mixture at 400 C. The oxides mixtures heated at 400 C were stables for the oxygen formation reaction. Therefore it is be able to say that the Ni O/Co{sub 3}O{sub 4} mixture counts on a great reactive area: electrocatalytic characteristic desirable to be a material used as anode in the electrolysis of water, which increases the oxygen release in the anode and so the hydrogen release in the cathode. (Author)

  5. TiO{sub 2} nanoparticle-induced ROS correlates with modulated immune cell function

    Energy Technology Data Exchange (ETDEWEB)

    Maurer-Jones, Melissa A.; Christenson, Jenna R.; Haynes, Christy L., E-mail: chaynes@umn.edu [University of Minnesota, Department of Chemistry (United States)

    2012-12-15

    Design of non-toxic nanoparticles will be greatly facilitated by understanding the nanoparticle-cell interaction mechanism on a cell function level. Mast cells are important cells for the immune system's first line of defense, and we can utilize their exocytotic behavior as a model cellular function as it is a conserved process across cell types and species. Perturbations in exocytosis can also have implications for whole organism health. One proposed mode of toxicity is nanoparticle-induced reactive oxygen species (ROS), particularly for titanium dioxide (TiO{sub 2}) nanoparticles. Herein, we have correlated changes in ROS with the perturbation of the critical cell function of exocytosis, using UV light to induce greater levels of ROS in TiO{sub 2} exposed cells. The primary culture mouse peritoneal mast cells (MPMCs) were exposed to varying concentrations of TiO{sub 2} nanoparticles for 24 h. ROS content was determined using 2,7-dihydrodichlorofluorescein diacetate (DCFDA). Cellular viability was determined with the MTT and Trypan blue assays, and exocytosis was measured by the analytical electrochemistry technique of carbon-fiber microelectrode amperometry. MPMCs exposed to TiO{sub 2} nanoparticles experienced a dose-dependent increase in total ROS content. While there was minimal impact of ROS on cellular viability, there is a correlation between ROS amount and exocytosis perturbation. As nanoparticle-induced ROS increases, there is a significant decrease (45 %) in the number of serotonin molecules being released during exocytosis, increase (26 %) in the amount of time for each exocytotic granule to release, and decrease (28 %) in the efficiency of granule trafficking and docking. This is the first evidence that nanoparticle-induced ROS correlates with chemical messenger molecule secretion, possibly making a critical connection between functional impairment and mechanisms contributing to that impairment.

  6. Alpha-Glucosidase Enzyme Biosensor for the Electrochemical Measurement of Antidiabetic Potential of Medicinal Plants.

    Science.gov (United States)

    Mohiuddin, M; Arbain, D; Islam, A K M Shafiqul; Ahmad, M S; Ahmad, M N

    2016-12-01

    A biosensor for measuring the antidiabetic potential of medicinal plants was developed by covalent immobilization of α-glucosidase (AG) enzyme onto amine-functionalized multi-walled carbon nanotubes (MWCNTs-NH2). The immobilized enzyme was entrapped in freeze-thawed polyvinyl alcohol (PVA) together with p-nitrophenyl-α-D-glucopyranoside (PNPG) on the screen-printed carbon electrode at low pH to prevent the premature reaction between PNPG and AG enzyme. The enzymatic reaction within the biosensor is inhibited by bioactive compounds in the medicinal plant extracts. The capability of medicinal plants to inhibit the AG enzyme on the electrode correlates to the potential of the medicinal plants to inhibit the production of glucose from the carbohydrate in the human body. Thus, the inhibition indicates the antidiabetic potential of the medicinal plants. The performance of the biosensor was evaluated to measure the antidiabetic potential of three medicinal plants such as Tebengau (Ehretis laevis), Cemumar (Micromelum pubescens), and Kedondong (Spondias dulcis) and acarbose (commercial antidiabetic drug) via cyclic voltammetry, amperometry, and spectrophotometry. The cyclic voltammetry (CV) response for the inhibition of the AG enzyme activity by Tebengau plant extracts showed a linear relation in the range from 0.423-8.29 μA, and the inhibition detection limit was 0.253 μA. The biosensor exhibited good sensitivity (0.422 μA/mg Tebengau plant extracts) and rapid response (22 s). The biosensor retains approximately 82.16 % of its initial activity even after 30 days of storage at 4 °C.

  7. Highly sensitive voltammetric sensor based on immobilization of bisphosphoramidate-derivative and quantum dots onto multi-walled carbon nanotubes modified gold electrode for the electrocatalytic determination of olanzapine

    Energy Technology Data Exchange (ETDEWEB)

    Mohammadi-Behzad, Leila [Department of Analytical Chemistry, Faculty of Chemistry, Razi University, Kermanshah (Iran, Islamic Republic of); Gholivand, Mohammad Bagher, E-mail: mbgholivand@yahoo.com [Department of Analytical Chemistry, Faculty of Chemistry, Razi University, Kermanshah (Iran, Islamic Republic of); Shamsipur, Mojtaba [Department of Analytical Chemistry, Faculty of Chemistry, Razi University, Kermanshah (Iran, Islamic Republic of); Gholivand, Khodayar [Department of Chemistry, Tarbiat Modares University, Tehran (Iran, Islamic Republic of); Barati, Ali [Department of Analytical Chemistry, Faculty of Chemistry, Razi University, Kermanshah (Iran, Islamic Republic of); Gholami, Akram [Department of Chemistry, Tarbiat Modares University, Tehran (Iran, Islamic Republic of)

    2016-03-01

    In the present paper, a new bisphosphoramidate derivative compound, 1, 4-bis(N-methyl)-benzene-bis(N-phenyl, N-benzoylphosphoramidate) (BMBPBP), was synthesized and used as a mediator for the electrocatalytic oxidation of olanzapine. The electro-oxidation of olanzapine at the surface of the BMBPBP/CdS-quantum dots/multi-walled carbon nanotubes (BMBPBP/CdS-QDs/MWCNTs) modified gold electrode was studied using cyclic voltammetry, chronoamperometry and electrochemical impedance spectroscopy. This sensor showed an excellent electrocatalytic oxidation activity toward olanzapine at less positive potential, pronounced current response, and good sensitivity. The diffusion coefficient and kinetic parameters (such as electron transfer coefficient and the heterogeneous rate constant) were determined for olanzapine oxidation, using the electrochemical approaches. Surface morphology and electrochemical properties of the prepared modified electrode were investigated by scanning electron microscopy (SEM), cyclic voltammetry and electrochemical impedance spectroscopy techniques. The hydrodynamic amperometry at rotating modified electrode at constant potential versus reference electrode was used for detection of olanzapine. Under optimized conditions, the calibration plot was linear in the concentration range of 20 nM to 100 μM and detection limit was found to be 6 nM. The proposed method was successfully applied to the determination of olanzapine in pharmaceuticals and human serum samples. - Highlights: • A highly sensitive sensor for OLZ determination was developed. • The sensor constructed based on immobilization of BMBPBP on CdS-QDs/MWCNTs Au electrode • The morphology of the modified electrode was examined by SEM. • The prepared sensor shows stable electrochemical behavior at a wide pH range. • The proposed sensor is used for trace determination of OLZ in real samples.

  8. Electrochemical study of bio-corrosion mechanisms at the carbon steel interface in presence of iron-reducing and hydrogenotrophic bacteria in the nuclear waste disposal context

    International Nuclear Information System (INIS)

    Leite-de-Souza-Moreira, Rebeca

    2013-01-01

    The safety of deep geological repository for nuclear waste is a very important and topical matter especially for the nuclear industry. Such as nuclear fuel the high level waste have to be stored for time frames of millions of years in metallic containers. Typically these containers should be placed in deep geological clay formations 500 metres underground. Corrosion processes, will take place after the re-saturation of the geological medium and under the prevalent anoxic conditions may lead to the generation of hydrogen. This gas accumulates in clay environment through the years and eventually becomes hazardous for steel containers. In the particular environment of geological repositories does not provide much biodegradable substances. This is the reason that hydrogen represents a new suitable energy source for hydrogenotrophic bacteria. Thereby formed bacterial bio-films on the containers may contribute to a process of fast decay of the steel, the so called bio-corrosion. The aim of this study is to characterize the electrochemical interfaces in order to obtain the mechanisms of bio-corrosion of carbon steels in presence of iron reducing and hydrogenotrophic bacterium Shewanella oneideinsis. The products of corrosion processes, namely hydrogen and iron (III) oxides are used as electron donor and acceptor, respectively. The amount of hydrogen consumed by Shewanella could be estimated with 10"-"4 mol s"-"1 using Scanning Electrochemical Microscopy (SECM) techniques. The influence of the local hydrogen generation was evaluated via chrono-amperometry. When hydrogen was locally generated above a carbon steel substrate an accelerated corrosion process can be observed. Eventually, using Local Electrochemical Impedance Spectroscopy (LEIS) techniques, the mechanism of the generalised corrosion process was demonstrated. (author)

  9. Electrochemical fabrication of a cauliflower-like nanostructured Pd film from pure Pd and its applications in electrocatalysis and electroanalysis

    International Nuclear Information System (INIS)

    Xu, Shili; Zhang, Hefang; Huang, Fuli; Wang, Pengshu; Xia, Yue; Li, Zelin; Huang, Wei

    2013-01-01

    Highlights: • A cauliflower-like nanostructured Pd film was fabricated by just applying one double-potential step method. • The film fabrication involves the formation of K 2 PdCl 4 salt from pure Pd and its electroreduction to Pd atoms. • The film electrode exhibits high electrocatalytic activities toward the oxidation of ethanol and ascorbic acid. • Good analytical performances in the higher-concentration regions are obtained on the film electrode. -- Abstract: A cauliflower-like nanostructured Pd film (CNPF) has been fabricated by just applying one double-potential step on a pure Pd substrate in a KCl solution. The CNPF formation mainly involves the formation of K 2 PdCl 4 salt from pure Pd and its electroreduction to Pd atoms. The as-prepared CNPF electrode exhibits high electrocatalytic activities toward the oxidation of ethanol and ascorbic acid (AA). The CNPF electrode is also employed to detect AA by means of constant potential amperometry (CPA) and cyclic voltammetry (CV), and good analytical performances in the higher-concentration regions are obtained. In CPA studies performed at −0.4 V, the oxidation current is linearly dependent on AA concentration in the range of 0.1–7.5 mM with a detection limit of 80 μM (based on S/N = 3), a short response time of about 3 s and a high sensitivity of 589.80 μA mM −1 cm −2 . Meanwhile, the peak current responses in CVs are linear over the broad range of 0.1–35 mM with a sensitivity of 178.56 μA mM −1 cm −2 . Besides, the CNPF electrode can also be used to detect AA in medicine vitamin C tablet with satisfactory results

  10. MISENS DEVICE AS A NEW AUTOMATED BIOSENSING PLATFORM BASED ON REAL-TIME ELECTROCHEMICAL PROFILING (REP

    Directory of Open Access Journals (Sweden)

    yıldız uludağ

    2016-09-01

    Full Text Available In various fields like health, environmental control, food security and military defense; there is an increasing demand for on-site detection, fast identification and urgent response which brings the necessity to employ laboratory detection procedures on standalone automatic devices. In response to that TUBITAK BILGEM’s Bioelectronic Devices and Systems Group has been developing portable and fully automated biosensor devices using optical and electrochemical biosensor detection techniques. Here we describe a new integrated and fully automated lab-on-a-chip based biosensor device ‘MiSens’. The key features of the MiSens include a new electrode array, an integrated microfluidic system and real-time amperometric measurements during the flow of enzyme substrate. While simple protocols can be controlled from the LCD display on the device, other main device control procedures can be run wireless by a tablet/PC using the MiCont™ software developed by the team. For the device, a new plug and play type sensor chip docking station has been designed that with one move it enables the formation of a ~ 7-10 µl capacity flow cell on the electrode array with the necessary microfluidic and electronic connections. The MiSens device has been developed by our multi-disciplinary team by integrating and automatising the earlier developed sensing platform REP™ (Real-time Electrochemical Profiling. The performance of the MiSens device has been tested using cyclic voltammetry and amperometry tests and the results were compared with an of the shelf potantiostat.

