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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. Amperometry of heparin polyion using a rotating disk electrode coated with a plasticized PVC membrane

    Czech Academy of Sciences Publication Activity Database

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

    2006-01-01

    Roč. 18, č. 2 (2006), s. 115-120 ISSN 1040-0397 R&D Projects: GA ČR GA203/04/0424 Institutional research plan: CEZ:AV0Z40400503 Keywords : amperometry * coulometry * heparin polyion * rotating glassy carbon electrode * PVC membrane Subject RIV: CG - Electrochemistry Impact factor: 2.444, year: 2006

  4. 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...

  5. 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

  6. 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

  7. 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 application of the newly developed method for the analysis of free cyanide in drinking water. Copyright © 2017 Elsevier Ltd. All rights reserved.

  8. Pulsed Amperometry for Anti-fouling of Boron-doped Diamond in Electroanalysis of β-Agonists: Application to Flow Injection for Pharmaceutical Analysis

    Directory of Open Access Journals (Sweden)

    Duangjai Nacapricha

    2006-01-01

    Full Text Available This work presents the construction and application of boron-doped diamond(BDD thin film electrode as sensor for the determination of three β-agonists, viz.salbutamol, terbutaline and clenbuterol. Although well-known as a chemically inertmaterial, BDD film however shows fouling in detection of these compounds using fixedpotentialmode amperometry. A suitable waveform for pulsed amperometric detection(PAD was developed and used to determine the agonist compounds. It was seen that thedeveloped PAD significantly refreshed the BDD surface for long-term detection in flowinjection analysis. Linear working ranges were 0.5-100 μM, 1.0-100 μM and 0.5-50 μM forsalbutamol, terbutaline and clenbuterol, respectively. The developed PAD-BDD system wasapplied to successfully determine salbutamol and terbutaline in commercial pharmaceuticalproducts. The methods were validated with a capillary electrophoresis method.

  9. Online Coupling of Lab-on-Valve Format to Amperometry Based on Polyvinylpyrrolidone-Doped Carbon Paste Electrode and Its Application to the Analysis of Morin

    Directory of Open Access Journals (Sweden)

    Yang Wang

    2012-01-01

    Full Text Available The potential capabilities and analytical performance of lab-on-valve (LOV manifold as a front end to amperometry have been explored for the on-line determination of morin. Meanwhile, the electrochemical behaviors of morin were investigated based on polyvinylpyrrolidone- (PVP- doped carbon paste electrode (CPE, which found that PVP can significantly improve its oxidation peak current. The excellent amperometric current response was achieved when the potential difference (ΔE of 0.6 V was implemented in pH 6.5 phosphate buffer solution (PBS that served as the supporting electrolyte. A well-defined oxidation peak has been obtained in studies using PVP as a modifier of CPE based on the oxidation of morin. The present work introduces the LOV technique as a useful tool for amperometric measurement, documents advantages of using programmable flow, and outlines means for miniaturization of assays on the basis of PVP modified CPE. The proposed method was applied successfully to the determination of morin in real samples, and the spiked recoveries were satisfactory.

  10. Simultaneous electrochemical measurement method of histamine and N(τ)-methylhistamine by high-performance liquid chromatography-amperometry with o-phthalaldehyde-sodium sulfite derivatization.

    Science.gov (United States)

    Maldonado, Martin; Maeyama, Kazutaka

    2013-01-01

    An electrochemical detection (ECD) method for analyzing sub-micro amounts of histamine (HA) and N(τ)-methylhistamine (N(τ)-MHA) in biological samples by high-performance liquid chromatography (HPLC)-amperometry has been developed. The method consists of a precolumn derivatization of the amines with o-phthalaldehyde (OPA) and sodium sulfite (Na(2)SO(3)) to N-alkyl-1-isoindole sulfonate and posterior separation with the HPLC system. Biological samples were pretreated by using a Vivapure sulfonic acid minifilter in which the reaction of the reagent with the amines took place during filtering. HA and N(τ)-MHA retention times were 11.8 ± 0.02 and 18.3 ± 0.03 min, respectively (means ± standard deviations, n = 3). The lowest limit of amperometric detection at a signal-to-noise ratio of 3:1 was 0.125 pmol in both cases. HA and N(τ)-MHA contents in hypothalamus, cortex, skin, and fundic gland, as well as histamine N-methyltransferase (HMT) activities of mast cell-deficient (Ws/Ws) and Wistar rats, were measured and compared with an HPLC-fluorometry system, among other experiments, in order to validate and demonstrate the usefulness of this assay system. Hence, this consequently confirms not only the sensitivity and specificity of the assay but also the potential and convenience it offers to laboratory work, especially in the analysis of the regulation of histaminergic neurons as well as enzymatic investigation of HA metabolism. Copyright © 2012 Elsevier Inc. All rights reserved.

  11. 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

  12. Transduction methods used on biosensors: amperometry and fluorescence

    Directory of Open Access Journals (Sweden)

    Juan Bernardo Cano

    2014-01-01

    Full Text Available Los biosensores tienen aplicación en una gran variedad de campos, incluyendo el análisis ambiental, biomedicina, biodefensa, alimentación y agricultura, entre otros. En este tipo de sensores, un material biológico (conocido como biomediador reacciona con el analito y un sistema de transducción apropiado transforma dicha reacción en una señal eléctrica que puede ser procesada, almacenada o transmitida usando sistemas electrónicos. En este artículo, se describen dos métodos de transducción usados en aplicaciones bio-sensoriales: la amperometria que consiste en la medida del transferimento electrónico (corriente del biomediador y fluorescencia que es basada en la medida de la luz re-emitida. Se enfatiza en el diseño electrónico (selección de componentes, topologia de los circuitos, problemas comunes y soluciones. Estos diseños han sido utilizados en el desarrollo de instrumentos comerciales para biosensores, caracterizados por bajos costes de producción y portabilidad.

  13. Determination of Phenolic Acids in Sugarcane Vinasse by HPLC with Pulse Amperometry

    Directory of Open Access Journals (Sweden)

    P. V. Freitas

    2018-01-01

    Full Text Available A reversed-phase liquid chromatographic separation with pulsed amperometric detection of phenolic acids at a glassy carbon electrode is described. Chromatographic separation was carried out in isocratic conditions using 0.20 mol·L−1 acetic acid (pH 5.0/water (80 : 20, v/v as mobile phase under constant working potential mode of 0.80 V. Chromatographic peaks presented high resolution and separation. Calibration curves exhibited excellent correlation coefficients, above 0.995. Linear ranges of the analytes, in mg L−1, were of 0.018–18 (gallic acid, 0.146–19 (vanillic acid, 0.13–17 (caffeic acid, 0.016–16 (ferulic acid, and 0.008–17 (p-coumaric acid, respectively. Limits of detection ranged from 1.6 to 97 μg·L−1 and precision varied in 1.73–3.78% interval. Concentrations of 19 ± 0.51 mg·L−1 and 7.8 ± 2.5 mg·L−1 were found for vanillic and caffeic acids, respectively, in a sugarcane vinasse sample. Gallic, ferulic, and p-coumaric acids were not detected. Recovery results demonstrated that the proposed method is accurate, and it can be used to detect and quantify phenolic acids in sugarcane vinasse without any influence of interferents.

  14. Potential-Dependent Stochastic Amperometry of Multiferrocenylthiophenes in an Electrochemical Nanogap Transducer

    NARCIS (Netherlands)

    Mathwig, Klaus; Zafarani, Hamid R.; Speck, J. Matthaus; Sarkar, S.; Lang, Heinrich; Lemay, Serge Joseph Guy; Rassaei, Liza; Schmidt, Oliver G.

    2016-01-01

    In nanofluidic electrochemical sensors based on redox cycling, zeptomole quantities of analyte molecules can be detected as redox-active molecules travel diffusively between two electrodes separated by a nanoscale gap. These sensors are employed to study the properties of multiferrocenylic compounds

  15. Amperometry with two polarisable electrodes-VII: chelometric determination of indium.

    Science.gov (United States)

    Vydra, F; Vorlícek, J

    1966-03-01

    Optimum conditions have been found for the chelometric determination of indium by biamperometric titration with EDTA. Two stationary platinum electrodes (Pt-Pt) or two graphite electrodes (C-C) may be used to indicate the end-point of the titration. At pH 1-1.5 the determination is highly selective. The applied potential only influences the absolute value of the current ; the accuracy of the determinations remains constant over a wide interval of applied potential. At a potential of 1.0-1.7 V the change of current during a titration with 0.05 M EDTA solution is of the order of 10 microA. Analytical applications of the method are discussed.

  16. Amperometry with two polarisable electrodes-XI Determination of bismuth by EDTA titration.

    Science.gov (United States)

    Vydra, F; Vorlícek, J

    1966-04-01

    Optimum conditions have been found for a highly selective determination of bismuth via EDTA titration with biamperometric indication of the end-point. The influence of the applied potential, pH and stirring on the accuracy and selectivity of the determination has been studied. In a medium of 0.4M nitric acid only high concentrations of iron(III) and copper(II) interfere with the determination of bismuth. Zirconium, thallium(III) and indium interfere even in small concentrations. The average error of the determination of 5-100 mg of bismuth (when titrated with 0.05M EDTA solution) is +/-0-1 % rel. and for the determination of 0.5-10 mg it is +/-0.3% rel. (0.005M EDTA). The method has been verified by the analysis of a Wood's metal of known composition.

  17. 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.

  18. 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

  19. 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...

  20. 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

  1. Corrosion behaviour of hot dip zinc and zinc–aluminium coatings on ...

    Indian Academy of Sciences (India)

    Zn–Al) alloy coatings started in the 1960s, although galvanized steels ... water. The galvanic current was measured using zero- resistance amperometry. The saturated calomel electrode. (SCE) and the platinum electrode were used as ...

  2. 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

  3. Nanoporous Ag template from partially sintered Ag–Zn compact by ...

    Indian Academy of Sciences (India)

    Administrator

    different dissolution methods, namely, simple immersion for 45 days and electrochemical way (holding the sample at critical potential), are employed. Electrochemical polarization tests are carried out to determine the critical potential for subsequent chrono-amperometry. X-ray diffraction, optical microscopy, scanning.

  4. 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)

  5. 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)

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

    NARCIS (Netherlands)

    Westerink, R.H.S.; Vijverberg, H.P.M.

    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. Composite Solid Electrodes - Tool for Organic Electrochemistry

    Czech Academy of Sciences Publication Activity Database

    Navrátil, Tomáš

    2011-01-01

    Roč. 15, č. 17 (2011), s. 2996-3013 ISSN 1385-2728 R&D Projects: GA AV ČR IAA400400806; GA ČR GAP206/11/1638 Institutional research plan: CEZ:AV0Z40400503 Keywords : amperometry * composite solid electrodes * polarography Subject RIV: CG - Electrochemistry Impact factor: 3.064, year: 2011

  8. 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

  9. 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

  10. 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

  11. 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

  12. 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 ...