  11. Electrochemical behaviour of platinum in hydrogen peroxide solution (1963); Comportement electrochimique du platine en solution d'eau oxygene (1963)

    Energy Technology Data Exchange (ETDEWEB)

    Prost, G H [Commisariat a l' Energie Atomique, Grenoble (France). Centre d' Etudes Nucleaires

    1963-06-15

    The relative stability of hydrogen peroxide in aqueous solution at 25 deg. C, allows its amperometric determination from the theory, using either its cathodic reduction or its anodic oxidation. The cathodic reduction yields a wave on a platinum electrode only when some oxygen is present in the solution. It cannot, therefore, be used for electrochemical determination. On the other hand, the anodic oxidation on platinum produces a wave which might be used. However, a passivation of platinum occurs at the same time. This passivation process is studied by means of potentio-kinetic, potentio-static, intensio-static curves and of pH measurements in the vicinity of the anode. A mechanism for passivation is presented, which takes into account the role of hydrogen peroxide as a reducing agent. This passivation rules out any analytical application of the oxidation reaction of hydrogen peroxide. (author) [French] La stabilite relative de l'eau oxygenee en solution aqueuse a 25 deg. C permet d'envisager theoriquement son dosage par amperometrie, en utilisant soit sa reduction cathodique, soit son oxydation anodique. La reduction cathodique ne donne lieu a une vague sur electrode de platine qu'en presence d'oxygene dissous. Il n'est donc pas utilisable pour un dosage. L'oxydation anodique sur platine donne une vague theoriquement utilisable mais s'accompagne d'une passivation du platine. Le processus de la passivation est etudie au moyen des courbes potentiocinetiques, potentiostatiques, intensiostatiques et par une mesure des variations de pH au voisinage de l'anode. On propose un mecanisme de passivation en tenant compte du role activant de l'eau oxygenee. Cette passivation interdit toute application analytique de la reaction d'oxydation de l'eau oxygenee. (auteur)

  12. Flow-based method for epinephrine determination using a solid reactor based on molecularly imprinted poly(FePP-MAA-EGDMA)

    Energy Technology Data Exchange (ETDEWEB)

    Sartori, Lucas Rossi [Programa de Pos-Graduacao em Ciencias Farmaceuticas, Universidade Federal de Alfenas (Unifal-MG), Rua Gabriel Monteiro da Silva, 714, 37130-000, Alfenas/MG (Brazil); Santos, Wilney de Jesus Rodrigues [Departamento de Quimica Analitica, Instituto de Quimica, Universidade Estadual de Campinas (Unicamp), Cidade Universitaria Zeferino Vaz s/n,13083-970, Campinas/SP (Brazil); Kubota, Lauro Tatsuo [Departamento de Quimica Analitica, Instituto de Quimica, Universidade Estadual de Campinas (Unicamp), Cidade Universitaria Zeferino Vaz s/n,13083-970, Campinas/SP (Brazil); Instituto Nacional de Ciencia e Tecnologia (INCT) de Bioanalitica, Universidade Estadual de Campinas (Unicamp), Instituto de Quimica, Departamento de Quimica Analitica, Cidade Universitaria Zeferino Vaz s/n, 13083-970, Campinas/SP (Brazil); Segatelli, Mariana Gava [Departamento de Quimica, Universidade Estadual de Londrina (UEL), Rod. Celso Garcia PR 445 Km 380, 86051-990, Londrina/PR (Brazil); Tarley, Cesar Ricardo Teixeira, E-mail: tarley@uel.br [Programa de Pos-Graduacao em Ciencias Farmaceuticas, Universidade Federal de Alfenas (Unifal-MG), Rua Gabriel Monteiro da Silva, 714, 37130-000, Alfenas/MG (Brazil); Instituto Nacional de Ciencia e Tecnologia (INCT) de Bioanalitica, Universidade Estadual de Campinas (Unicamp), Instituto de Quimica, Departamento de Quimica Analitica, Cidade Universitaria Zeferino Vaz s/n, 13083-970, Campinas/SP (Brazil)

    2011-03-12

    A solid phase reactor based on molecularly imprinted poly(iron (III) protoporphyrin-methacrylic acid-ethylene glycol dimethacrylate) (MIP-MAA) has been synthesized by bulk method and applied as an selective material for the epinephrine determination in the presence of hydrogen peroxide. In order to prove the selective behaviour of MIP, two blank polymers named non-imprinted polymer (NIP1), non-imprinted polymer in the absence of hemin (NIP2) as well as a poly(iron (III) protoporphyrin-4-vynilpyridine-ethylene glycol dimethacrylate) (MIP-4VPy) were synthesized. The epinephrine-selective MIP-MAA reactor was used in a flow injection system, in which an epinephrine solution (120 {mu}L) at pH 8.0 percolates in the presence of hydrogen peroxide (300 {mu}mol L{sup -1}) through MIP-MAA. The oxidation of epinephrine by hydrogen peroxide is increased by using MIP-MAA, being the product formed monitored by amperometry at 0.0 V vs. Ag/AgCl. The MIP-MAA showed better selective behaviour than NIP1, NIP2 and MIP-4VPy, demonstrating the effectiveness of molecular imprinting effect. Highly improved response was observed for epinephrine in detriment of similar substances (phenol, ascorbic acid, methyl-L-DOPA, p-aminophenol, catechol, L-DOPA and guaiacol). The method provided a calibration curve ranging from 10 to 500 {mu}mol L{sup -1} and a limit of detection of 5.2 {mu}mol L{sup -1}. Kinetic data indicated a value of maximum rate V{sub max} (0.993 {mu}A) and apparent Michaelis-Menten constant of K{sub m}{sup app}(725.6 {mu}mol L{sup -1}). The feasibility of biomimetic solid reactor was attested by its successful application for epinephrine determination in pharmaceutical formulation.

  13. Imidazoline derivative templated synthesis of broccoli-like Bi2S3 and its electrocatalysis towards the direct electrochemistry of hemoglobin.

    Science.gov (United States)

    Chen, Xiaoqian; Wang, Qingxiang; Wang, Liheng; Gao, Feng; Wang, Wei; Hu, Zhengshui

    2015-04-15

    A broccoli-like bismuth sulfide (bBi2S3) was synthesized via a solvothermal method using a self-made imidazoline derivative of 2-undecyl-1-dithioureido-ethyl-imidazoline as the soft template. The morphology and chemical constitution of the product were characterized by scanning electron microscope (SEM), transmission electron microscope (TEM) and X-ray diffraction (XRD). Electrochemical characterization experiments show that the bBi2S3 has the higher specific surface area and standard heterogeneous electron transfer rate constant than the rod-like Bi2S3 (rBi2S3). Hemoglobin (Hb) was then chosen as a protein model to investigate the electrocatalytic property of the synthesized bBi2S3. The results show that Hb entrapped in the composite film of chitosan and bBi2S3 displays an excellent direct electrochemistry, and retains its biocatalytic activity toward the electro-reduction of hydrogen peroxide. The current response in the amperometry shows a linear response to H2O2 concentrations in the range from 0.4 to 4.8µM with high sensitivity (444µAmM(-1)) and low detection limit (0.096µM). The Michaelis-Menten constant (KM(app)) of the fabricated bioelectrode for H2O2 was determined as low as 1µM. These results demonstrate that the synthesized bBi2S3 offers a new path for the immobilization of redox-active protein and the construction of the third-generation biosensors. Copyright © 2014 Elsevier B.V. All rights reserved.

  14. Direct growth of metal-organic frameworks thin film arrays on glassy carbon electrode based on rapid conversion step mediated by copper clusters and hydroxide nanotubes for fabrication of a high performance non-enzymatic glucose sensing platform.

    Science.gov (United States)

    Shahrokhian, Saeed; Khaki Sanati, Elnaz; Hosseini, Hadi

    2018-07-30

    The direct growth of self-supported metal-organic frameworks (MOFs) thin film can be considered as an effective strategy for fabrication of the advanced modified electrodes in sensors and biosensor applications. However, most of the fabricated MOFs-based sensors suffer from some drawbacks such as time consuming for synthesis of MOF and electrode making, need of a binder or an additive layer, need of expensive equipment and use of hazardous solvents. Here, a novel free-standing MOFs-based modified electrode was fabricated by the rapid direct growth of MOFs on the surface of the glassy carbon electrode (GCE). In this method, direct growth of MOFs was occurred by the formation of vertically aligned arrays of Cu clusters and Cu(OH) 2 nanotubes, which can act as both mediator and positioning fixing factor for the rapid formation of self-supported MOFs on GCE surface. The effect of both chemically and electrochemically formed Cu(OH) 2 nanotubes on the morphological and electrochemical performance of the prepared MOFs were investigated. Due to the unique properties of the prepared MOFs thin film electrode such as uniform and vertically aligned structure, excellent stability, high electroactive surface area, and good availability to analyte and electrolyte diffusion, it was directly used as the electrode material for non-enzymatic electrocatalytic oxidation of glucose. Moreover, the potential utility of this sensing platform for the analytical determination of glucose concentration was evaluated by the amperometry technique. The results proved that the self-supported MOFs thin film on GCE is a promising electrode material for fabricating and designing non-enzymatic glucose sensors. Copyright © 2018 Elsevier B.V. All rights reserved.

  15. Utilization of highly purified single wall carbon nanotubes dispersed in polymer thin films for an improved performance of an electrochemical glucose sensor

    Energy Technology Data Exchange (ETDEWEB)

    Goornavar, Virupaxi [Molecular Toxicology Laboratory, Center for Biotechnology and Biomedical Sciences, Norfolk State University, 700 Park Avenue, Norfolk, VA 23504 (United States); Center for Materials Research, Norfolk State University, 555 Park Avenue, Norfolk, VA 23504 (United States); Jeffers, Robert [Molecular Toxicology Laboratory, Center for Biotechnology and Biomedical Sciences, Norfolk State University, 700 Park Avenue, Norfolk, VA 23504 (United States); Luna Innovations, Inc., 706 Forest St., Suite A, Charlottesville, VA 22902 (United States); Biradar, Santoshkumar [RICE University, 6100 Main St, Houston, TX 77251 (United States); Ramesh, Govindarajan T., E-mail: gtramesh@nsu.edu [Molecular Toxicology Laboratory, Center for Biotechnology and Biomedical Sciences, Norfolk State University, 700 Park Avenue, Norfolk, VA 23504 (United States); Center for Materials Research, Norfolk State University, 555 Park Avenue, Norfolk, VA 23504 (United States)

    2014-07-01

    In this work we report the improved performance an electrochemical glucose sensor based on a glassy carbon electrode (GCE) that has been modified with highly purified single wall carbon nanotubes (SWCNTs) dispersed in polyethyleneimine (PEI), polyethylene glycol (PEG) and polypyrrole (PPy). The single wall carbon nanotubes were purified by both thermal and chemical oxidation to achieve maximum purity of ∼ 98% with no damage to the tubes. The SWCNTs were then dispersed by sonication in three different organic polymers (1.0 mg/ml SWCNT in 1.0 mg/ml of organic polymer). The stable suspension was coated onto the GCE and electrochemical characterization was performed by Cyclic Voltammetry (CV) and Amperometry. The electroactive enzyme glucose oxidase (GOx) was immobilized on the surface of the GCE/(organic polymer–SWCNT) electrode. The amperometric detection of glucose was carried out at 0.7 V versus Ag/AgCl. The GCE/(SWCNT–PEI, PEG, PPY) gave a detection limit of 0.2633 μM, 0.434 μM, and 0.9617 μM, and sensitivities of 0.2411 ± 0.0033 μA mM{sup −1}, r{sup 2} = 0.9984, 0.08164 ± 0.001129 μA mM{sup −1}, r{sup 2} = 0.9975, 0.04189 ± 0.00087 μA mM{sup −1}, and r{sup 2} = 0.9944 respectively and a response time of less than 5 s. The use of purified SWCNTs has several advantages, including fast electron transfer rate and stability in the immobilized enzyme. The significant enhancement of the SWCNT modified electrode as a glucose sensor can be attributed to the superior conductivity and large surface area of the well dispersed purified SWCNTs. - Highlights: • Purification method employed here use cheap and green oxidants. • The method does not disrupt the electronic structure of nanotubes. • This method removes nearly < 2% metallic impurities. • Increases the sensitivity and performance of glassy carbon electrode • This system can detect as low as 0.066 μM of H{sub 2}O{sub 2} and 0.2633 μM of glucose.

  16. Self-assembly of glucose oxidase on reduced graphene oxide-magnetic nanoparticles nanocomposite-based direct electrochemistry for reagentless glucose biosensor.

    Science.gov (United States)

    Pakapongpan, Saithip; Poo-Arporn, Rungtiva P

    2017-07-01

    A novel approach of the immobilization of a highly selective and stable glucose biosensor based on direct electrochemistry was fabricated by a self-assembly of glucose oxidase (GOD) on reduced graphene oxide (RGO) covalently conjugated to magnetic nanoparticles (Fe 3 O 4 NPs) modified on a magnetic screen-printed electrode (MSPE). The RGO-Fe 3 O 4 nanocomposite has remarkable enhancement in large surface areas, is favorable environment for enzyme immobilization, facilitates electron transfer between enzymes and electrode surfaces and possesses superparamagnetism property. The morphology and electrochemical properties of RGO-Fe 3 O 4 /GOD were characterized by scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, cyclic voltammetry (CV) and amperometry. The modified electrode was a fast, direct electron transfer with an apparent electron transfer rate constant (k s ) of 13.78s -1 . The proposed biosensor showed fast amperometric response (3s) to glucose with a wide linear range from 0.05 to 1mM, a low detection limit of 0.1μM at a signal to noise ratio of 3 (S/N=3) and good sensitivity (5.9μA/mM). The resulting biosensor has high stability, good reproducibility, excellent selectivity and successfully applied detection potential at -0.45V. This mediatorless glucose sensing used the advantages of covalent bonding and self-assembly as a new approach for immobilizing enzymes without any binder. It would be worth noting that it opens a new avenue for fabricating excellent electrochemical biosensors. This is a new approach that reporting the immobilization of glucose oxidase on reduced graphene oxide (RGO) covalently conjugated to magnetic nanoparticles (Fe 3 O 4 NPs) by electrostatic interaction and modified screen printed electrode. We propose the reagentless with fabrication method without binder and adhesive agents for immobilized enzyme. Fe 3 O 4 NPs increasing surface area to enhance the immobilization and prevent

  17. Electrosorption of Os(III)-complex at single-wall carbon nanotubes immobilized on a glassy carbon electrode: Application to nanomolar detection of bromate, periodate and iodate

    International Nuclear Information System (INIS)

    Salimi, Abdollah; Kavosi, Begard; Babaei, Ali; Hallaj, Rahman

    2008-01-01

    A simple procedure was developed to prepare a glassy carbon electrode modified with single-wall carbon nanotubes (SWCNTs) and Os(III)-complex. The glassy carbon (GC) electrode modified with CNTs was immersed into Os(III)-complex solution (direct deposition) for a short period of time (60 s). 1,4,8,12-Tetraazacyclotetradecane osmium(III) chloride, (Os(III)LCl 2 ).ClO 4 , irreversibly and strongly adsorbed on SWCNTs immobilized on the surface of GC electrode. Cyclic voltammograms of the Os(III)-complex-incorporated-SWCNTs indicate a pair of well defined and nearly reversible redox couple with surface confined characteristic at wide pH range (1-8). The surface coverage (Γ) and charge transfer rate constant (k s ) of the immobilized Os-complex on SWCNTs were 3.07 x 10 -9 mol cm -2 , 5.5 (±0.2) s -1 , 2.94 x 10 -9 mol cm -2 , 7.3 (±0.3) s -1 at buffer solution with pH 2 and 7, respectively, indicate high loading ability of SWCNTs for Os(III) complex and great facilitation of the electron transfer between electroactive redox center and carbon nanotubes immobilized on the electrode surface. Modified electrodes showed higher electrocatalytic activity toward reduction of BrO 3 - , IO 3 - and IO 4 - in acidic solutions. The catalytic rate constants for catalytic reduction bromate, periodate and iodate were 3.79 (±0.2) x 10 3 , 7.32 (±0.2) x 10 3 and 1.75 (±0.2) x 10 3 M -1 s -1 , respectively. The hydrodynamic amperometry of rotating modified electrode at constant potential (0.3 V) was used for nanomolar detection of selected analytes. Excellent electrochemical reversibility of the redox couple, good reproducibility, high stability, low detection limit, long life time, fast amperometric response time, wide linear concentration range, technical simplicity and possibility of rapid preparation are great advantage of this sensor

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

    Energy Technology Data Exchange (ETDEWEB)

    Kurd, Masoumeh [Department of Chemistry, University of Kurdistan, P. O. Box 416, Sanandaj (Iran, Islamic Republic of); Salimi, Abdollah, E-mail: absalimi@uok.ac.ir [Department of Chemistry, University of Kurdistan, P. O. Box 416, Sanandaj (Iran, Islamic Republic of); Research Center for Nanotechnology, University of Kurdistan, P. O. Box 416, Sanandaj (Iran, Islamic Republic of); Hallaj, Rahman [Department of Chemistry, University of Kurdistan, P. O. Box 416, Sanandaj (Iran, Islamic Republic of)

    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 (k{sub s}) of immobilized Fe(II)–Pc were calculated as 1.26 × 10{sup −10} mol cm{sup −2} and 28.13 s{sup −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 CCl{sub 3}COOH to CH{sub 3}COOH have been clearly seen. The observed chronoamperometric currents are linearly increased with the concentration of TCA at concentration range up to 20 mM. Detection limit and sensitivity of the modified electrode were 2.0 μM and 0.10 μA μM{sup −1} cm{sup −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. Highlights: ► Phthalocyanine (PC) and Fe(II) immobilized onto MWCNTs modified GC electrode. ► A pair of well-defined redox couple correspondent to (Fe(III)Pc/Fe(II)Pc) observed. ► Modified electrode shows excellent catalytic activity to electroreduction of CCl{sub 3}COOH. ► Amperometry and cyclic voltammetry techniques were used for detection of CCl{sub 3}COOH. ► Detection limit and sensitivity were 2.0 μM and 0.10 μA μM{sup −1} cm{sup −2}, respectively.