  13. Electrochemistry of surface wired cytochrome c and ...

    Indian Academy of Sciences (India)

    Mixed self-assembled monolayer; pyrazine; cytochrome c; superoxide sensing; amperometry. 1. Introduction. Superoxide (O. −. 2 ) is one of the reactive oxygen species produced in vivo, involved in various physiological and pathological procedures.1–3 Superoxide is implicated in the pathology of many human diseases.

  14. 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

  15. 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...

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

    OpenAIRE

    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 eval...

  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

    In this paper, we present techniques to trap a group of neuronal cells (PC 12) close to band microelectrodes and quantitatively measure cellular transmitter release. Different trapping approaches were investigated including coating of electrodes by layers enhancing cell attachment and by pressure...... 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. Electrochemical Behavior and Determination of Rutin on Modified Carbon Paste Electrodes

    OpenAIRE

    Macikova, Pavla; Halouzka, Vladimir; Hrbac, Jan; Bartak, Petr; Skopalova, Jana

    2012-01-01

    The performances of ionic liquid (1-hexyl-3-methylimidazolium-bis(trifluoromethylsulfonyl)imide, IL/CPE) and iron phthalocyanine (IP/CPE) modified carbon paste electrodes in electroanalytical determinations of rutin were evaluated and compared to the performance of unmodified carbon paste electrode (CPE). Cyclic voltammetry (CV), differential pulse voltammetry (DPV), differential pulse adsorptive stripping voltammetry (DPAdSV), and amperometry were used for rutin analysis. The best current re...

  19. 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.

  20. 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

  1. 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.

  2. 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)

  3. Development of intraoperative electrochemical detection: wireless instantaneous neurochemical concentration sensor for deep brain stimulation feedback.

    Science.gov (United States)

    Van Gompel, Jamie J; Chang, Su-Youne; Goerss, Stephan J; Kim, In Yong; Kimble, Christopher; Bennet, Kevin E; Lee, Kendall H

    2010-08-01

    Deep brain stimulation (DBS) is effective when there appears to be a distortion in the complex neurochemical circuitry of the brain. Currently, the mechanism of DBS is incompletely understood; however, it has been hypothesized that DBS evokes release of neurochemicals. Well-established chemical detection systems such as microdialysis and mass spectrometry are impractical if one is assessing changes that are happening on a second-to-second time scale or for chronically used implanted recordings, as would be required for DBS feedback. Electrochemical detection techniques such as fast-scan cyclic voltammetry (FSCV) and amperometry have until recently remained in the realm of basic science; however, it is enticing to apply these powerful recording technologies to clinical and translational applications. The Wireless Instantaneous Neurochemical Concentration Sensor (WINCS) currently is a research device designed for human use capable of in vivo FSCV and amperometry, sampling at subsecond time resolution. In this paper, the authors review recent advances in this electrochemical application to DBS technologies. The WINCS can detect dopamine, adenosine, and serotonin by FSCV. For example, FSCV is capable of detecting dopamine in the caudate evoked by stimulation of the subthalamic nucleus/substantia nigra in pig and rat models of DBS. It is further capable of detecting dopamine by amperometry and, when used with enzyme linked sensors, both glutamate and adenosine. In conclusion, WINCS is a highly versatile instrument that allows near real-time (millisecond) detection of neurochemicals important to DBS research. In the future, the neurochemical changes detected using WINCS may be important as surrogate markers for proper DBS placement as well as the sensor component for a "smart" DBS system with electrochemical feedback that allows automatic modulation of stimulation parameters. Current work is under way to establish WINCS use in humans.

  4. 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 ...

  5. Fabrication of Functionalized Carbon Nanotube Buckypaper Electrodes for Application in Glucose Biosensors

    Directory of Open Access Journals (Sweden)

    Henry Papa

    2014-11-01

    Full Text Available A highly sensitive glucose detection method was developed using functionalized carbon nanotube buckypaper as a free standing electrode in an electrochemical biosensor. Glucose oxidase was immobilized onto various buckypaper samples in order to oxidize glucose resulting in a measureable current/voltage signal output of the biosensor. Cyclic voltammetry (CV and amperometry were utilized to determine the sensitivity of these buckypaper electrodes. Sensors of three different types of buckypaper were prepared and compared. These modified buckypaper electrode-based sensors showed much higher sensitivity to glucose compared to other electrochemical glucose sensors.

  6. Acetylcholinesterase Immobilized on Magnetic Beads for Pesticides Detection: Application to Olive Oil Analysis

    Directory of Open Access Journals (Sweden)

    Ihya Ait-Ichou

    2012-06-01

    Full Text Available This work presents the development of bioassays and biosensors for the detection of insecticides widely used in the treatment of olive trees. The systems are based on the covalent immobilisation of acetylcholinesterase on magnetic microbeads using either colorimetry or amperometry as detection technique. The magnetic beads were immobilised on screen-printed electrodes or microtitration plates and tested using standard solutions and real samples. The developed devices showed good analytical performances with limits of detection much lower than the maximum residue limit tolerated by international regulations, as well as a good reproducibility and stability.

  7. Quality control of PET labeled agents by TLC, GC and HPLC

    International Nuclear Information System (INIS)

    Dietzel, G.

    2003-01-01

    Radioactive nuclides emitting β + -radiation are used for labeling in PET diagnostic. Before the radioactive labeled agent can be used, the radiochemical purity has to be determined by means of two separate radio-chromatography methods. For HPLC, TLC, GC and CE special radioactivity detectors sensitive for β + -radiation are required, which fulfil the regulations of various international and national authorities. All conventional chromatography detectors in applications of HPLC, TLC, GC and CE like UV-absorption, fluorescence, reflective index, conductivity, amperometry etc. have an analog signal output 0-1 V. Therefore all signal recording and peak integration systems for chromatography have analog inputs of 0-1 V. (author)

  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. [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.

  10. 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.

  11. 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.

  12. 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.

  13. Pulse electrodeposited nickel-indium tin oxide nanocomposite as an electrocatalyst for non-enzymatic glucose sensing

    Energy Technology Data Exchange (ETDEWEB)

    Sivasakthi, P.; Ramesh Bapu, G.N.K., E-mail: rameshbapugnk@cecri.res.in; Chandrasekaran, Maruthai

    2016-01-01

    Nickel and nickel-ITO nanocomposite on mild steel substrate were prepared by pulse electrodeposition method from nickel sulphamate electrolyte and were examined as electrocatalysts for non-enzymatic glucose sensing. The surface morphology, chemical composition, preferred orientation and oxidation states of the nickel metal ion in the deposits were characterized by SEM, EDAX, XRD and XPS. Electrochemical sensing of glucose was studied by cyclic voltammetry and amperometry. The modified Ni-ITO nanocomposite electrode showed higher electrocatalytic activity for the oxidation of glucose in alkaline medium and exhibited a linear range from 0.02 to 3.00 mM with a limit of detection 3.74 μM at a signal-to-noise ratio of 3. The higher selectivity, longer stability and better reproducibility of this electrode compared to nickel in the sensing of glucose are pointers for exploitation in practical clinical applications. - Highlights: • Ni-ITO nanocomposites are prepared by pulse electrocodeposition method from nickel sulphamate solutions. • Ni-ITO nanocomposites are characterized using SEM, EDAX, XRD and XPS. • Electrochemical characteristics of the Ni and Ni-ITO nanocomposite deposits are studied by CV and amperometry techniques. • Ni-ITO nanocomposite electrode could be used as sensing material for detection of glucose in practical condition.

  14. 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.

  15. 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.

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

    Science.gov (United States)

    Prabakaran, E; Pandian, K

    2015-01-01

    A simple and sensitive electrochemical method was developed to determine the concentration of Sudan I in chili powder based on silver nanoparticles decorated graphene oxide modified glassy carbon electrode (AgNPs@GO/GCE). The voltammetry behaviour of Sudan I on modified GCE was investigated in phosphate buffer medium (PBS) with various pH ranges and the electron transfer properties were studied. It is found that the AgNPs@GO/GCE can catalyse the reduction of azo group, -N=N- followed by electrochemical oxidation of (-)OH group present in Sudan I dye molecule. Quantitative detection of Sudan I present in food products was carried out by amperometry method in which reduction potential was fixed at -0.77 V vs. Ag/AgCl. The amperometry method showed an excellent performance with a sensitivity of 6.83 μA mM(-1) and a detection limit of 11.4 × 10(-7)ML(-1). A linear calibration graph was constructed in the ranging 3.90 × 10(-6) to 3.19 × 10(-5)ML(-1). The method was successfully applied for the determination of Sudan I in red chili powder samples. Copyright © 2014 Elsevier Ltd. All rights reserved.

  17. Electrochemical Determination of Pentachlorophenol in Water on a Multi-Wall Carbon Nanotubes-Epoxy Composite Electrode

    Science.gov (United States)

    Remes, Adriana; Pop, Aniela; Manea, Florica; Baciu, Anamaria; Picken, Stephen J.; Schoonman, Joop

    2012-01-01

    The aim of this study was the preparation, characterization, and application of a multi-wall carbon nanotubes-epoxy composite electrode (MWCNT-EP) with 25%, wt. MWCNTs loading for the voltammetric/amperometric determination of pentachlorophenol (PCP) in aqueous solutions. The structural and morphological aspects of the MWCNT-EP composite electrode were examined by scanning electron microscopy. The electrical properties were characterized by direct-current conductivity measurements in relation with the percolation threshold. The electrochemical behavior of PCP at the MWCNT-EP composite electrode was investigated using cyclic voltammetry in 0.1 M Na2SO4 supporting electrolyte in order to establish the parameters for amperometric/voltammetric determination of PCP. The linear dependence of current vs. PCP concentrations was reached in a wide concentration range from 0.2 to 12 μM PCP using cyclic voltammetry, differential-pulsed voltammetry, square-wave voltammetry, chronoamperometry, and multiple-pulsed amperometry techniques. The best electroanalytical performances of this composite electrode were achieved using a pre-concentration/square-wave voltammetric technique and also multiple-pulsed amperometry techniques envisaging the practical applications. The ease of preparation, high sensitivity, and stability of this composite electrode should open novel avenues and applications for fabricating robust sensors for detection of many important species. PMID:22969335

  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. 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)

  20. Electrochemical Analysis of Neurotransmitters

    Science.gov (United States)

    Bucher, Elizabeth S.; Wightman, R. Mark

    2016-01-01

    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. PMID:25939038

  1. High Performance Non-enzymatic Glucose Sensor Based on One-Step Electrodeposited Nickel Sulfide.

    Science.gov (United States)

    Kannan, Padmanathan Karthick; Rout, Chandra Sekhar

    2015-06-22

    Nanostructured NiS thin film was prepared by a one-step electrodeposition method and the structural, morphological characteristics of the as-prepared films were analyzed by X-ray diffractometry (XRD), field emission scanning electron microscopy (FESEM) and energy dispersive X-ray analysis (EDAX). The electrocatalytic activity of NiS thin film towards glucose oxidation was investigated by fabricating a non-enzymatic glucose sensor and the sensor performance was studied by cyclic voltammetry (CV) and amperometry. The fabricated sensor showed excellent sensitivity and low detection limit with values of 7.43 μA μM(-1)  cm(-2) and 0.32 μM, respectively, and a response time of <8 s. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  2. Investigation of amperometric detection of phosphate Application in seawater and cyanobacterial biofilm samples.

    Science.gov (United States)

    Quintana, Josefina Calvo; Idrissi, Laila; Palleschi, Giuseppe; Albertano, Patrizia; Amine, Aziz; El Rhazi, Mama; Moscone, Danila

    2004-06-17

    Detection of phosphate using amperometry was investigated. The phosphomolybdate complex, formed by addition of nitric acid, ammonium molybdate and phosphate, was reduced at a carbon paste electrode polarised at +0.3V (versus Ag/AgCl). The major characteristics observed were simplicity of the equipment, a limited consumption of reagents and a low detection limit (0.3mumoll(-1)), with a linear range between 1 and 20mumoll(-1). The interference of silicate was completely eliminated using an appropriate concentration of nitric acid and ammonium molybdate. The amperometric detection of orthophosphate in seawater using the batch injection analysis (BIA) technique was reported. Moreover, a carbon paste microelectrode was constructed. Its use allows the analysis of small volume of samples with little dilution in supporting electrolyte. This method was applied to the determination of orthophosphate in cyanobacterial biofilms collected from Roman catacombs. There was a good statistical correlation between results obtained with the proposed method and the standard spectrophotometric method.

  3. 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...

  4. 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)

  5. 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.

  6. The use of microorganisms with broad range substrate utilisation for the ferricyanide-mediated rapid determination of biochemical oxygen demand.

    Science.gov (United States)

    Catterall, K; Morris, K; Gladman, C; Zhao, H; Pasco, N; John, R

    2001-12-24

    The feasibility of replacing oxygen with a synthetic electron acceptor in microbial catabolism was investigated as a rapid method for the determination of biochemical oxygen demand (BOD). Microorganisms known for their broad range organic substrate utilisation were investigated. It was shown that Trichosporon cutaneum, Pseudomonas putida and Bacillus licheniformis could utilize the ferricyanide ion as an alternative electron acceptor, in place of oxygen, for the catabolic oxidation of a range of simple organic compounds. The biochemical reactions were monitored by measuring the amount of microbially produced ferrocyanide using amperometry at a Pt disk microelectrode. Catabolic degradation efficiencies approaching those of the conventional 5-day assay were achieved in 1 h. BOD(5) equivalent values for a range of simple organic solutions were determined for each of the microorganisms. The effect of increased incubation time and the choice of appropriate calibration standards for rapid BOD assays were also considered.

  7. 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)

  8. Electrochemical Dynamics of a Single Platinum Nanoparticle Collision Event for the Hydrogen Evolution Reaction.

    Science.gov (United States)

    Xiang, Zhi-Peng; Deng, Hai-Qiang; Peljo, Pekka; Fu, Zhi-Yong; Wang, Su-Li; Mandler, Daniel; Sun, Gong-Quan; Liang, Zhen-Xing

    2018-03-19

    Chronoamperometry was used to study the dynamics of Pt nanoparticle (NP) collision with an inert ultramicroelectrode via electrocatalytic amplification (ECA) in the hydrogen evolution reaction. ECA and dynamic light scattering (DLS) results reveal that the NP colloid remains stable only at low proton concentrations (1.0 mm) under a helium (He) atmosphere, ensuring that the collision events occur at genuinely single NP level. Amperometry of single NP collisions under a He atmosphere shows that each discrete current profile of the collision event evolves from spike to staircase at more negative potentials, while a staircase response is observed at all of the applied potentials under hydrogen-containing atmospheres. The particle size distribution estimated from the diffusion-controlled current in He agrees well with electron microscopy and DLS observations. These results shed light on the interfacial dynamics of the single nanoparticle collision electrochemistry. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. 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.

  10. Amperometric Detection of Bacillus anthracis Spores: A Portable, Low-Cost Approach to the ELISA

    Directory of Open Access Journals (Sweden)

    Gabriel D. Peckham

    2013-01-01

    Full Text Available Antibody-based detection assays are generally robust, a desirable characteristic for in-the-field use. However, to quantify the colorimetric or fluorescent signal, these assays require expensive and fragile instruments which are ill-suited to in-the-field use. Lateral flow devices (LFDs circumvent these barriers to portability but suffer from poor sensitivity and subjective interpretation. Here, an antibody-based method for detecting Bacillus anthracis spores via amperometric signal generation is compared to ELISA and LFDs. This amperometric immunoassay uses antibody conjugated to magnetic beads and glucose oxidase (GOX along with the electron mediator 2, 6-dichlorophenolindophenol (DCPIP for production of a measurable current from a 0.4 V bias voltage. With similar sensitivity to ELISA, the assay can be completed in about 75 minutes while being completely powered and operated from a laptop computer. Immunoassay amperometry holds promise for bringing low-cost, quantitative detection of hazardous agents to the field.

  11. Facile synthesis of hierarchically mesoporous NiCo2O4 nanowires for sensitive nonenzymatic glucose detection

    Science.gov (United States)

    Qin, Zhenhua; Cheng, Qunpeng; Lu, Yao; Li, Jianfen

    2017-07-01

    Glucose nonenzymatic detection is of significance in the fields of biological, environmental, food monitoring, and clinical analysis. By employing mesoporous NiCo2O4 nanowires as electrochemical sensor, highly sensitive nonenzymatic detection of glucose has been realized. The NiCo2O4 nanowires were synthesized via a facile hydrothermal method and subsequent thermal treatment. Their crystalline structures were analyzed by X-ray diffraction, and morphologies were characterized using scanning electron microscopy and transmission electron microscopy. The porous characteristics and real surface areas of the synthesized NiCo2O4 were studied by Brunauer-Emmett-Teller method. Electro-catalytic oxidation of glucose on the NiCo2O4 electrode was investigated by cyclic voltammetry, linear sweep voltammetry, and amperometry. The nonenzymatic sensor based on NiCo2O4 exhibited superior performance for glucose detection, with a low detection limit and excellent sensitivity.

  12. Tehnici de analiză privind influenţa utilizării armăturii zincate termic asupra durabilităţii betonului armat

    Directory of Open Access Journals (Sweden)

    Carmen Dico

    2010-12-01

    Full Text Available The paper briefly presents the results of experimental research on the influence of using zinc hot dip galvanized rebar on the durability of reinforced concrete. For this purpose, the loss of adherence between the rebar and the concrete matrix was determined, as well as the reduction of resistance to splitting due to accelerated corrosion of samples of hot dip galvanized rebar vs. steel not protected against corrosion. Using electrochemical analysis techniques (chrono-amperometry, linear polarization, electrochemical impedance spectroscopy the kinetics and mechanism of the corrosion of the rebar in the reinforced concrete due to the action of chlorine ions was studied. The results prove a lower speed and better resistance to corrosion of yinc hot dip galvanized rebar, leading to an increased lifetime of reinforced concrete structures.

  13. 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.

  14. Amperometric noise at thin film band electrodes.

    Science.gov (United States)

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

    2012-09-18

    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 polymers and measured the current noise in physiological buffer solution for a wide range of different electrode areas. The noise measurements could be modeled by an analytical expression, representing the electrochemical cell as a resistor and capacitor in series. The studies revealed three domains; for electrodes with low capacitance, the amplifier noise dominated, for electrodes with large capacitances, the noise from the resistance of the electrochemical cell was dominant, while in the intermediate region, the current noise scaled with electrode capacitance. The experimental results and the model presented here can be used for choosing an electrode material and dimensions and when designing chip-based devices for low-noise current measurements.

  15. 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.

  16. 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.

  17. 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

  18. 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.

  19. 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-time......’s disease. (4) The combination of amperometry, EIS monitoring and microscopic visualization in microfluidics assays for real-time multi-parameter analysis on the same cell population. The research carried out in this thesis branches out from the context of the EU-funded FP7 project EXCELL (Exploring...... Cellular Dynamics at Nanoscale) aimed at developing innovative systems for the investigation of real time cellular dynamics. The main focus of the EXCELL project was related to the development of a multi-parameter microfluidic cell culture and detection platform, combining electrochemical and optical...

  20. Analysis of inorganic sulphur compounds by means of ion chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Weiss, J.; Goebl, M.

    1985-03-01

    Ionic inorganic sulphur compounds can be separated and determined by ion-chromatographic techniques. In aqueous solution the species of interest mostly exist as anions. Separation techniques include both ion exchange and ion-pair chromatography. The stationary phases are latexed anion exchangers based on polystyrene/divinylbenzene as well as neutral resins of an unpolar character. The most widely used detection system is the conductometric detector. The high background conductivity of the eluent is eliminated by the use of a suppressor device. Sulphide is detected by amperometry due to the high pK-value of the corresponding acid formed in the suppressor. Amperometric detection can also be employed for detection of other sulphur containing species like thiocyanate and thiosulphate in a complex matrix. Detection limits for the species investigated are in the lowest ppb region.

  1. 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.

  2. Effect of the scan rate on the kinetic parameters of active dissolution and passivation of iron in a neutral solution

    International Nuclear Information System (INIS)

    Garmanov, M.E.; Kuznetsov, Yu.I.

    2004-01-01

    The effect of polarization rate (V = 0.2-100 mV/s) of a rotating disk-like electrode (with rotation rate v = 6000 rot/min) on kinetics of active anodic dissolution and active-passive transition of Armco iron in deaerated borate duffer solution with 7.40 pH is studied by the method of cyclic volt-amperometry. It is shown that in the whole V range studied without diffusion limitations the rate of active dissolution and formation of a primary passivating film is determined by slow electrochemical stages of electron transport, and a cyclic volt-ampere curve is a nonstationary thermodynamically nonequilibrium one. A linear growth of current at anodic maximum and a positive shift of its potential with a lg V increase are observed [ru

  3. 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.