  19. Modification of glassy carbon electrode with multi-walled carbon nanotubes and iron(III)-porphyrin film: Application to chlorate, bromate and iodate detection

    International Nuclear Information System (INIS)

    Salimi, Abdollah; MamKhezri, Hussein; Hallaj, Rahman; Zandi, Shiva

    2007-01-01

    In this study, multi-wall carbon nanotubes (MWCTs) is evaluated as a transducer, stabilizer and immobilization matrix for the construction of amperometric sensor based on iron-porphyrin. 5,10,15,20-Tetraphenyl-21H,23H-porphine iron(III) chloride (Fe(III)P) adsorbed on MWCNTs immobilized on the surface of glassy carbon electrode. Cyclic voltammograms of the Fe(III)P-incorporated-MWCNTs indicate a pair of well-defined and nearly reversible redox couple with surface confined characteristics at wide pH range (2-12). The surface coverage (Γ) and charge transfer rate constant (k s ) of Fe(III)P immobilized on MWCNTs were 7.68 x 10 -9 mol cm -2 and 1.8 s -1 , respectively, indicating high loading ability of MWCNTs for Fe(III)P and great facilitation of the electron transfer between Fe(III)P and carbon nanotubes immobilized on the electrode surface. Modified electrodes exhibit excellent electrocatalytic activity toward reduction of ClO 3 - , IO 3 - and BrO 3 - in acidic solutions. The catalytic rate constants for catalytic reduction of bromate, chlorate and iodate were 6.8 x 10 3 , 7.4 x 10 3 and 4.8 x 10 2 M -1 s -1 , respectively. The hydrodynamic amperometry of rotating-modified electrode at constant potential versus reference electrode was used for detection of bromate, chlorate and iodate. The detection limit, linear calibration range and sensitivity for chlorate, bromate and iodate detections were 0.5 μM, 2 μM to 1 mM, 8.4 nA/μM, 0.6 μM, 2 μM to 0.15 mM, 11 nA/μM, and 2.5 μM, 10 μM to 4 mM and 1.5 nA/μM, respectively. Excellent electrochemical reversibility of the redox couple, good reproducibility, high stability, low detection limit, long life time, fast amperometric response time, wide linear concentration range, technical simplicity and possibility of rapid preparation are great advantages of this sensor. The obtained results show promising practical application of the Fe(III)P-MWCNTs-modified electrode as an amperometric sensor for chlorate, iodate and

  20. Characterization of binding and mobility of metals and xenobiotics in continuous flow and soil biosystems

    International Nuclear Information System (INIS)

    Sunovska, A.

    2016-01-01

    The main aim of the dissertation thesis was to contribute to development of analytical tools and approaches application in characterization of binding and mobility of heavy metals and organic compounds (xenobiotics) in continuous flow and soil biosystems. Within the solution of this aim, a wide range of analytical methods (gamma-spectrometry, UV-VIS spectrophotometry, AAS, X-ray fluorescence spectrometry, ion chromatography, and stripping volt-amperometry) and approaches (mathematical modelling - methods of nonlinear regression and in silico prediction modelling; chemometrics and statistical analysis of the data; single-step extraction methods, and lysimetry) were applied. In the first step of thesis solution, alternative sorbents of biological origin (biomass of microalgae, freshwater mosses, and waste biomass of hop) were obtained and physico-chemically characterized mainly in order to prediction of sorption capacities of Cd and synthetic dyes thioflavine T (TT), malachite green (MG) or methylene blue (MB) removal from single component or binary aqueous solutions and under conditions of batch or continuous flow systems. For these purposes, mathematical models of adsorption isotherms and models originated from chromatographic separation methods by application of methods of nonlinear regression analysis were used. In the second part of the work, methods of multivariate analysis in the evaluation of processes of synthetic dyes TT and MB binding in terms of the finding of relationships between sorption-desorption variables describing the stability of the bond and parameters defining the physic-chemical properties of river sediments and the environment of real or model waters were applied. In the last part of the work, a special laboratory lysimeter system was designed and applied within the soil biosystem defined by: soil additive (SA) derived from sewage sludge representing the source of microelements Zn and Cu <-> agriculturally used soil <-> soil solution <-> root

  1. Fisiologi dan Gangguan Keseimbangan Natrium, Kalium dan Klorida serta Pemeriksaan Laboratorium

    Directory of Open Access Journals (Sweden)

    Rismawati Yaswir

    2012-09-01

    +, potassium (K+, chloride(Cl-, and bicarbonate (HCO3-. Fourth Inspection of the major electrolyte in clinic known as "electrolyteprofile”.Sodium is cation many in extracell fluid, potassium is cation many in intrasel fluid, and chloride is anionmany in extracell fluid. Amount of natrium, chloride and potassium in body are balance which enter especially fromdigest and excretion especially through kidney.Balance disorders of natrium, chloride and potassium in the form ofhipo- and hyper-. Hipo- happened when the electrolyte concentration in body go down more than somemiliekuivalen under normal values and hyper- when the concentration of mounting above normal.Laboratoryfindings to determine concentration of natrium, chloride and potassium are with ion selective electrode (ISEmethod, flame emission spectrophotometry (FES, atomic absorption spectrophotometry, spektrofotometrypursuant to enzyme activation, determine concentration of chloride with titration method of merkurimeter, and withtitration method of colorimetry-amperometry.Keywords: Electrolyte, balance, balance disorders

  2. Gold-copper bimetallic nanoparticles supported on nano P zeolite modified carbon paste electrode as an efficient electrocatalyst and sensitive sensor for determination of hydrazine.

    Science.gov (United States)

    Amiripour, Fatemeh; Azizi, Seyed Naser; Ghasemi, Shahram

    2018-06-01

    In this report, a facile, efficient and low cost electrochemical sensor based on bimetallic Au-Cu nanoparticles supported on P nanozeolite modified carbon paste electrode (Au-Cu/NPZ/CPE) was constructed and its efficiency for determination of hydrazine in trace level was studied. For this purpose, agro waste material, stem sweep ash (SSA) was employed as the starting material (silica source) for the synthesis of nano P zeolite (NPZ). After characterization of the synthesized NPZ by analytical instruments (scanning electronic microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and Fourier transform infrared (FT-IR) spectroscopy), construction of Au-Cu/NPZ/CPE was performed by three steps procedure involving preparation of nano P zeolite modified carbon paste electrode (NPZ/CPE), introducing Cu +2 ions into nano zeolite structure by ion exchange and electrochemical reduction of Cu +2 ions upon applying constant potential. This procedure is followed by partial replacement of Cu by Au due to galvanic replacement reaction (GRR). The electrochemical properties of hydrazine at the surface of Au-Cu/NPZ/CPE was evaluated using cyclic voltammetry (CV), amperometry, and chronoamperometry methods in 0.1 M phosphate buffer solution (PBS). It was found that the prepared sensor has higher electrocatalytic activity at a relatively lower potential compared to other modified electrodes including Au/NPZ/CPE, Cu/NPZ/CPE, Au-Cu/CPE and etc. Moreover, the proposed electrochemical sensor presented the favorable analytical properties for determination of hydrazine such as low detection limit (0.04 µM), rapid response time (3 s), wide linear range (0.01-150 mM), and high sensitivity (99.53 µA mM -1 ) that are related to the synergic effect of bimetallic of Au-Cu, porous structure and enough surface area of NPZ. In addition, capability of Au-Cu/NPZ/CPE sensor was successfully tested in real samples with good accuracy and precision. Copyright

  3. Characterization of binding and mobility of metals and xenobiotics in continuous flow and soil biosystems

    International Nuclear Information System (INIS)

    Sunovska, A.

    2016-01-01

    The main aim of the dissertation thesis was to contribute to development of analytical tools and approaches application in characterization of binding and mobility of heavy metals and organic compounds (xenobiotics) in continuous flow and soil biosystems. Within the solution of this aim, a wide range of analytical methods (gamma-spectrometry, UV-VIS spectrophotometry, AAS, X-ray fluorescence spectrometry, ion chromatography, and stripping volt-amperometry) and approaches (mathematical modelling - methods of nonlinear regression and in silico prediction modelling; chemometrics and statistical analysis of the data; single-step extraction methods, and lysimetry) were applied. In the first step of thesis solution, alternative sorbents of biological origin (biomass of microalgae, freshwater mosses, and waste biomass of hop) were obtained and physico-chemically characterized mainly in order to prediction of sorption capacities of Cd and synthetic dyes thioflavine T (TT), malachite green (MG) or methylene blue (MB) removal from single component or binary aqueous solutions and under conditions of batch or continuous flow systems. For these purposes, mathematical models of adsorption isotherms and models originated from chromatographic separation methods by application of methods of nonlinear regression analysis were used. In the second part of the work, methods of multivariate analysis in the evaluation of processes of synthetic dyes TT and MB binding in terms of the finding of relationships between sorption-desorption variables describing the stability of the bond and parameters defining the physic-chemical properties of river sediments and the environment of real or model waters were applied. In the last part of the work, a special laboratory lysimeter system was designed and applied within the soil biosystem defined by: soil additive (SA) derived from sewage sludge representing the source of microelements Zn and Cu agriculturally used soil soil solution root system of

  4. Electrocatalytic oxidation of ascorbic acid by [Fe(CN){sub 6}]{sup 3-/4-} redox couple electrostatically trapped in cationic N,N-dimethylaniline polymer film electropolymerized on diamond electrode

    Energy Technology Data Exchange (ETDEWEB)

    Roy, Protiva Rani [Department of Electronic Chemistry, Interdisciplinary Graduate School of Science and Engineering, Tokyo Institute of Technology, Mail Box G1-5, 4259 Nagatsuta, Midori-ku, Yokohama 226-8502 (Japan); Saha, Madhu Sudan [Department of Electronic Chemistry, Interdisciplinary Graduate School of Science and Engineering, Tokyo Institute of Technology, Mail Box G1-5, 4259 Nagatsuta, Midori-ku, Yokohama 226-8502 (Japan); Okajima, Takeyoshi [Department of Electronic Chemistry, Interdisciplinary Graduate School of Science and Engineering, Tokyo Institute of Technology, Mail Box G1-5, 4259 Nagatsuta, Midori-ku, Yokohama 226-8502 (Japan); Ohsaka, Takeo [Department of Electronic Chemistry, Interdisciplinary Graduate School of Science and Engineering, Tokyo Institute of Technology, Mail Box G1-5, 4259 Nagatsuta, Midori-ku, Yokohama 226-8502 (Japan)]. E-mail: ohsaka@echem.titech.ac.jp

    2006-06-01

    Multinegatively charged metal complex, hexacyanoferrate ([Fe(CN){sub 6}]{sup 4-}), was electrostatically trapped in the cationic polymer film of N,N-dimethylaniline (PDMA) which was electrochemically deposited on the boron-doped diamond (BDD) electrode by controlled-potential electro-oxidation of the monomer. This ferrocyanide-trapped PDMA film was used to catalyze the oxidation of ascorbic acid (AA). Increase in the oxidation current response with a negative shift of the anodic peak potential was observed at the cationic PDMA film-coated BDD (PDMA|BDD) electrode, compared with that at the bare BDD electrode. A more drastic enhancement in the oxidation peak current as well as more negative shift of oxidation potential was found at the ferrocyanide-trapped PDMA film-coated BDD ([Fe(CN){sub 6}]{sup 3-/4-}|PDMA|BDD) electrode. This [Fe(CN){sub 6}]{sup 3-/4-}|PDMA|BDD electrode can be used as an amperometric sensor of AA. Ferrocyanide, electrostatically trapped in the polymer film shows more electrocatalytic activity than that coordinatively attached to the polymer film or dissolved in the solution phase. The electrocatalytic current depends on the surface coverage of ferricyanide, {gamma} {sub Fe}, within the polymer film. Diffusion coefficient (D) of AA in the solution was estimated by rotating disk electrode voltammetry: D = (5.8 {+-} 0.3) x 10{sup -6} cm{sup 2} s{sup -1}. The second-order rate constant for the catalytic oxidation of AA by ferricyanide was also estimated to be 9.0 x 10{sup 4} M{sup -1} s{sup -1}. In the hydrodynamic amperometry using the [Fe(CN){sub 6}]{sup 3-/4-}|PDMA|BDD electrode, a successive addition of 1 {mu}M AA caused the successive increase in current response with equal amplitude and the sensitivity was calculated as 0.233 {mu}A cm{sup -2} {mu}M{sup -1}.