  4. Surface coverage dictates the surface bio-activity of D-amino acid oxidase.

    Science.gov (United States)

    Herrera, Elisa; Giacomelli, Carla E

    2014-05-01

    This work presents a systematic study on the relationship between the adsorption mechanism and the surface bio-activity of D-amino acid oxidase (pkDAAO). This rational approach is based on measuring the characteristic filling and relaxation times under different experimental conditions. With such a goal, real-time adsorption-desorption experiments at different degrees of surface coverage were performed tuning the electrostatic and hydrophobic interactions by changing the pH condition for the adsorption and the substrate properties (silica or gold). Surface bio-activity was measured in situ by amperometry using the bio-functional surface as the working electrode and ex situ by spectrophotometry. On both solid substrates, pkDAAO adsorption is a transport-controlled process, even under unfavorable electrostatic interactions (charged protein and substrate with the same sign) due to the high percentage of basic amino acids in the enzyme. On silica, the relaxation step is electrostatic in nature and occurs in the same time-scale as filling the surface when the substrate and the enzyme are oppositely charged at low surface coverage. Under unfavorable electrostatic conditions, the relaxation (if any) occurs at long time. Accordingly, the bio-activity of the native pkDAAO is preserved at any surface coverage. On gold, this step is driven by hydrophobic interactions (pH-independent) and the surface bio-activity is highly dependent on the degree of surface coverage. Under these conditions, the surface bio-activity is preserved only at high surfaces coverage. Our results clearly indicate that pkDAAO bio-functionalized surfaces cannot be coupled to amperometry because the analyte interferes the electrochemical signal. However, this simple bio-functionalized strategy can be joined to other detection methods. Copyright © 2014 Elsevier B.V. All rights reserved.

  5. 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)

  6. Extracellular Osmotic Stress Reduces the Vesicle Size while Keeping a Constant Neurotransmitter Concentration.

    Science.gov (United States)

    Fathali, Hoda; Dunevall, Johan; Majdi, Soodabeh; Cans, Ann-Sofie

    2017-02-15

    Secretory cells respond to hypertonic stress by cell shrinking, which causes a reduction in exocytosis activity and the amount of signaling molecules released from single exocytosis events. These changes in exocytosis have been suggested to result from alterations in biophysical properties of cell cytoplasm and plasma membrane, based on the assumption that osmotic stress does not affect the secretory vesicle content and size prior to exocytosis. To further investigate whether vesicles in secretory cells are affected by the osmolality of the extracellular environment, we used intracellular electrochemical cytometry together with transmission electron microscopy imaging to quantify and determine the catecholamine concentration of dense core vesicles in situ before and after cell exposure to osmotic stress. In addition, single cell amperometry recordings of exocytosis at chromaffin cells were used to monitor the effect on exocytosis activity and quantal release when cells were exposed to osmotic stress. Here we show that hypertonic stress hampers exocytosis secretion after the first pool of readily releasable vesicles have been fused and that extracellular osmotic stress causes catecholamine filled vesicles to shrink, mainly by reducing the volume of the halo solution surrounding the protein matrix in dense core vesicles. In addition, the vesicles demonstrate the ability to perform adjustments in neurotransmitter content during shrinking, and intracellular amperometry measurements in situ suggest that vesicles reduce the catecholamine content to maintain a constant concentration within the vesicle compartment. Hence, the secretory vesicles in the cell cytoplasm are highly affected and respond to extracellular osmotic stress, which gives a new perspective to the cause of reduction in quantal size by these vesicles when undergoing exocytosis.

  7. 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

  8. 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)

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

    International Nuclear Information System (INIS)

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

    2016-01-01

    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 2 O 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 −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 2 O 2 with R 2 of 0.9977. • Nanocomposite shows

  10. Development of Microelectrode Arrays Using Electroless Plating for CMOS-Based Direct Counting of Bacterial and HeLa Cells.

    Science.gov (United States)

    Niitsu, Kiichi; Ota, Shoko; Gamo, Kohei; Kondo, Hiroki; Hori, Masaru; Nakazato, Kazuo

    2015-10-01

    The development of two new types of high-density, electroless plated microelectrode arrays for CMOS-based high-sensitivity direct bacteria and HeLa cell counting are presented. For emerging high-sensitivity direct pathogen counting, two technical challenges must be addressed. One is the formation of a bacteria-sized microelectrode, and the other is the development of a high-sensitivity and high-speed amperometry circuit. The requirement for microelectrode formation is that the gold microelectrodes are required to be as small as the target cell. By improving a self-aligned electroless plating technique, the dimensions of the microelectrodes on a CMOS sensor chip in this work were successfully reduced to 1.2 μm × 2.05 μm. This is 1/20th of the smallest size reported in the literature. Since a bacteria-sized microelectrode has a severe limitation on the current flow, the amperometry circuit has to have a high sensitivity and high speed with low noise. In this work, a current buffer was inserted to mitigate the potential fluctuation. Three test chips were fabricated using a 0.6- μm CMOS process: two with 1.2 μm × 2.05 μm (1024 × 1024 and 4 × 4) sensor arrays and one with 6- μm square (16 × 16) sensor arrays; and the microelectrodes were formed on them using electroless plating. The uniformity among the 1024 × 1024 electrodes arranged with a pitch of 3.6 μm × 4.45 μm was optically verified. For improving sensitivity, the trenches on each microelectrode were developed and verified optically and electrochemically for the first time. Higher sensitivity can be achieved by introducing a trench structure than by using a conventional microelectrode formed by contact photolithography. Cyclic voltammetry (CV) measurements obtained using the 1.2 μm × 2.05 μm 4 × 4 and 6- μm square 16 × 16 sensor array with electroless-plated microelectrodes successfully demonstrated direct counting of the bacteria-sized microbeads and HeLa cells.

  11. 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.

  12. 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)

  13. 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.

  14. 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 2 O/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)

  15. 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.

  16. Combination of laccase and catalase in construction of H2O2-O2 based biocathode for applications in glucose biofuel cells.

    Science.gov (United States)

    Ammam, Malika; Fransaer, Jan

    2013-01-15

    In this study, we propose a new strategy to boost the power density of glucose biofuel cells (GBFCs) biocathodes. By combining laccase with catalase enzymes electrophoretically deposited by means of AC electric fields on multiple walled carbon nanotubes modified platinum black and, then stabilized by an outer layer of polypyrrole in the construction of GC/MWCNTs/Ptb/LAc-CAt/PPy biocathode, we can take advantage of the H(2)O(2) present in the solution or body tissue to increase the level of the dissolved O(2). The results from cyclic voltammetry, amperometry and electrochemical impedance spectroscopy demonstrate that the deposited enzymes laccase and catalase by means of AC-EPD did not inhibit each other and carry out ∼90% of the catalytic reduction process of O(2)-H(2)O(2). The power density of the non-compartmentalized GBFC constructed from GC/MWCNTs/Ptb/LAc-CAt/PPy biocathode and GC/MWCNTs/GOx/PPy bioanode in phosphate buffer containing 10mM glucose and equal amounts of dissolved O(2) and H(2)O(2) (0.3mM) is almost doubled because of the presence of catalase enzyme in the constructed biocathode. The latter might be of great interest for in vivo studies of GBFCs where the concentration of dissolved O(2) in the body tissues or biological fluids is very low compared to in vitro conditions (buffers under air). Copyright © 2012 Elsevier B.V. All rights reserved.

  17. 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.

  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. 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.

  20. Phosphate determination in seawater: toward an autonomous electrochemical method.

    Science.gov (United States)

    Jońca, Justyna; León Fernández, Violeta; Thouron, Danièle; Paulmier, Aurélien; Graco, Michelle; Garçon, Véronique

    2011-12-15

    Initial steps to create an autonomous in situ electrochemical sensor for orthophosphate determination in seawater are presented. First, the optimal conditions to form the molybdophosphate complex in artificial seawater medium were determined by addition of sulphuric acid and sodium molybdate to the solution containing orthophosphate. Secondly, the anodic oxidation of molybdenum to form molybdate ions and protons was used to create the molybdophosphate complex without addition of any liquid reagents. The molybdophosphate complex is detectable by amperometry with an average precision of 2.2% for the concentration range found in the open ocean and the detection limit is 0.12 μM. Three solutions are proposed to address the silicate interferences issue and one of these methods is used for the natural samples collected in the coastal waters offshore Peru during the Pelagico 1011-12-BIC OLAYA cruise in November-December 2010. Results showed a good precision with an average of 2.5% and a reasonable deviation of the amperometric analysis as compared with colorimetric measurements (4.9%). Copyright © 2011 Elsevier B.V. All rights reserved.

  1. 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).

  2. 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.

  3. Highly sensitive and selective electrochemical detection of sub-ppb level chromium(VI) using nano-sized gold particle.

    Science.gov (United States)

    Jena, Bikash Kumar; Raj, C Retna

    2008-06-30

    Gold nanoparticle based nanostructured electrode has been developed for the amperometric detection of ultratrace amount of toxic Cr(VI). The nano-sized Au particles have been grown on a conducting substrate modified with sol-gel-derived thiol functionalized silicate network and used for the electroanalysis of Cr(VI). The nanostructured interface show well-defined voltammetric peak for the reduction of Cr(VI) at approximately 0.4 V. The voltammetric behavior of Cr(VI) strongly depends on the coverage of nanoparticle on the electrode surface. Constant potential amperometry has been used for the detection of Cr(VI) at well below the guideline value set by World Health Organization (WHO). This electrode is highly sensitive (30+/-0.2 nA/ppb) and the detection limit (S/N=9) was 0.1 ppb. Cr(III) and coexisting other metal ions and surface active agent present in water do not interfere with the amperometric measurement of Cr(VI). This nanostructured electrode is highly stable and it can be used for continuous measurement of Cr(VI) without using any pretreatment or activation procedures. The accuracy of the measurement has been validated by measuring the concentration of Cr(VI) in the certified reference material (CRM).

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

    Science.gov (United States)

    Thuy, Tran Nguyen Thanh; Tseng, Tina T-C

    2016-05-26

    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.

  5. 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.

  6. 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.

  7. 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.

  8. 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

  9. Yeast-based Biochemical Oxygen Demand Sensors Using Gold-modified Boron-doped Diamond Electrodes.

    Science.gov (United States)

    Ivandini, Tribidasari A; Harmesa; Saepudin, Endang; Einaga, Yasuaki

    2015-01-01

    A gold nanoparticle modified boron-doped diamond electrode was developed as a transducer for biochemical oxygen demand (BOD) measurements. Rhodotorula mucilaginosa UICC Y-181 was immobilized in a sodium alginate matrix, and used as a biosensing agent. Cyclic voltammetry was applied to study the oxygen reduction reaction at the electrode, while amperometry was employed to detect oxygen, which was not consumed by the microorganisms. The optimum waiting time of 25 min was observed using 1-mm thickness of yeast film. A comparison against the system with free yeast cells shows less sensitivity of the current responses with a linear dynamic range (R(2) = 0.99) of from 0.10 mM to 0.90 mM glucose (equivalent to 10 - 90 mg/L BOD) with an estimated limit of detection of 1.90 mg/L BOD. However, a better stability of the current responses could be achieved with an RSD of 3.35%. Moreover, less influence from the presence of copper ions was observed. The results indicate that the yeast-immobilized BOD sensors is more suitable to be applied in a real condition.

  10. Facile fabrication of 3D layer-by-layer graphene-gold nanorod hybrid architecture for hydrogen peroxide based electrochemical biosensor

    Directory of Open Access Journals (Sweden)

    Chenming Xue

    2015-03-01

    Full Text Available Three-dimensional (3D layer-by-layer graphene-gold nanorod (GNR architecture has been constructed. The resulting hybrid nanomaterials’ architecture has been tested for detecting hydrogen peroxide (H2O2 through the electrocatalytic reaction on a three electrode disposable biosensor platform. Cyclic voltammetry and amperometry were used to characterize and assess the performance of the biosensor. The 3D layer-by-layer modified electrode exhibited the highest sensitivity compared to the active carbon, graphene-oxide, cysteine-graphene oxide and GNR coated electrodes. This research explored the feasibility of using the 3D hybrid graphene-GNR as a template for biosensor. The 3D hybrid structure exhibited higher sensitivity than GNRs alone. SEM showed the explanation that GNRs had self-aggregates reducing the contact surface area when coated on the active carbon electrode, while there were no such aggregates in the 3D structure, and TEM illustrated that GNRs dispersed well in the 3D structure. This research demonstrated a better way to prepare well-separated metal nanoparticles by using the 3D layer-by-layer structure. Consequently, other single and bi-metallic metal nanoparticles could be incorporated into such structure. As a practical example, 3D layer-by-layer nanomaterials modified active carbon electrode was used for detecting glucose showing very good sensitivity and minimum interference by ascorbic acid and uric acid in test solution, which indicated a good selectivity of the biosensor as well.

  11. Investigation of the interaction between Tc85-11 protein and antibody anti-T. cruzi by AFM and amperometric measurements

    Energy Technology Data Exchange (ETDEWEB)

    Ferreira, A.A.P. [UNESP, Institute of Chemistry, CP 355, 14801-970 Araraquara, SP (Brazil); Colli, W. [USP, Institute of Chemistry, Av. Prof. Lineu Prestes 748, 05508-900 Sao Paulo, SP (Brazil); Alves, M.J.M. [USP, Institute of Chemistry, Av. Prof. Lineu Prestes 748, 05508-900 Sao Paulo, SP (Brazil); Oliveira, D.R. [USP, Institute of Chemistry, Av. Prof. Lineu Prestes 748, 05508-900 Sao Paulo, SP (Brazil); Costa, P.I. [UNESP, Faculty of Pharmaceutical Sciences, Rodovia Araraquara/Jau Km 1, 14801-902 Araraquara, SP (Brazil); Gueell, A.G. [CBEN, University of Barcelona, Scientific Park of Barcelona, C/ Josep Samitier 1-5, 08028 Barcelona (Spain); Sanz, F. [CBEN, University of Barcelona, Scientific Park of Barcelona, C/ Josep Samitier 1-5, 08028 Barcelona (Spain); Benedetti, A.V. [UNESP, Institute of Chemistry, CP 355, 14801-970 Araraquara, SP (Brazil); Yamanaka, H. [UNESP, Institute of Chemistry, CP 355, 14801-970 Araraquara, SP (Brazil)]. E-mail: hidekoy@iq.unesp.br

    2006-07-15

    This present work reports on development of an amperometric immunosensor for the diagnosis of Chagas' disease using a specific glycoprotein of the trypomastigote surface, which belongs to the Tc85-11 protein family of Trypanosoma cruzi (T. cruzi). An atomically flat gold surface on a silicon substrate and gold screen-printed electrodes were functionalized with cystamine and later activated with glutaraldehyde (GA), which was used to form covalent bonds with the purified recombinant antigen (Tc85-11). The antigen reacts with the antibody from the serum, and the affinity reaction was monitored directly using atomic force microscopy or amperometry through a secondary antibody tagged to peroxidase (HRP). Surface imaging allowed to us to differentiate the modification steps and antigen-antibody interaction allowed to distinguish the affinity reactions. In the amperometric immunosensor, peroxidase catalyses the L{sub 2} formation in the presence of hydrogen peroxide and potassium iodide, and the reduction current intensity was measured at a given potential with screen-printed electrodes. The immunosensor was applied to sera of chagasic patients and patients having different systemic diseases.

  12. 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)

  13. More Transparency in BioAnalysis of Exocytosis: Coupling of Electrochemistry and Fluorescence Microscopy at ITO Electrodes

    Directory of Open Access Journals (Sweden)

    Liu Xiaoqing

    2016-01-01

    Full Text Available Vesicular exocytosis is an essential biological mechanism used by cellular organisms to release bioactive molecules (hormones, neurotransmitters… in their environment. For instance, this is the pathway by which chromaffin cells deliver catecholamines (adrenaline, nor-adrenaline, dopamine… in blood. During this process, secretory vesicles that initially stored the (biochemical messengers dock to the cell membrane. The subsequent fusion of vesicle and cell membranes induces the formation of a fusion pore that initiates the first exchanges between the intravesicular and extracellular media. Its following expansion thus favours a larger release of the vesicular content into the external medium. Several analytical methods have been developed in order to study exocytosis at the single living cell level in real time. Among those techniques, mostly based on electric or optic measurements, amperometry with a carbon-fiber ultramicroelectrode [1], used in the first part of this report, and total internal reflection fluorescence microscopy (TIRFM appear as the most powerful [2] Practically, physico-chemical properties of ultramicroelectrodes induce a high detection sensitivity and temporal resolution, thus being particularly well adapted to monitor exocytosis of electroactive molecules in real time.

  14. 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.

  15. 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.

  16. 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.

  17. 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.

  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. Electrochemistry and current control in surface films based on silica-azure redox nanoparticles, carbon nanotubes, enzymes, and polyelectrolytes.

    Science.gov (United States)

    Karra, Sushma; Zhang, Maogen; Gorski, Waldemar

    2013-01-15

    The redox active nanoparticles were developed by covalently attaching redox dye Azure C (AZU) to commercial silica nanoparticles (SN) via the silylated amine and glutaric dialdehyde links. The SN-AZU nanoparticles were studied as redox mediators for the oxidation of reduced β-nicotinamide adenine dinucleotide (NADH) in two polymeric films. The first film (F1) was composed of SN-AZU, carbon nanotubes, and cationic polyelectrolyte chitosan. The second film (F2) contained also added enzyme glucose dehydrogenase and its cofactor β-nicotinamide adenine dinucleotide (NAD(+)). The films F1 and F2 were cast on the glassy carbon electrodes, covered with an anionic polyelectrolyte Nafion, and their electrochemical properties were probed with NADH and glucose, respectively, using voltammetry, amperometry, and potentiometry. The Nafion overcoat reduced the sensitivity of F1/Nafion film electrodes to NADH by >98%. In contrast, depending on the concentration of Nafion, the sensitivity of the F2/Nafion film electrodes (reagentless biosensors) to glucose increased by up to 340%. The amplification of glucose signal was ascribed to the Donnan exclusion and ensuing Nafion-gated ionic fluxes, which enhanced enzyme activity in films F2. The proposed model predicts that such signal amplification should be also feasible in the case of other enzyme-based biosensors.

  1. Electrochemical Behavior and Determination of Rutin on Modified Carbon Paste Electrodes

    Directory of Open Access Journals (Sweden)

    Pavla Macikova

    2012-01-01

    Full Text Available The performances of ionic liquid (1-hexyl-3-methylimidazolium-bis(trifluoromethylsulfonylimide, IL/CPE and iron phthalocyanine (IP/CPE modified carbon paste electrodes in electroanalytical determinations of rutin were evaluated and compared to the performance of unmodified carbon paste electrode (CPE. Cyclic voltammetry (CV, differential pulse voltammetry (DPV, differential pulse adsorptive stripping voltammetry (DPAdSV, and amperometry were used for rutin analysis. The best current responses of rutin were obtained at pH 4.0 for all tested techniques. IL/CPE electrode was found to perform best with DPAdSV technique, where a detection limit (LOD as low as 5 nmol L-1 of rutin was found. On the other hand, IP/CPE showed itself to be an optimum choice for DPV technique, where LOD of 80 nmol L-1 was obtained. Analytical applicability of newly prepared electrodes was demonstrated on determination of rutin in the model samples and the extracts of buckwheat seeds. To find an optimum method for buckwheat seeds extraction, a boiling water extraction (BWE, Soxhlet extraction (SE, pressurized solvent extraction (PSE, and supercritical fluid extraction (SFE were tested.

  2. Highly sensitive electrochemical determination of nitric oxide using fused spherical gold nanoparticles modified ITO electrode

    Energy Technology Data Exchange (ETDEWEB)

    Kannan, P. [Department of Chemistry, Gandhigram Rural University, Gandhigram 624 302, Dindigul, Tamil Nadu (India); John, S. Abraham, E-mail: abrajohn@yahoo.co.i [Department of Chemistry, Gandhigram Rural University, Gandhigram 624 302, Dindigul, Tamil Nadu (India)

    2010-04-01

    This paper describes the highly sensitive electrochemical determination of nitric oxide (NO) using the fused spherical gold nanoparticles (FAuNPs) modified ITO electrode. The FAuNPs were self-assembled on a (3-mercaptopropyl)-trimethoxysilane (MPTS) sol-gel film, which was preassembled on ITO electrode. The attachment of FAuNPs on MPTS sol-gel film was confirmed by UV-vis absorption spectroscopy, atomic force microscopy (AFM) and cyclic voltammetry (CV). The AFM image shows that the AuNPs retain their fused morphology after immobilized on MPTS sol-gel film. The FAuNPs modified ITO electrode shows an excellent electrocatalytic activity towards the oxidation of NO. Using FAuNPs modified electrode, the detection of 12 nM NO was achieved for the first time by amperometry method. Further, the current response was increased linearly with increasing NO concentration in the range of 1.2 x 10{sup -8} to 7 x 10{sup -4} M and the detection limit was found to be 3.1 x 10{sup -10} M (S/N = 3). The FAuNPs modified ITO electrode displays an excellent selectivity towards the determination of 12 nM NO even in the presence of 1000-fold excess common interfering agents.

  3. 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)

  4. 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

  5. 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

  6. 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

  7. Implementation of a new integrated d-lactic acid biosensor in a semiautomatic FIA system for the simultaneous determination of lactic acid enantiomers. Application to the analysis of beer samples.