  5. Chemical attachment of functionalized multiwalled carbon nanotubes on glassy carbon electrode for electrocatalytic application

    International Nuclear Information System (INIS)

    Rajalakshmi, K.; Abraham John, S.

    2015-01-01

    present strategy of modifying FMWCNTs was extended to prepare a composite electrode by electrochemically depositing 5-amino-2-mercapto-1,3,4-thiadiazole (AMT) film. The FMWCNTs-polymer composite electrode dramatically enhanced the GMP oxidation current when compared to polymerization of AMT (p-AMT) and FMWCNTs alone. The polymer composite electrode was successfully employed for the sensitive determination of GMP. Using amperometry, a limit of detection of 0.27 μM (S/N = 3) was achieved for GMP at a composite modified electrode

  6. Architecture of poly(o-phenylenediamine)–Ag nanoparticle composites for a hydrogen peroxide sensor

    International Nuclear Information System (INIS)

    Wang Li; Zhu Haozhi; Song Yonghai; Liu Li; He Zhifang; Wan Lingli; Chen Shouhui; Xiang Ying; Chen Shusheng; Chen Jie

    2012-01-01

    Graphical abstract: Schematic representation of the formation process of AgNPs/PoPD/GCE via a two-step procedure consisting of electropolymerization of o-PD and electrodeposition of AgNPs and their application in H 2 O 2 detection. Highlights: ► o-Phenylenediamine (o-PD) was electropolymerized on a glassy carbon electrode (GCE). ► The conductive PoPD film was three-dimensional (3D) porous structure. ► Ag NPs formed by electrodepositing and uniformly dispersed on the 3D PoPD film. ► AgNPs/PoPD/GCE displayed good electrocatalytic activity to the reduction of H 2 O 2 . - Abstract: A novel strategy to fabricate a hydrogen peroxide (H 2 O 2 ) sensor was developed by electrodepositing Ag nanoparticles (AgNPs) on a poly(o-phenylenediamine) (PoPD) film modified glassy carbon electrode (GCE). Firstly, the o-phenylenediamine was polymerized on a GCE by potential cycling to produce PoPD film. Then the AgNPs were electrodeposited on the PoPD film to form AgNPs/PoPD/GCE. The morphology of the electropolymerized PoPD film and the electrodeposited AgNPs were characterized by atomic force microscopy. The results showed the PoPD film was porous and the AgNPs dispersed uniformly on the PoPD film. Cylic voltammetry and amperometry were used to evaluate electrocatalytic properties of the AgNPs/PoPD/GCE. The electrode displayed good electrocatalytic activity in the reduction of H 2 O 2 and could be used as a sensor for H 2 O 2 detection. The sensor exhibited fast amperometric response to H 2 O 2 with high selectivity, good reproducibility and stability. The linear range was 6.0 μM to 67.3 mM with a detection limit of 1.5 μM. Thus, it is considered to be an ideal candidate for practical application.

  7. Simultaneous determination of dopamine, uric acid and nitrite using carboxylated graphene oxide/lanthanum modified electrode

    International Nuclear Information System (INIS)

    Ye, Fengying; Feng, Chenqi; Jiang, Jibo; Han, Sheng

    2015-01-01

    Highlights: • The carboxylated graphene oxide/lanthanum-modified glassy carbon electrode (GO-COOLa/GCE) was successfully utilized for the simultaneous detection and quantification of DA, UA and NO 2 − . • Combining the benefits of carboxylated graphene oxide and lanthanum, the modified sensor displayed large peak separations, long linear ranges and low detection limits for simultaneously detecting DA, UA and NO 2 − . • The GO-COOLa/GCE electrode showed well stability, good repeatability, rapid response, and high catalytic performance toward the oxidations of DA, UA and NO 2 − . - Abstract: A bare glassy carbon electrode (GCE) was reformed by carboxylated graphene oxide/lanthanum, and the modified electrode, called GO-COOLa/GCE, was fabricated for simultaneously detecting dopamine (DA), uric acid (UA) and nitrite (NO 2 − ) by cyclic voltammetry (CV), differential pulse voltammetry (DPV) and amperometry. Several factors which affected the electrocatalytic activity of the GO-COOLa/GCE electrode, such as the effect of pH, scan rate and concentration were studied. Due to the combination of carboxylated graphene oxide and lanthanum ions, the GO-COOLa/GCE sensor showed rapid response, excellent selectivity and high catalytic performance toward the electrooxidation of DA, UA and NO 2 − . In optimized conditions, two linear response ranges for determining DA were obtained over ranges of 0.01-1.96×10 2 μM and 1.96×10 2 -1.23×10 3 μM with detection limit of 0.018 μM (S/N = 3). And the responses of the GO-COOLa/GCE electrode for UA and NO 2 − were linear in the region of 1-1.53×10 3 μM and 1-2.75×10 3 μM with detection limits of 0.058 μM and 0.070 μM, respectively. Furthermore, this reformed electrode was successfully used to the detection of DA, UA and NO 2 − in real urine and serum samples, showing its promising application in the electroanalysis of real samples.

  8. Synthesis and semiconducting properties of tin(II) sulfide: Application to photocatalytic degradation of Rhodamine B under sun light

    Energy Technology Data Exchange (ETDEWEB)

    Kabouche, S. [Laboratory of Electrochemistry-Corrosion, Metallurgy and Inorganic Chemistry, Faculty of Chemistry, U.S.T.H.B., BP 32, Algiers, 16111 (Algeria); Bellal, B. [Laboratory of Storage and Valorization of Renewable Energies, Faculty of the Chemistry, U.S.T.H.B., BP 32, Algiers, 16111 (Algeria); Louafi, Y. [Laboratory of Electrochemistry-Corrosion, Metallurgy and Inorganic Chemistry, Faculty of Chemistry, U.S.T.H.B., BP 32, Algiers, 16111 (Algeria); Trari, M., E-mail: solarchemistry@gmail.com [Laboratory of Storage and Valorization of Renewable Energies, Faculty of the Chemistry, U.S.T.H.B., BP 32, Algiers, 16111 (Algeria)

    2017-07-01

    We have investigated the semiconducting and photoelectrochemical properties of SnS grown by a template-free chemical route using thiourea as precursor. Tin(II) sulfide is characterized by X-ray diffraction, scanning electron microscopy, diffuse reflectance and Raman spectroscopy. The X-ray diffraction indicates an orthorhombic SnS phase (SG: Pbnm) with a crystallite size of 52 nm while the optical measurements give a direct band gap of 1.33 eV. The Mott–Schottky plot exhibits a linear behavior, characteristic of n-type conductivity with a flat band potential of 0.19 V{sub SCE} and a donor density of 4.12 × 10{sup 18} cm{sup -3}. The electrochemical impedance spectroscopy (EIS) measured in the range (10{sup -2}–5 × 10{sup 4} Hz) shows one semicircle attributed to the bulk resistance (R{sub b} = 20.37 kΩ cm{sup 2}). The conduction band, located at 4.84 eV below vacuum, is made up of Sn{sup 2+:}5p while the valence band (6.17 eV) derives mainly from S{sup 2-}: 3p character. The energy band diagram, constructed from the photoelectrochemical characterization, predicts the photodegradation of Rhodamine B on SnS by H{sub 2}O{sub 2} generated photoelectrochemically. 88.46% of the initial concentration (10 mg L{sup -1}) disappears after adsorption and 4 h of exposure to solar light. The photoactivity is nearly restored during the second cycle and follows a second order kinetic with a rate constant of 1.55 × 10{sup -3} mg{sup -1} L min{sup -1}. - Highlights: • The semiconducting properties of SnS synthesized by chemical route are studied. • The n type conductivity is evidenced by chrono-amperometry and photoelectrochemistry. • The conduction band, located at 4.84 eV below vacuum, is made up of Sn{sup 2+}: 5p. • SnS was successfully used for the Rhodamine B oxidation under sunlight.

  9. Wireless Instantaneous Neurotransmitter Concentration System-based amperometric detection of dopamine, adenosine, and glutamate for intraoperative neurochemical monitoring.

    Science.gov (United States)

    Agnesi, Filippo; Tye, Susannah J; Bledsoe, Jonathan M; Griessenauer, Christoph J; Kimble, Christopher J; Sieck, Gary C; Bennet, Kevin E; Garris, Paul A; Blaha, Charles D; Lee, Kendall H

    2009-10-01

    In a companion study, the authors describe the development of a new instrument named the Wireless Instantaneous Neurotransmitter Concentration System (WINCS), which couples digital telemetry with fast-scan cyclic voltammetry (FSCV) to measure extracellular concentrations of dopamine. In the present study, the authors describe the extended capability of the WINCS to use fixed potential amperometry (FPA) to measure extracellular concentrations of dopamine, as well as glutamate and adenosine. Compared with other electrochemical techniques such as FSCV or high-speed chronoamperometry, FPA offers superior temporal resolution and, in combination with enzyme-linked biosensors, the potential to monitor nonelectroactive analytes in real time. The WINCS design incorporated a transimpedance amplifier with associated analog circuitry for FPA; a microprocessor; a Bluetooth transceiver; and a single, battery-powered, multilayer, printed circuit board. The WINCS was tested with 3 distinct recording electrodes: 1) a carbon-fiber microelectrode (CFM) to measure dopamine; 2) a glutamate oxidase enzyme-linked electrode to measure glutamate; and 3) a multiple enzyme-linked electrode (adenosine deaminase, nucleoside phosphorylase, and xanthine oxidase) to measure adenosine. Proof-of-principle analyses included noise assessments and in vitro and in vivo measurements that were compared with similar analyses by using a commercial hardwired electrochemical system (EA161 Picostat, eDAQ; Pty Ltd). In urethane-anesthetized rats, dopamine release was monitored in the striatum following deep brain stimulation (DBS) of ascending dopaminergic fibers in the medial forebrain bundle (MFB). In separate rat experiments, DBS-evoked adenosine release was monitored in the ventrolateral thalamus. To test the WINCS in an operating room setting resembling human neurosurgery, cortical glutamate release in response to motor cortex stimulation (MCS) was monitored using a large-mammal animal model, the pig. The

  10. Wireless Instantaneous Neurotransmitter Concentration System–based amperometric detection of dopamine, adenosine, and glutamate for intraoperative neurochemical monitoring

    Science.gov (United States)

    Agnesi, Filippo; Tye, Susannah J.; Bledsoe, Jonathan M.; Griessenauer, Christoph J.; Kimble, Christopher J.; Sieck, Gary C.; Bennet, Kevin E.; Garris, Paul A.; Blaha, Charles D.; Lee, Kendall H.