    Science.gov (United States)

    Vargas, E; Ruiz, M A; Campuzano, S; González de Rivera, G; López-Colino, F; Reviejo, A J; Pingarrón, J M

    2016-05-15

    An integrated amperometric d-lactic acid biosensor involving a gold film deposited by sputtering on a stainless steel disk electrode where the enzymes D-lactic acid dehydrogenase (DLDH) and diaphorase (DP) as well as the redox mediator tetrathiafulvalene (TTF) are coimmobilized by using a dialysis membrane, is reported in this work. Amperometry in stirred solutions at a detection potential of +0.15 V (vs Ag/AgCl reference electrode) provided a linear calibration plot for D-lactic acid over the 1.0×10(-4) to 3.8×10(-3) g L(-1) concentration range, with a limit of detection of 3.1×10(-5) g L(-1). The usefulness of the biosensor was demonstrated by determining D-lactic acid in beer samples with good results. Additionally, the biosensor was implemented together with a commercial L-lactic amperometric biosensor in a semiautomatic flow-injection analysis (FIA) system able to perform a rapid and simple stereo-specific determination of D- and D-lactic without a previous separation step. The operational characteristics of the biosensors under flow conditions were evaluated and its applicability was demonstrated through the simultaneous determination of both enantiomers in beer samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  8. 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.

  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. 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.

  12. 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.

  13. 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.

  14. 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.

  15. 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)

  16. 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.

  17. 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.

  18. 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.

  19. 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.

  20. 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.

  1. 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).

  2. Detection of Nitric Oxide from Living Cells Using Polymeric Zinc Organic Framework-Derived Zinc Oxide Composite with Conducting Polymer.

    Science.gov (United States)

    Kim, Min-Yeong; Naveen, Malenahalli Halappa; Gurudatt, Nanjanagudu Ganesh; Shim, Yoon-Bo

    2017-07-01

    Sensitive and selective detection of nitric oxide (NO) in the human body is crucial since it has the vital roles in the physiological and pathological processes. This study reports a new type of electrochemical NO biosensor based on zinc-dithiooxamide framework derived porous ZnO nanoparticles and polyterthiophene-rGO composite. By taking advantage of the synergetic effect between ZnO and poly(TTBA-rGO) (TTBA = 3'-(p-benzoic acid)-2,2':5',2″-terthiophene, rGO = reduced graphene oxide) nanocomposite layer, the poly(TTBA-rGO)/ZnO sensor probe displays excellent electrocatalytic activity and explores to detect NO released from normal and cancer cell lines. The ZnO is immobilized on a composite layer of poly(TTBA-rGO). The highly porous ZnO offers a high electrolyte accessible surface area and high ion-electron transport rates that efficiently catalyze the NO reduction reaction. Amperometry with the modified electrode displays highly sensitive response and wide dynamic range of 0.019-76 × 10 -6 m with the detection limit of 7.7 ± 0.43 × 10 -9 m. The sensor probe is demonstrated to detect NO released from living cells by drug stimulation. The proposed sensor provides a powerful platform for the low detection limit that is feasible for real-time analysis of NO in a biological system. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. 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.

  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. Electrochemical detection of peroxynitrite using hemin-PEDOT functionalized boron-doped diamond microelectrode.

    Science.gov (United States)

    Peteu, Serban F; Whitman, Brandon W; Galligan, James J; Swain, Greg M

    2016-03-07

    Peroxynitrite is a potent nitroxidation agent and highly reactive metabolite, clinically correlated with a rich pathophysiology. Its sensitive and selective detection is challenging due to its high reactivity and short sub-second lifetime. Boron-doped diamond (BDD) microelectrodes have attracted interest because of their outstanding electroanalytical properties that include a wide working potential window and enhanced signal-to-noise ratio. Herein, we report on the modification of a BDD microelectrode with an electro-polymerized film of hemin and polyethylenedioxythiophene (PEDOT) for the purpose of selectively quantifying peroxynitrite. The nanostructured modified polymer layer was characterized by Raman spectroscopy and scanning electron microscopy (SEM). The electrochemical response to peroxynitrite was studied by voltammetry and time-based amperometry. The measured detection limit was 10 ± 0.5 nM (S/N = 3), the sensitivity was 4.5 ± 0.5 nA nM(-1) and the response time was 3.5 ± 1 s. The hemin-PEDOT BDD sensors exhibited a response variability of 5% or less (RSD). The stability of the sensors after a 20-day storage in 0.1 M PB (pH 7.4) at 4 °C was excellent as at least 93% of the initial response to 50 nM PON was maintained. The presence of PEDOT was correlated with a sensitivity increase.

  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. Electrochemical behavior and determination of rutin on modified carbon paste electrodes.

    Science.gov (United States)

    Macikova, Pavla; Halouzka, Vladimir; Hrbac, Jan; Bartak, Petr; Skopalova, Jana

    2012-01-01

    The performances of ionic liquid (1-hexyl-3-methylimidazolium-bis(trifluoromethylsulfonyl)imide, IL/CPE) and iron phthalocyanine (IP/CPE) modified carbon paste electrodes in electroanalytical determinations of rutin were evaluated and compared to the performance of unmodified carbon paste electrode (CPE). Cyclic voltammetry (CV), differential pulse voltammetry (DPV), differential pulse adsorptive stripping voltammetry (DPAdSV), and amperometry were used for rutin analysis. The best current responses of rutin were obtained at pH 4.0 for all tested techniques. IL/CPE electrode was found to perform best with DPAdSV technique, where a detection limit (LOD) as low as 5 nmol L(-1) of rutin was found. On the other hand, IP/CPE showed itself to be an optimum choice for DPV technique, where LOD of 80 nmol L(-1) was obtained. Analytical applicability of newly prepared electrodes was demonstrated on determination of rutin in the model samples and the extracts of buckwheat seeds. To find an optimum method for buckwheat seeds extraction, a boiling water extraction (BWE), Soxhlet extraction (SE), pressurized solvent extraction (PSE), and supercritical fluid extraction (SFE) were tested.

  9. 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.

  10. 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.

  11. 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

  12. A Disposable Amperometric Sensor Based on High-Performance PEDOT:PSS/Ionic Liquid Nanocomposite Thin Film-Modified Screen-Printed Electrode for the Analysis of Catechol in Natural Water Samples.

    Science.gov (United States)

    Krampa, Francis D; Aniweh, Yaw; Awandare, Gordon A; Kanyong, Prosper

    2017-07-26

    A conducting polymer-based composite material of poly(3,4-ethylenedioxythiophene) (PEDOT): poly(4-styrenesulfonate) (PSS) doped with different percentages of a room temperature ionic liquid (IL), 1-ethyl-3-methylimidazolium tetrafluoroborate ([EMIM][BF₄]), was prepared and a very small amount of the composite (2.0 µL) was drop-coated on the working area of a screen-printed carbon electrode (SPCE). The SPCE, modified with PEDOT:PSS/IL composite thin-film, was characterized by cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS), scanning electron microscopy (SEM), profilometry and sessile contact angle measurements. The prepared PEDOT:PSS/IL composite thin-film exhibited a nano-porous microstructure and was found to be highly stable and conductive with enhanced electrocatalytic properties towards catechol, a priority pollutant. The linear working range for catechol was found to be 0.1 µM-330.0 µM with a sensitivity of 18.2 mA·mM·cm -2 and a calculated limit of detection (based on 3× the baseline noise) of 23.7 µM. When the PEDOT:PSS/IL/SPCE sensor was used in conjunction with amperometry in stirred solution for the analysis of natural water samples, the precision values obtained on spiked samples (20.0 µM catechol added) ( n = 3) were 0.18% and 0.32%, respectively, with recovery values that were well over 99.0%.

  13. A Disposable Amperometric Sensor Based on High-Performance PEDOT:PSS/Ionic Liquid Nanocomposite Thin Film-Modified Screen-Printed Electrode for the Analysis of Catechol in Natural Water Samples

    Directory of Open Access Journals (Sweden)

    Francis D. Krampa

    2017-07-01

    Full Text Available A conducting polymer-based composite material of poly(3,4-ethylenedioxythiophene (PEDOT: poly(4-styrenesulfonate (PSS doped with different percentages of a room temperature ionic liquid (IL, 1-ethyl-3-methylimidazolium tetrafluoroborate ([EMIM][BF4], was prepared and a very small amount of the composite (2.0 µL was drop-coated on the working area of a screen-printed carbon electrode (SPCE. The SPCE, modified with PEDOT:PSS/IL composite thin-film, was characterized by cyclic voltammetry (CV, electrochemical impedance spectroscopy (EIS, scanning electron microscopy (SEM, profilometry and sessile contact angle measurements. The prepared PEDOT:PSS/IL composite thin-film exhibited a nano-porous microstructure and was found to be highly stable and conductive with enhanced electrocatalytic properties towards catechol, a priority pollutant. The linear working range for catechol was found to be 0.1 µM–330.0 µM with a sensitivity of 18.2 mA·mM·cm−2 and a calculated limit of detection (based on 3× the baseline noise of 23.7 µM. When the PEDOT:PSS/IL/SPCE sensor was used in conjunction with amperometry in stirred solution for the analysis of natural water samples, the precision values obtained on spiked samples (20.0 µM catechol added (n = 3 were 0.18% and 0.32%, respectively, with recovery values that were well over 99.0%.

  14. 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.

  15. 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.

  16. 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.

  17. 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)

  18. 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.

  19. 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.

  20. 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.

  1. Nitric oxide regulation of colonic epithelial ion transport: a novel role for enteric glia in the myenteric plexus.

    Science.gov (United States)

    MacEachern, Sarah J; Patel, Bhavik A; McKay, Derek M; Sharkey, Keith A

    2011-07-01

    Enteric glia are increasingly recognized as important in the regulation of a variety of gastrointestinal functions.Here we tested the hypothesis that nicotinic signalling in the myenteric plexus results in the release of nitric oxide (NO) from neurons and enteric glia to modulate epithelial ion transport. Ion transport was assessed using full-thickness or muscle-stripped segments of mouse colon mounted in Ussing chambers. The cell-permeant NO-sensitive dye DAR-4M AM and amperometry were utilized to identify the cellular sites of NO production within the myenteric plexus and the contributions from specific NOS isoforms. Nicotinic receptors were localized using immunohistochemistry. Nicotinic cholinergic stimulation of colonic segments resulted in NO-dependent changes in epithelial active electrogenic ion transport that were TTX sensitive and significantly altered in the absence of the myenteric plexus. Nicotinic stimulation of the myenteric plexus resulted in NO production and release from neurons and enteric glia, which was completely blocked in the presence of nitric oxide synthase (NOS) I and NOS II inhibitors. Using the NO scavenger 2-phenyl-4,4,5,5-tetramethylimidazoline-1-oxyl-3-oxide (PTIO), neuronal and enteric glial components of NO production were demonstrated. Nicotinic receptors were identified on enteric neurons, which express NOS I, and enteric glia, which express NOS II. These data identify a unique pathway in the mouse colon whereby nicotinic cholinergic signalling in myenteric ganglia mobilizes NO from NOS II in enteric glia, which in coordinated activity with neurons in the myenteric plexus modulates epithelial ion transport, a key component of homeostasis and innate immunity.

  2. 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.

  3. 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.

  4. 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

  5. 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.

  6. 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.

  7. 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

  8. 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.

  9. 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)

  10. 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.

  11. 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.

  12. 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.

  13. Hierarchical 3-dimensional nickel-iron nanosheet arrays on carbon fiber paper as a novel electrode for non-enzymatic glucose sensing.

    Science.gov (United States)

    Kannan, Palanisamy; Maiyalagan, Thandavarayan; Marsili, Enrico; Ghosh, Srabanti; Niedziolka-Jönsson, Joanna; Jönsson-Niedziolka, Martin

    2016-01-14

    Three-dimensional nickel-iron (3-D/Ni-Fe) nanostructures are exciting candidates for various applications because they produce more reaction-active sites than 1-D and 2-D nanostructured materials and exhibit attractive optical, electrical and catalytic properties. In this work, freestanding 3-D/Ni-Fe interconnected hierarchical nanosheets, hierarchical nanospheres, and porous nanospheres are directly grown on a flexible carbon fiber paper (CFP) substrate by a single-step hydrothermal process. Among the nanostructures, 3-D/Ni-Fe interconnected hierarchical nanosheets show excellent electrochemical properties because of its high conductivity, large specific active surface area, and mesopores on its walls (vide infra). The 3-D/Ni-Fe hierarchical nanosheet array modified CFP substrate is further explored as a novel electrode for electrochemical non-enzymatic glucose sensor application. The 3-D/Ni-Fe hierarchical nanosheet arrays exhibit significant catalytic activity towards the electrochemical oxidation of glucose, as compared to the 3-D/Ni-Fe hierarchical nanospheres, and porous nanospheres. The 3-D/Ni-Fe hierarchical nanosheet arrays can access a large amount of glucose molecules on their surface (mesopore walls) for an efficient electrocatalytic oxidation process. Moreover, 3-D/Ni-Fe hierarchical nanosheet arrays showed higher sensitivity (7.90 μA μM(-1) cm(-2)) with wide linear glucose concentration ranging from 0.05 μM to 0.2 mM, and the low detection limit (LOD) of 0.031 μM (S/N = 3) is achieved by the amperometry method. Further, the 3-D/Ni-Fe hierarchical nanosheet array modified CFP electrode can be demonstrated to have excellent selectivity towards the detection of glucose in the presence of 500-fold excess of major important interferents. All these results indicate that 3-D/Ni-Fe hierarchical nanosheet arrays are promising candidates for non-enzymatic glucose sensing.

  14. Synthesis, characterization and modification of functionalized pyrimidine stabilized gold nanoparticles on ITO electrode for the determination of tannic acid.

    Science.gov (United States)

    Raj, M Amal; Revin, S Brillians; John, S Abraham

    2013-02-01

    This paper describes the synthesis of 4-amino-6-hydroxy-2-mercaptopyrimidine capped gold nanoparticles (AHMP-AuNPs) in aqueous medium and their immobilization on indium tin oxide (ITO) electrode modified with (3-mercaptopropyl)trimethoxysilane (MPTS) sol-gel for the determination of tannic acid (TA). The high resolution transmission electron microscopy (HR-TEM) images show that the particles are spherical in shape with a diameter of ~6 nm. The heterogeneous electron transfer rate constant (k(et)) of [Fe(CN)₆]³⁻/⁴⁻ at ITO/MPTS/AHMP-AuNPs electrode was found to be 1.14×10⁻⁷ m/s. This value was much higher than the values obtained at ITO/MPTS (4.94×10⁻⁹ m/s) and bare ITO (8.79×10⁻⁸ m/s) electrodes, indicating that the electron transfer reaction was faster at AuNPs modified electrode. Further, the ITO/MPTS/AHMP-AuNPs electrode shows excellent electrocatalytic activity toward TA oxidation when compared to bare ITO electrode. This was understood from the obtained higher heterogeneous rate constant (k(s)) value at AuNPs modified electrode (7.35×10⁻⁵ m/s) than at bare ITO electrode (5.45×10⁻⁶ m/s). Using the amperometry method, detection of 20 nmol/L TA was achieved. The practical application of the present method was demonstrated by determining the concentration of TA in commercial beer samples. Copyright © 2012 Elsevier B.V. All rights reserved.

  15. 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.

  16. 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.

  17. 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)

  18. Polymerized hemin as an electrocatalytic platform for peroxynitrite's oxidation and detection.

    Science.gov (United States)

    Peteu, Serban F; Bose, Tiyash; Bayachou, Mekki

    2013-05-30

    Peroxynitrite (ONOO(-)) constitutes a major cytotoxic agent, implicated in a host of pathophysiological conditions, thereby stimulating a tremendous interest in evaluating its role as an oxidant in vivo. Some of the detection methods for peroxynitrite include oxidation of fluorescent probes, EPR spectroscopy, chemiluminescence, immunohistochemistry, and probe nitration; however, these are more difficult to apply for real-time quantification due to their inherent complexity. The electrochemical detection of peroxynitrite is a simpler and more convenient technique, but the best of our knowledge there are only few papers to date studying its electrochemical signature, or reporting amperometric microsensors for peroxynitrite. Recently, we have reported the use of layered composite films of poly(3,4-ethylenedioxythiophene) (PEDOT) and hemin (iron protoporphyrin IX) as a platform for amperometric measurement of peroxynitrite. The main goal herein is to investigate the intrinsic catalytic role of hemin electropolymerized thin films on carbon electrodes in oxidative detection of peroxynitrite. The electrocatalytic oxidation of peroxynitrite is characterized by cyclic voltammetry. The catalytic current increased as a function of peroxynitrite's concentration, with a peak potential shifting positively with peroxynitrite's concentration. The catalytic efficiency decreased as the scan rate increased, and the peak potential of the catalytic oxidation was found to depend on pH. We show that optimized hemin-functionalized carbon electrodes can be used as simple platforms for peroxinitrite detection and quantification. We report dose-response amperometry as an electroanalytical determination of this analyte on hemin films and we contrast the intrinsic hemin catalytic role with its performance in the case of the PEDOT-hemin as a composite matrix. Finally, we include some work extending the use of simple hemin films for peroxynitrite determination on carbon microfiber electrodes in

  19. 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.

  20. Analysis of Arterial Blood Gas Report in Chronic Kidney Diseases - Comparison between Bedside and Multistep Systematic Method.

    Science.gov (United States)

    Ghatak, Ishita; Dhat, Vaishali; Tilak, Mona A; Roy, Indranath

    2016-08-01

    Acid Base Disorders (ABDs) are commonly encountered in critically ill Chronic Kidney Disease (CKD) patients. Timely and correct analysis of Arterial Blood Gases (ABG) is critical for the diagnosis, treatment and prediction of outcome of the patients. The aim was to explore type and prevalence of ABDs in 31 critically ill CKD patients from a tertiary care hospital in Maharashtra, to compare two methods of analysis- bedside and systematic approaches and to clinically correlate the nature of ABDs in these patients. The initial ABG reports of 31 consecutive CKD patients were analysed by two methods. Medica Easy stat analyser was the equipment for analysis with Principle of potentiometry and ion selective electrode for pH and pCO2 and amperometry for pO2. Serum albumin was also measured by Bromocresol green dye binding method using liquixx albumin kit in Erba XL 300 autoanalyser. Chi-square test was used for statistical analysis using Epi Info version 3.5.4 and SPSS 14.0 softwares. The systematic method showed a significantly higher prevalence of mixed disorders (50%) compared to bedside method (12.9%). Most prevalent disorder by bedside method was metabolic acidosis in 15 cases (48.39%). By the systematic method, 3 reports were invalid. As a single category, most prevalent type was both simple respiratory alkalosis and mixed metabolic acidosis with respiratory alkalosis- 6 of 31 cases in each type (19.36% each). As a whole, metabolic acidosis (including both High Anion Gap Metabolic Acidosis or HAGMA and Non Anion Gap Metabolic Acidosis or NAGMA with 4 in each type) was most prevalent- 8 of 31(25.8%). Systematic approach was more effective in diagnosing mixed acid base disorders. By systematic method the findings of analysis in most cases could be correlated with the clinical condition and provisional diagnosis. Thus interpretation of ABDs by using stepwise approach could be useful to the clinicians in early diagnosis and management of the patients.

  1. 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.

  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. 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}.

  4. 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.

  5. In situ fabrication of cobalt nanoflowers on sulfonated and fluorinated poly (arylene ether ketone-benzimidazole) template film for the electrocatalytic oxidation of glucose.

    Science.gov (United States)

    Wang, Tengfei; Xi, Lingling; Wang, Jianli

    2018-02-01

    Using sulfonated and fluorinated poly (arylene ether ketone) comprising functional strong coordination group benzimidazole (SPAEK-F-BI) as a template film, a novel fabrication method of cobalt nanoflowers (CoNFs) and non-enzymatic glucose electrochemical sensor was developed in this work. After the precursors Co 2+ ions were cooperatively bound by sulfonate and imidazole functionalities contained in SPAEK-F-BI film through ion exchange and strong coordination action, cobalt colloid nuclei were formed and grew to flower-like nanostructures by subsequent in-situ electrochemical reduction on SPAEK-F-BI film modified GCE. Characterization of SPAEK-F-BI film and CoNFs/SPAEK-F-BI film on GCE was performed in detail by FT-IR spectroscopy and scanning electron microscopy (SEM) attached with energy dispersive spectroscopy (EDS), electrochemical impedance spectroscopy (EIS) and cyclic voltammetry (CV). The results of SEM showed that beautiful CoNFs constructed by Co colloid nanosheets with just a few nanometers thickness were well dispersed on uniform SPAEK-F-BI film modified GCE, and the density of CoNFs was mainly influenced by the concentration of the precursor solution CoSO 4 . The CoNFs/SPAEK-F-BI composite modified electrode exhibited good electrocatalytic activity toward glucose oxidation in 0.1M NaOH solution, and the kinetic parameters of glucose oxidation were determined using chronoamperometry. When it was applied for the determination of glucose by amperometry at a potential of 0.6V versus Ag/AgCl, the linear range from 5μM to 1.14mM and the detection limit of 800nM (S/N = 3) were obtained. Finally, it was successfully employed to detect the glucose in human serum real samples, and the results were agreed closely with those measured in hospital. Copyright © 2017. Published by Elsevier B.V.

  6. 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.

  7. 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.

  8. 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.)

  9. 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

  10. Determination of Myo-Inositol in Infant, Pediatric, and Adult Formulas by Liquid Chromatography-Pulsed Amperometric Detection with Column Switching: Collaborative Study, Final Action 2011.18.