    2009-01-01

    Object In a companion study, the authors describe the development of a new instrument named the Wireless Instantaneous Neurotransmitter Concentration System (WINCS), which couples digital telemetry with fast-scan cyclic voltammetry (FSCV) to measure extracellular concentrations of dopamine. In the present study, the authors describe the extended capability of the WINCS to use fixed potential amperometry (FPA) to measure extracellular concentrations of dopamine, as well as glutamate and adenosine. Compared with other electrochemical techniques such as FSCV or high-speed chronoamperometry, FPA offers superior temporal resolution and, in combination with enzyme-linked biosensors, the potential to monitor nonelectroactive analytes in real time. Methods The WINCS design incorporated a transimpedance amplifier with associated analog circuitry for FPA; a microprocessor; a Bluetooth transceiver; and a single, battery-powered, multilayer, printed circuit board. The WINCS was tested with 3 distinct recording electrodes: 1) a carbon-fiber microelectrode (CFM) to measure dopamine; 2) a glutamate oxidase enzyme-linked electrode to measure glutamate; and 3) a multiple enzyme-linked electrode (adenosine deaminase, nucleoside phosphorylase, and xanthine oxidase) to measure adenosine. Proof-of-principle analyses included noise assessments and in vitro and in vivo measurements that were compared with similar analyses by using a commercial hardwired electrochemical system (EA161 Picostat, eDAQ; Pty Ltd). In urethane-anesthetized rats, dopamine release was monitored in the striatum following deep brain stimulation (DBS) of ascending dopaminergic fibers in the medial forebrain bundle (MFB). In separate rat experiments, DBS-evoked adenosine release was monitored in the ventrolateral thalamus. To test the WINCS in an operating room setting resembling human neurosurgery, cortical glutamate release in response to motor cortex stimulation (MCS) was monitored using a large-mammal animal

  11. Phosphomimetic mutation of cysteine string protein-α increases the rate of regulated exocytosis by modulating fusion pore dynamics in PC12 cells.

    Directory of Open Access Journals (Sweden)

    Ning Chiang

    Full Text Available BACKGROUND: Cysteine string protein-α (CSPα is a chaperone to ensure protein folding. Loss of CSPα function associates with many neurological diseases. However, its function in modulating regulated exocytosis remains elusive. Although cspα-knockouts exhibit impaired synaptic transmission, overexpression of CSPα in neuroendocrine cells inhibits secretion. These seemingly conflicting results lead to a hypothesis that CSPα may undergo a modification that switches its function in regulating neurotransmitter and hormone secretion. Previous studies implied that CSPα undergoes phosphorylation at Ser10 that may influence exocytosis by altering fusion pore dynamics. However, direct evidence is missing up to date. METHODOLOGY/PRINCIPAL FINDINGS: Using amperometry, we investigated how phosphorylation at Ser10 of CSPα (CSPα-Ser10 modulates regulated exocytosis and if this modulation involves regulating a specific kinetic step of fusion pore dynamics. The real-time exocytosis of single vesicles was detected in PC12 cells overexpressing control vector, wild-type CSPα (WT, the CSPα phosphodeficient mutant (S10A, or the CSPα phosphomimetic mutants (S10D and S10E. The shapes of amperometric signals were used to distinguish the full-fusion events (i.e., prespike feet followed by spikes and the kiss-and-run events (i.e., square-shaped flickers. We found that the secretion rate was significantly increased in cells overexpressing S10D or S10E compared to WT or S10A. Further analysis showed that overexpression of S10D or S10E prolonged fusion pore lifetime compared to WT or S10A. The fraction of kiss-and-run events was significantly lower but the frequency of full-fusion events was higher in cells overexpressing S10D or S10E compared to WT or S10A. Advanced kinetic analysis suggests that overexpression of S10D or S10E may stabilize open fusion pores mainly by inhibiting them from closing. CONCLUSIONS/SIGNIFICANCE: CSPα may modulate fusion pore dynamics

  12. Modification of glassy carbon electrode with multi-walled carbon nanotubes and iron(III)-porphyrin film: Application to chlorate, bromate and iodate detection

    Energy Technology Data Exchange (ETDEWEB)

    Salimi, Abdollah [Department of Chemistry, University of Kurdistan, P.O. Box 416, Sanandaj (Iran, Islamic Republic of); Nanotechnology Research Center of University of Kurdistan, P.O. Box 416, Sanandaj (Iran, Islamic Republic of); E-mail: absalimi@uok.ac.ir; MamKhezri, Hussein [Department of Chemistry, University of Kurdistan, P.O. Box 416, Sanandaj (Iran, Islamic Republic of); Hallaj, Rahman [Department of Chemistry, University of Kurdistan, P.O. Box 416, Sanandaj (Iran, Islamic Republic of); Zandi, Shiva [Laboratory of Biochemistry, Kurdistan Medical University, Sanandaj (Iran, Islamic Republic of)

    2007-06-10

    In this study, multi-wall carbon nanotubes (MWCTs) is evaluated as a transducer, stabilizer and immobilization matrix for the construction of amperometric sensor based on iron-porphyrin. 5,10,15,20-Tetraphenyl-21H,23H-porphine iron(III) chloride (Fe(III)P) adsorbed on MWCNTs immobilized on the surface of glassy carbon electrode. Cyclic voltammograms of the Fe(III)P-incorporated-MWCNTs indicate a pair of well-defined and nearly reversible redox couple with surface confined characteristics at wide pH range (2-12). The surface coverage ({gamma}) and charge transfer rate constant (k {sub s}) of Fe(III)P immobilized on MWCNTs were 7.68 x 10{sup -9} mol cm{sup -2} and 1.8 s{sup -1}, respectively, indicating high loading ability of MWCNTs for Fe(III)P and great facilitation of the electron transfer between Fe(III)P and carbon nanotubes immobilized on the electrode surface. Modified electrodes exhibit excellent electrocatalytic activity toward reduction of ClO{sub 3} {sup -}, IO{sub 3} {sup -} and BrO{sub 3} {sup -} in acidic solutions. The catalytic rate constants for catalytic reduction of bromate, chlorate and iodate were 6.8 x 10{sup 3}, 7.4 x 10{sup 3} and 4.8 x 10{sup 2} M{sup -1} s{sup -1}, respectively. The hydrodynamic amperometry of rotating-modified electrode at constant potential versus reference electrode was used for detection of bromate, chlorate and iodate. The detection limit, linear calibration range and sensitivity for chlorate, bromate and iodate detections were 0.5 {mu}M, 2 {mu}M to 1 mM, 8.4 nA/{mu}M, 0.6 {mu}M, 2 {mu}M to 0.15 mM, 11 nA/{mu}M, and 2.5 {mu}M, 10 {mu}M to 4 mM and 1.5 nA/{mu}M, respectively. Excellent electrochemical reversibility of the redox couple, good reproducibility, high stability, low detection limit, long life time, fast amperometric response time, wide linear concentration range, technical simplicity and possibility of rapid preparation are great advantages of this sensor. The obtained results show promising practical

  13. An improved glycerol biosensor with an Au-FeS-NAD-glycerol-dehydrogenase anode.

    Science.gov (United States)

    Mahadevan, Aishwarya; Fernando, Sandun

    2017-06-15

    An improved glycerol biosensor was developed via direct attachment of NAD + -glycerol dehydrogenase coenzyme-apoenzyme complex onto supporting gold electrodes, using novel inorganic iron (II) sulfide (FeS)-based single molecular wires. Sensing performance factors, i.e., sensitivity, a detection limit and response time of the FeS and conventional pyrroloquinoline quinone (PQQ)-based biosensor were evaluated by dynamic constant potential amperometry at 1.3V under non-buffered conditions. For glycerol concentrations ranging from 1 to 25mM, a 77% increase in sensitivity and a 53% decrease in detection limit were observed for the FeS-based biosensor when compared to the conventional PQQ-based counterpart. The electrochemical behavior of the FeS-based glycerol biosensor was analyzed at different concentrations of glycerol, accompanied by an investigation into the effects of applied potential and scan rate on the current response. Effects of enzyme stimulants ((NH 4 ) 2 SO 4 and MnCl 2 ·4H 2 O) concentrations and buffers/pH (potassium phosphate buffer pH 6-8, Tris buffer pH 8-10) on the current responses generated by the FeS-based glycerol biosensor were also studied. The optimal detection conditions were 0.03M (NH 4 ) 2 SO 4 and 0.3µm MnCl 2 ·4H 2 O in non-buffered aqueous electrolyte under stirring whereas under non-stirring, Tris buffer at pH 10 with 0.03M (NH 4 ) 2 SO 4 and 30µm MnCl 2 ·4H 2 O were found to be optimal detection conditions. Interference by glucose, fructose, ethanol, and acetic acid in glycerol detection was studied. The observations indicated a promising enhancement in glycerol detection using the novel FeS-based glycerol sensing electrode compared to the conventional PQQ-based one. These findings support the premise that FeS-based bioanodes are capable of biosensing glycerol successfully and may be applicable for other enzymatic biosensors. Copyright © 2016 Elsevier B.V. All rights reserved.

  14. Photoelectrochemical properties of TiO2 Nanotube Arrays Modified with BiOCl nanosheets

    International Nuclear Information System (INIS)

    Liu, Haipeng; Xu, Guangqing; Wang, Jinwen; Lv, Jun; Zheng, Zhixiang; Wu, Yucheng

    2014-01-01

    Highlights: • BiOCl were deposited on TiO2 NTAs by sequential chemical bath deposition. • BiOCl can decrease background photocurrent and increase current response. • High sensitivity BiOCl/TiO2 is due to the direct oxidation of organics on BiOCl. - Abstract: BiOCl nanosheets were deposited on anodized TiO 2 nanotube arrays (NTAs) by sequential chemical bath deposition method to get BiOCl/TiO 2 NTAs for photoelectrochemical detection of organic compounds (represented by glucose). The structures, elemental components and morphologies of TiO 2 and BiOCl/TiO 2 NTAs were characterized by using X-ray diffraction diffractometer, scanning electron microscope and transmission electron microscope. The photoelectrochemical behaviors of TiO 2 and BiOCl/TiO 2 NTAs in the buffer and glucose solutions were measured by cyclic votammetry and amperometry with different optical powers. The modification of BiOCl nanosheets on TiO 2 NTAs decreases the photocurrents of TiO 2 NTAs in the buffer solution and increases the current response to glucose. Both of the background photocurrent decrease and current response increase are benefit for photoelectrochemical detection of organic compounds. When glucose was used as the target organic compound, the optimized BiOCl/TiO 2 NTAs sensor achieved a sensitivity of 0.327 μA/μM (0.417 μA·cm −2 ·μM −1 ), linear range from 0 to 1300 μM and calculated detection limit of 5.7 μM. Mechanisms of BiOCl modification were studied by measuring the optical absorption and hydroxyl radical HO· productivity. The transfer of holes from TiO 2 to BiOCl and the direct oxidation of organic compounds on BiOCl nanosheets led to the decrease of background photocurrent (lower reaction rate of water splitting on BiOCl nanosheets) and the increase of current response to organic compounds (higher reaction rate of direct oxidation of organic compounds)

  15. Chrono-potentiometry in molten chlorides. Application to the study of the electrochemical properties of uranium and plutonium in the LiCl-KCl eutectic; Chronopotentiometrie dans les chlorures fondus. Application a l'etude des proprietes electrochimiques de l'uranium et du plutonium dans l'eutectique LiCl-KCl

    Energy Technology Data Exchange (ETDEWEB)

    Leseur, A. [Commissariat a l' Energie Atomique, Fontenay-aux-Roses (France). Centre d' Etudes Nucleaires

    1969-05-01

    Using solutions of cadmium chloride in the eutectic LiCl-KCl, a chrono-potentiometric method has been developed with a view to its application to the study of molten solutions. Particular attention has been paid to the choice of the indicator electrodes. The method makes it possible to analyze molten solutions quantitatively and to determine diffusion coefficients and their activation energies; it yields furthermore information about the nature and the behaviour of ionic species in solution. The method has been applied to the study of solutions of uranium and plutonium chloride in the eutectic LiCl-KCl. Linear chrono-amperometry has been used for studying these solutions quantitatively, but chrono-potentiometry, of which the theory is better developed, is better suited to a quantitative study. The results obtained have made it possible to determine the diffusion coefficients of the ions Cd{sup 2+}, U{sup 3+}, U{sup 4+} and U(IV) in the presence of F{sup -} and Pu{sup 3+} ions, as well as the activation energy of the diffusion coefficients. (author) [French] La mise au point de la chronopotentiometrie comme moyen d'etude des solutions fondues a ete effectuee avec des solutions de chlorure de cadmium dans l'eutectique LiCl-KCl. Le probleme du choix des electrodes indicatrices a ete particulierement etudie. La methode permet l'analyse quantitative des solutions fondues ainsi que la determination des coefficients de diffusion et de leurs energies d'activation: elle donne en outre des renseignements sur la nature et le comportement des especes ioniques en solution. Elle a ete appliquee a l'etude des solutions des chlorures d'uranium et de plutonium dans l'eutectique LiCl-KCl. La chronoamperometrie lineaire a ete utilisee pour l'etude qualitative de ces solutions, mais la chronopotentiometrie, dont la theorie est plus complete, convient mieux pour l'etude quantitative. Les resultats obtenus ont permis de determiner les

  16. Direct and mediated electrochemistry of peroxidase and its electrocatalysis on a variety of screen-printed carbon electrodes: amperometric hydrogen peroxide and phenols biosensor.

    Science.gov (United States)

    Chekin, Fereshteh; Gorton, Lo; Tapsobea, Issa

    2015-01-01

    This study compares the behaviour of direct and mediated electrochemistry of horseradish peroxidase (HRP) immobilised on screen-printed carbon electrodes (SPCEs), screen-printed carbon electrodes modified with carboxyl-functionalised multi-wall carbon nanotubes (MWCNT-SPCEs) and screen-printed carbon electrodes modified with carboxyl-functionalised single-wall carbon nanotubes (SWCNT-SPCEs). The techniques of cyclic voltammetry and amperometry in the flow mode were used to characterise the properties of the HRP immobilised on screen-printed electrodes. From measurements of the mediated and mediatorless currents of hydrogen peroxide reduction at the HRP-modified electrodes, it was concluded that the fraction of enzyme molecules in direct electron transfer (DET) contact with the electrode varies substantially for the different electrodes. It was observed that the screen-printed carbon electrodes modified with carbon nanotubes (MWCNT-SPCEs and SWCNT-SPCEs) demonstrated a substantially higher percentage (≈100 %) of HRP molecules in DET contact than the screen-printed carbon electrodes (≈60 %). The HRP-modified electrodes were used for determination of hydrogen peroxide in mediatorless mode. The SWCNT-SPCE gave the lowest detection limit (0.40 ± 0.09 μM) followed by MWCNT-SPCE (0.48 ± 0.07 μM) and SPCE (0.98 ± 0.2 μM). These modified electrodes were additionally developed for amperometric determination of phenolic compounds. It was found that the SWCNT-SPCE gave a detection limit for catechol of 110.2 ± 3.6 nM, dopamine of 640.2 ± 9.2 nM, octopamine of 3341 ± 15 nM, pyrogallol of 50.10 ± 2.9 nM and 3,4-dihydroxy-L-phenylalanine of 980.7 ± 8.7 nM using 50 μM H2O2 in the flow carrier.

  17. [Comparative evaluation of antioxidant activity and content of prooxidant factors in different classes of foods].

    Science.gov (United States)

    Bykov, I M; Basov, A A; Bykov, M I; Khanfer'ian, R A

    2014-01-01

    By using the biophysical methods (chemiluminescence, amperometry) in laboratory in vitro experiments it was demonstrated that the study of antioxidant and pro-oxidant activities of different food groups allows to perform a preliminary assessment of their pro-oxidant-antioxidant capacity. It have been shown that some food prevails ability to exert pro-oxidant effects (in vitro) due to the short-term induction of free radical oxidation. Thus, among the fresh juices the increase of the maximum of flash chemiluminescence has been detected in avocado (1080, 89%) and pearjuices (136,33%), whereas the lowest ability to enhance the intensity of free radical processes has been marked for pomegranate (1,63%), orange (9, 68%) and apples juices (12, 84%). Among milk products it has been marked for sour milk (9, 06%) and yogurt (15, 11-16,02%), that allows the use of the past to correct pro-oxidant-antioxidant balance diet for people with potential danger gain peroxide processes, such as special physiological states, sport endurance, mental and emotional overload. The ability to increase the intensity of free radical oxidation have been also identified for snacks, especially buns, biscuits, bread sticks, showing the risk of formation of oxidative stress in the body during their prolonged use, particularly under the above described conditions. In some cases, foods (processed cheese and cheese curds) showed dominance factors sustained oxidative effect (in 2,1-20,7%), that indicates the possibility of an imbalance in the pro-oxidant-antioxidant system after its prolonged use in the diet, even in small quantities, especially in individuals with a reduced level of antioxidant potential of the nonspecific defense system. Investigation of antioxidant activity of foods revealed significant predominance of reducing equivalents in all freshly squeezed and some packaged fruit juices, as well as dairy products, indicating their possibility to increase the capacity of reducing components of

  18. Immunogenicity and ecotoxicity of engineered nanoparticles

    Science.gov (United States)

    Maurer-Jones, Melissa Ann

    The growing use of nanoscale materials in commercially available products and therapeutics has created an urgent need to determine the toxicity of these materials so that they may be designed and employed safely. As nanoparticles have unique physical and chemical properties, the challenges in determining their physiological and environmental impact have been numerous. It is, therefore, the goal of my thesis work to employ sensitive analytical tools to fundamentally understand the how nanoparticles interact with immunologically and ecologically relevant models. My project approaches nanotoxicity studies starting with a relevant model system exposed to well-characterized nanoparticles to (1) determine if cells/organisms survive exposure using traditional toxicological assays and, if the majority survives exposure, (2) use sensitive analytical tools to determine if there are changes to critical cell/organism function. If perturbation of function is detected, (3) the mechanism or cause of changes in cell function should be determined, including assessment of nanoparticle uptake and localization. Once a mechanism of interaction is determined, this process could begin again with a modified particle that may address the toxic response. Chapter Two describes the impact of metal oxide (TiO2 and SiO2) nanoparticles on mast cells, critical immune system cells, and utilizes the sensitive technique of carbon-fiber microelectrode amperometry (CFMA) to monitor changes in the important mast cell function of exocytosis. Chapter Three expands upon Chapter Two and examines in more detail the mechanism by which TiO2 nanoparticles impact exocytotic cell function, completing the process nanotoxicity described above. From these studies, it was determined that, while nanoparticles do not decrease the viability of mast cells, there are significant changes to exocytosis upon nanoparticle exposure, and in the case of TiO2, these changes in exocytosis are correlated to nanoparticle

  19. A novel reagentless glutamate microband biosensor for real-time cell toxicity monitoring

    Energy Technology Data Exchange (ETDEWEB)

    Hughes, G.; Pemberton, R.M. [Centre for Research in Biosciences, Faculty of Health and Applied Sciences, University of the West of England, Bristol, Coldharbour Lane, Bristol, BS16 1QY (United Kingdom); Fielden, P.R. [Department of Chemistry, Lancaster University, Bailrigg, Lancaster, LA1 4YB (United Kingdom); Hart, J.P., E-mail: john.hart@uwe.ac.uk [Centre for Research in Biosciences, Faculty of Health and Applied Sciences, University of the West of England, Bristol, Coldharbour Lane, Bristol, BS16 1QY (United Kingdom)

    2016-08-24

    A reagentless glutamate biosensor was applied to the determination of glutamate released from liver hepatocellular carcinoma cells (HepG2) in response to toxic challenge from various concentrations of paracetamol. A screen printed carbon electrode (SPCE) containing the electrocatalyst Meldola's Blue (MB-SPCE) served as the electron mediator for the oxidation of NADH. A mixture of the enzyme glutamate dehydrogenase (GLDH), cofactor nicotinamide adenine dinucleotide (NAD{sup +}) and the biopolymer chitosan (CHIT) were drop-coated onto the surface of the transducer (MB-SPCE) in a simple one step fabrication process. The reagentless biosensor was used with amperometry in stirred solution at an applied potential of +0.1 V (vs. Ag/AgCl). All experiments were carried out at the following conditions: pH 7, temperature 37 °C, atmosphere 5% CO{sub 2}. The linear range of the device was found to be 25–125 μM in phosphate buffer (75 mM, containing 0.05 M NaCl) and 25–150 μM in cell culture medium. The limits of detection (LOD) were found to be 1.2 μM and 4.2 μM based on three times signal to noise, using PBS and culture medium respectively. The sensitivity was calculated to be 106 nA μM{sup −1} cm{sup −2} and 210 nA μM{sup −1} cm{sup −2} in PBS and cell medium respectively. The response time was ∼60 s in an agitated solution. HepG2 cells were exposed to various concentrations of paracetamol (1 mM, 5 mM and 10 mM) in order to investigate the drug-induced release of glutamate into the culture medium in real time. Two toxicity studies were investigated using different methods of exposure and analysis. The first method consisted of a single measurement of the glutamate concentration, using the method of standard addition, after 24 h incubation. The concentrations of glutamate were found to be 52 μM, 93 μM and 177 μM, released on exposure to 1 mM, 5 mM and 10 mM paracetamol respectively. The second method involved the

  20. A novel reagentless glutamate microband biosensor for real-time cell toxicity monitoring

    International Nuclear Information System (INIS)

    Hughes, G.; Pemberton, R.M.; Fielden, P.R.; Hart, J.P.