    Science.gov (United States)

    Butler-Thompson, Linda D; Jacobs, Wesley A; Schimpf, Karen J

    2015-01-01

    AOAC First Action Method 2011.18, Myo-Inositol (Free and Bound as Phosphatidylinositol) in Infant and Pediatric Formulas and Adult Nutritionals, was collaboratively studied. With this method free myo-inositol and phosphatidylinositol bound myo-inositol are extracted using two different sample preparation procedures, separated by ion chromatography using a combination of Dionex Carbo Pac PA1 and MA1 columns with column switching, and detected with pulsed amperometry using a gold electrode. Free myo-inositol is extracted from samples with dilute hydrochloric acid and water. Phosphatidylinositol is extracted from samples with chloroform and separated from other fats with silica SPE cartridges. Myo-inositol is then released from the glycerol backbone with concentrated acetic and hydrochloric acids at 120°C. During this collaborative study, nine laboratories from five different countries analyzed blind duplicates of nine infant and pediatric nutritional formulas for both free and phosphatidylinositol bound myo-inositol, and one additional laboratory only completed the free myo-inositol analyses. The method demonstrated acceptable repeatability and reproducibility and met the AOAC Stakeholder Panel on Infant Formula and Adult Nutritionals (SPIFAN) Standard Method Performance Requirements (SMPRs®) for free myo-inositol plus phosphatidylinositol bound myo-inositol for all the matrixes analyzed. SMPRs for repeatability were ≤5% RSD at myo-inositol concentrations of 2-68 mg/100 g ready-to-feed (RTF) liquid. SMPRs for reproducibility were ≤8% RSD in products with myo-inositol concentrations ranging from 2 to 68 mg/100 g RTF liquid. During this collaborative study, repeatability RSDs ranged from 0.51 to 3.22%, and RSDs ranged from 2.66 to 7.55% for free myo-inositol plus phosphatidylinositol bound myo-inositol.

  11. Chaos evidence in catecholamine secretion at chromaffin cells

    International Nuclear Information System (INIS)

    Quiroz, G.; Bonifas, I.; Barajas-Ramirez, J.G.; Femat, R.

    2012-01-01

    Highlights: ► Nonlinear behavior in protein secretion. ► Nonlinear characterization of complex behavior in catecholamine secretion. ► Chaos in chromaffin cells activity at the adrenaline secretion. ► Preliminary evidences on the chaotic behavior in catecholamine secretion. - Abstract: Chromaffin cells secrete catecholamine molecules via exocytosis process. Each exocytotic event is characterized by a current spike, which corresponds to the amount of released catecholamine from secretory vesicles after fusing to plasma membrane. The current spike might be measured by the oxidation of catecholamine molecules and can be experimentally detected through amperometry technique. In this contribution, the secretion of catecholamine, namely adrenaline, of a set of bovine chromaffin cells is measured individually at each single cell. The aim is to study quantitative results of chaotic behavior in catecholamine secretion. For analysis, time series were obtained from amperometric measurements of each single chromaffin cell. Three analysis techniques were exploited: (i) A low-order attractor was generated by means of phase space reconstruction, Average Mutual Information (AMI) and False Nearest Neighbors (FNN) were used to compute embedding lag and embedding dimension, respectively. (ii) The properties of power spectrum density of time series were studied by Fast Fourier Transform (FFT) looking for possible dominant frequencies in power spectrum. (iii) Maximun Lyapunov Exponent (MLE) analysis was done to study the divergence of trajectories of the time series. Nevertheless, in order to dismiss the possibility of positiveness of MLE are due to the inherent noise in experiments, seven surrogate data sets computed using the Amplitude Adjusted Fourier Transform (AAFT) algorithm was computed. The phase space reconstruction showed that, in all cases, the trajectories lie in an embedding subspace suggesting oscillatory nature. The FFT analysis showed high dispersion of the power

  12. [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

  13. 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

  14. 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.

  15. 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

  16. 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.

  17. 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

  18. 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.

  19. 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

  20. 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

  1. 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.

  2. Amperometric microsensor for direct probing of ascorbic acid in human gastric juice

    Energy Technology Data Exchange (ETDEWEB)

    Hutton, Emily A.; Pauliukaite, Rasa; Hocevar, Samo B. [Analytical Chemistry Laboratory, National Institute of Chemistry, Hajdrihova 19, SI-1000 Ljubljana (Slovenia); Ogorevc, Bozidar, E-mail: bogorevc@ki.s [Analytical Chemistry Laboratory, National Institute of Chemistry, Hajdrihova 19, SI-1000 Ljubljana (Slovenia); Smyth, Malcolm R. [National Centre for Sensor Research, School of Chemical Sciences, Dublin City University, Dublin 9 (Ireland)

    2010-09-30

    This article reports on a novel microsensor for amperometric measurement of ascorbic acid (AA) under acidic conditions (pH 2) based on a carbon fiber microelectrode (CFME) modified with nickel oxide and ruthenium hexacyanoferrate (NiO-RuHCF). This sensing layer was deposited electrochemically in a two-step procedure involving an initial galvanostatic NiO deposition followed by a potentiodynamic RuHCF deposition from solutions containing the precursor salts. Several important parameters were examined to characterize and optimize the NiO-RuHCF sensing layer with respect to its current response to AA by using cyclic voltammetry, and scanning electron microscopy-energy dispersive X-ray spectroscopy methods. With the NiO-RuHCF coated CFME, the AA oxidation potential under acidic conditions was shifted to a less positive value for about 0.2 V (E{sub p} of ca. 0.23 V vs. Ag/AgCl) as compared to a bare CFME, which greatly improves the electrochemical selectivity. Using the hydrodynamic amperometry mode, the current vs. AA concentration in 0.01 M HCl, at a selected operating potential of 0.30 V, was found to be linear over a wide range of 10-1610 {mu}M (n = 22, r = 0.999) with a calculated limit of detection of 1.0 {mu}M. The measurement repeatability was satisfactory with a relative standard deviation (r.s.d.) ranging from 4% to 5% (n = 6), depending on the AA concentration, and with a sensor-to-sensor reproducibility (r.s.d.) of 6.9% at 100 {mu}M AA. The long-term reproducibility, using the same microsensor for 112 consecutive measurements of 20 {mu}M AA over 11 h of periodic probing sets over 4 days, was 16.1% r.s.d., thus showing very good stability at low AA levels and suitability for use over a prolonged period of time. Moreover, using the proposed microsensor, additionally coated with a protective cellulose acetate membrane, the calibration plot obtained in the extremely complex matrix of real undiluted gastric juice was linear from 10 to 520 {mu}M (n = 14, r = 0

  3. Amperometric microsensor for direct probing of ascorbic acid in human gastric juice

    International Nuclear Information System (INIS)

    Hutton, Emily A.; Pauliukaite, Rasa; Hocevar, Samo B.; Ogorevc, Bozidar; Smyth, Malcolm R.

    2010-01-01

    This article reports on a novel microsensor for amperometric measurement of ascorbic acid (AA) under acidic conditions (pH 2) based on a carbon fiber microelectrode (CFME) modified with nickel oxide and ruthenium hexacyanoferrate (NiO-RuHCF). This sensing layer was deposited electrochemically in a two-step procedure involving an initial galvanostatic NiO deposition followed by a potentiodynamic RuHCF deposition from solutions containing the precursor salts. Several important parameters were examined to characterize and optimize the NiO-RuHCF sensing layer with respect to its current response to AA by using cyclic voltammetry, and scanning electron microscopy-energy dispersive X-ray spectroscopy methods. With the NiO-RuHCF coated CFME, the AA oxidation potential under acidic conditions was shifted to a less positive value for about 0.2 V (E p of ca. 0.23 V vs. Ag/AgCl) as compared to a bare CFME, which greatly improves the electrochemical selectivity. Using the hydrodynamic amperometry mode, the current vs. AA concentration in 0.01 M HCl, at a selected operating potential of 0.30 V, was found to be linear over a wide range of 10-1610 μM (n = 22, r = 0.999) with a calculated limit of detection of 1.0 μM. The measurement repeatability was satisfactory with a relative standard deviation (r.s.d.) ranging from 4% to 5% (n = 6), depending on the AA concentration, and with a sensor-to-sensor reproducibility (r.s.d.) of 6.9% at 100 μM AA. The long-term reproducibility, using the same microsensor for 112 consecutive measurements of 20 μM AA over 11 h of periodic probing sets over 4 days, was 16.1% r.s.d., thus showing very good stability at low AA levels and suitability for use over a prolonged period of time. Moreover, using the proposed microsensor, additionally coated with a protective cellulose acetate membrane, the calibration plot obtained in the extremely complex matrix of real undiluted gastric juice was linear from 10 to 520 μM (n = 14, r = 0.998). These

  4. 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.

  5. 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

  6. 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

  7. Chemical composition, pH, and redox state of sulfur and iron in complete vertical porewater profiles from two Sphagnum peat bogs, Jura Mountains, Switzerland

    Science.gov (United States)

    Steinmann, Philipp; Shotyk, William

    1997-03-01

    Complete porewater profiles from two peat bogs in the Jura Mountains were analysed for major and trace inorganic anions and cations. At La Tourbière des Genevez (TGe) and Etang de la Gruère (EGr), peat formation began approximately 5,000 and 10,000 years BP, respectively. The maximum depths of peat accumulation are 140 cm (TGe) and 650 cm (EGr); previous geochemical studies showed that the ombrogenic sections of the bogs extend to depths of approximately 20 cm (TGe) and 250 cm (EGr). Water samples were obtained using in situ diffusion equilibrium samplers (peepers), which allow filtered (0.2 μm) porewaters to be obtained while preventing degassing and oxidation. These samplers were found to be well suited to bog porewaters and allowed volatile (dissolved CO 2, acetate) and redox-sensitive species (HS -, Fe 2+) to be quantified without further sample preparation or treatment. Aqueous species concentrations were determined immediately afterwards using ion chromatography with either conductivity (acetate, HCO 3-, Cl -, Br -, NO 3-, HPO 42-, SO 42-, Na +, NH 4+, K +, Mg 2+, Ca 2+), amperometry (HS -), or absorbance detection (Fe(III) and Fe(II)). The comprehensive analyses of anions and cations allowed humic substances to be calculated by the difference in electrical charge balance (i.e., the anion deficit). Concentrations of total dissolved CO 2 (2-12 mM) showed that carbonate equilibria play a significant role in the acid-base chemistry throughout the profiles. In near surface, ombrogenic porewaters with pH around 4, however, protons (approx. 160 μeq/L) are contributed mainly by the dissociation of humic substances (2-7 mM DOC). In the deepest, minerogenic layers H 2CO 3 is the predominant acid at both sites. At these depths, carbonate alkalinity (up to 3 meq/L at EGr, up to 8 meq/L at TGe) arises from reaction of the pore fluids with mineral matter in the underlying sediments. In the transition zone between the ombrogenic and minerogenic extremes, organic and

  8. 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

  9. 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

  10. 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.

  11. 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

  12. 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