    2016-01-01

    A reagentless glutamate biosensor was applied to the determination of glutamate released from liver hepatocellular carcinoma cells (HepG2) in response to toxic challenge from various concentrations of paracetamol. A screen printed carbon electrode (SPCE) containing the electrocatalyst Meldola's Blue (MB-SPCE) served as the electron mediator for the oxidation of NADH. A mixture of the enzyme glutamate dehydrogenase (GLDH), cofactor nicotinamide adenine dinucleotide (NAD"+) and the biopolymer chitosan (CHIT) were drop-coated onto the surface of the transducer (MB-SPCE) in a simple one step fabrication process. The reagentless biosensor was used with amperometry in stirred solution at an applied potential of +0.1 V (vs. Ag/AgCl). All experiments were carried out at the following conditions: pH 7, temperature 37 °C, atmosphere 5% CO_2. The linear range of the device was found to be 25–125 μM in phosphate buffer (75 mM, containing 0.05 M NaCl) and 25–150 μM in cell culture medium. The limits of detection (LOD) were found to be 1.2 μM and 4.2 μM based on three times signal to noise, using PBS and culture medium respectively. The sensitivity was calculated to be 106 nA μM"−"1 cm"−"2 and 210 nA μM"−"1 cm"−"2 in PBS and cell medium respectively. The response time was ∼60 s in an agitated solution. HepG2 cells were exposed to various concentrations of paracetamol (1 mM, 5 mM and 10 mM) in order to investigate the drug-induced release of glutamate into the culture medium in real time. Two toxicity studies were investigated using different methods of exposure and analysis. The first method consisted of a single measurement of the glutamate concentration, using the method of standard addition, after 24 h incubation. The concentrations of glutamate were found to be 52 μM, 93 μM and 177 μM, released on exposure to 1 mM, 5 mM and 10 mM paracetamol respectively. The second method involved the continuous monitoring of glutamate

  1. Electrochemical properties of uranium, cerium, and zirconium in the lithium fluoride - barium fluoride eutectic; Proprietes electrochimiques de l'uranium, du cerium et du zirconium dans l'eutectique fluorure de lithium - fluorure de baryum

    Energy Technology Data Exchange (ETDEWEB)

    Cartier, R [Commissariat a l' Energie Atomique, Fontenay-aux-Roses (France). Centre d' Etudes Nucleaires

    1969-07-01

    The aim of this work has been to determine the possibility of carrying out an electrochemical analysis of the ions U{sup 4+}, Ce{sup 3+}, Zr{sup 4+} in a fluoride melt, and to obtain some of the electrochemical properties of these ions. It was first of all necessary to develop a method for purifying the LiF-BaF{sub 2} eutectic so as to have melts of sufficient purity for carrying out an electrochemical study using linear chrono-amperometry and chrono-potentiometry. The polarization curves recorded in solutions for the ions U{sup 4+}, Ce{sup 3+}, Zr{sup 4+} show that the systems U{sup 4+}/U{sup 3+}, Ce{sup 3+}/Ce{sup 4+} and Zr{sup 4+}/Zr are rapid. After it had been checked that mass transport on the electrode is controlled by diffusion, the diffusion coefficients for the ions Ce{sup 3+}, U{sup 4+} and Zr{sup 4+} were determined. The oxidizing nature of the ion Ce{sup 4+} makes it possible to dissolve ceric oxide in the molten fluoride. Furthermore the existence of two zirconium oxyfluorides has been demonstrated, they appear after dissolution of the zirconia in a solution of zirconium tetrafluoride. From a practical point of view these results are of interest for the preparation of metals by electrolytic reduction of their oxides. (author) [French] Le but de ce travail est de determiner la possibilite d'analyse electrochimique des ions U{sup 4+}, Ce{sup 3+}, Zr{sup 4+} dans un bain de fluorures fondus et de mettre en evidence quelques proprietes electrochimiques de ces ions. Il a tout d'abord ete necessaire de mettre au point une methode de purification de l'eutectique LiF-BaF{sub 2} afin d'obtenir des bains suffisamment purs pour realiser une etude electrochimique par chronoamperometrie lineaire et par chronopotentiometrie. L'enregistrement des courbes de polarisation dans des solutions des ions U{sup 4+}, Ce{sup 3+}, Zr{sup 4+} montre que les systemes U{sup 4+}/U{sup 3+}, Ce{sup 3+}/Ce{sup 4+}, Zr{sup 4+}/Zr sont rapides. Apres avoir verifie que le transport de

  2. Corrosion kinetics of alloy Ni-22Cr-13Mo-3W as structural material in high level nuclear waste containers

    International Nuclear Information System (INIS)

    Rodriguez, Martin A.

    2004-01-01

    Alloy Ni-22Cr-13Mo-3W (also known as C-22) is one of the candidates to fabricate high level nuclear waste containers. These containers are designed to maintain isolation of the waste for a minimum of 10,000 years. In this period, the material must be resistant to corrosion. If the containers were in contact with water, it is assumed that alloy C-22 may undergo three different corrosion mechanisms: general corrosion, localized corrosion and stress corrosion cracking. This thesis discusses only the first two types of degradation. Electrochemical techniques such as amperometry, potentiometry, potentiodynamic polarization and electrochemical impedance spectroscopy (EIS) and non-electrochemical techniques such as microscopic observation, X-ray fluorescence (XRF) and X-ray photoelectron spectroscopy (XPS) were applied to study the corrosion behavior of alloy C-22 in 1 M NaCl, 25 C degrees saturated NaF (approximately 1 M) and 0,5 M NaCl + 0,5 M NaF solutions. Effects of temperature, pH and alloy thermal aging were analyzed. The corrosion rates obtained at 90 C degrees were low ranging from 0.04 μm/year to 0.48 μm /year. They increased with temperature and decreased with solution pH. Most of the impedance measurements showed a simply capacitive behavior. A second high-frequency time constant was detected in some cases. It was attributed to the formation of a nickel oxide and/or hydroxide at potentials near the reversible potential for this reaction. The active/passive transition detected in some potentiodynamic polarization curves was attributed to the same process. The corrosion potential showed an important increase after 24 hours of immersion. This increase in the corrosion potential was associated with an improvement of the passive film. The corrosion potential was always lower than the re-passivation potential for the corresponding media. The trans passive behavior of alloy C-22 was mainly influenced by temperature and solution chemistry. A clear trans passive peak

  3. Development of a nanowire based titanium needle probe sensor for glucose monitoring

    Science.gov (United States)

    Deshpande, Devesh C.

    glucose monitoring. The working electrode of the sensor comprised of vertically aligned, free standing Au nanowires to utilize the advantages of nanostructures. The sensor was fabricated on biocompatible titanium substrate using Micro/Nano fabrication processes such as Plasma Enhanced Chemical Vapor Deposition (PECVD), Electron Beam Evaporation, Lithography, aligned nanowire growth and wet and plasma etching. Arrays of free-standing nanowires were grown at room temperature and pressure using a novel template based growth process. After fabrication of the sensor, immobilization of an enzyme was carried out on the sensing electrode to ensure selectivity of the sensor to glucose. This was achieved by using self-assembled thiol monolayers and entrapment in a conducting polymer matrix. Glucose oxidase was used for this purpose, which catalyzed the conversion of glucose to gluconic acid, producing hydrogen peroxide in the process. Amperometry was used for glucose detection, in which a constant voltage was applied to the sensor. This potential oxidized the hydrogen peroxide and produced changes in the current which were correlated to the glucose concentration. This dissertation will address the importance of continuous glucose monitoring, current technology and problems faced, the design and fabrication of the sensor and electrochemical sensing to detect glucose levels in solution. Finally, the problems encountered during the process will be discussed and the future work will be detailed.

  4. Continuous glucose monitoring microsensor with a nanoscale conducting matrix and redox mediator

    Science.gov (United States)

    Pesantez, Daniel

    The major limiting factor in kidney clinical transplantation is the shortage of transplantable organs. The current inability to distinguish viability from non-viability on a prospective basis represents a major obstacle in any attempt to expand organ donor criteria. Consequently, a way to measure and monitor a relevant analyte to assess kidney viability is needed. For the first time, the initial development and characterization of a metabolic microsensor to assess kidney viability is presented. The rate of glucose consumption appears to serve as an indicator of kidney metabolism that may distinguish reversible from irreversible kidney damage. The proposed MetaSense (Metabolic Sensor) microdevice would replace periodic laboratory diagnosis tests with a continuous monitor that provides real-time data on organ viability. Amperometry, a technique that correlates an electrical signal with analyte concentration, is used as a method to detect glucose concentrations. A novel two-electrode electrochemical sensing cell design is presented. It uses a modified metallic working electrode (WE) and a bare metallic reference electrode (RE) that acts as a pseudo-reference/counter electrode as well. The proposed microsensor has the potential to be used as a minimally invasive sensor for its reduced number of probes and very small dimensions achieved by micromachining and lithography. In order to improve selectivity of the microdevice, two electron transfer mechanisms or generations were explored. A first generation microsensor uses molecular oxygen as the electron acceptor in the enzymatic reaction and oxidizes hydrogen peroxide (H2O2) to get the electrical signal. The microsensor's modified WE with conductive polymer polypyrrole (PPy) and corresponding enzyme glucose oxidase (GOx) immobilized into its matrix, constitutes the electrochemical detection mechanism. Photoluminescence spectroscopic analysis confirmed and quantified enzyme immobilized concentrations within the matrix. In