Square-wave adsorptive stripping voltammetric determination of nanomolar levels of bezafibrate using a glassy carbon electrode modified with multi-walled carbon nanotubes within a dihexadecyl hydrogen phosphate film.

PubMed

Ardila, Jorge Armando; Oliveira, Geiser Gabriel; Medeiros, Roberta Antigo; Fatibello-Filho, Orlando

2014-04-07

A highly sensitive method for bezafibrate determination using a glassy carbon electrode (GCE) modified with multi-walled carbon nanotubes within a dihexadecyl hydrogen phosphate film based on square-wave adsorptive stripping voltammetry (SWAdSV) is proposed. The electrochemical behaviour of bezafibrate has been studied by cyclic voltammetry, showing an irreversible anodic peak at a potential of 1.09 V in 0.1 mol L(-1) phosphate buffer solution (pH 2.0). A study of the scan rate showed that the oxidation of bezafibrate is an adsorptive-controlled process, involving the transfer of two electrons and two protons per molecule. The analytical curve was linear over a bezafibrate concentration range from 50 to 910 nmol L(-1), with a detection limit of 16 nmol L(-1). This analytical method was successfully applied for benzafibrate determination in pharmaceutical formulations, with results showing good agreement with those obtained using a comparative spectrophotometric method, and has the potential for field application.

Development of square wave voltammetry method for the assessment of organophosphorus compound impact on the cholinesterase of Pheretima with 2,6-dichloroindophenol as a redox indicator.

PubMed

Qiu, Jingxia; Chen, Jin; Ma, Qianqian; Miao, Yuqing

2009-09-01

A square wave voltammetry method was developed for the assessment of organophosphorus (OPs) compound impact on the cholinesterase of Pheretima with 2,6-dichloroindophenol (2,6-DCIP) as a redox indicator. The substrate of acetylthiocholine is hydrolysed by the cholinesterase (ChE) from soil animal pheretima, and the produced thiocholine reacts with the 2,6-DCIP to give obvious shift of electrochemical signal. The inhibition of ChE was assessed by measuring the enzyme activity before and after incubating with parathion-methyl. The reduction peak current of 2,6-DCIP decreases with the time of enzymatical reaction. The ChE loses almost 32.74% activity after 10 min incubation with 1ng mL(-1) paraoxon and 54.62% with 10 microg mL(-1) paraoxon, while the activity that corresponds to 100 microg mL(-1) paraoxon was nearly completely inhibited. This method can be employed to assess the inhibition of ChE and investigate OPs impact on environmental animals.

A graphene-based electrochemical competitive immunosensor for the sensitive detection of okadaic acid in shellfish

NASA Astrophysics Data System (ADS)

Eissa, Shimaa; Zourob, Mohammed

2012-11-01

A novel graphene-based voltammetric immunosensor for sensitive detection of okadaic acid (OA) was developed. A simple and efficient electrografting method was utilized to functionalize graphene-modified screen-printed carbon electrodes (GSPE) by the electrochemical reduction of in situ generated 4-carboxyphenyl diazonium salt in acidic aqueous solution. Next, the okadaic acid antibody was covalently immobilized on the carboxyphenyl modified graphene electrodes via carbodiimide chemistry. Square wave voltammetry (SWV) was used to investigate the stepwise assembly of the immunosensor. A competitive assay between OA and a fixed concentration of okadaic acid-ovalbumin conjugate (OA-OVA) for the immobilized antibodies was employed for the detection of okadaic acid. The decrease of the [Fe(CN)6]3-/4- reduction peak current in the square wave voltammetry for various concentrations of okadaic acid was used for establishing the calibration curve. A linear relationship between the SWV peak current difference and OA concentration was obtained up to ~5000 ng L-1. The developed immunosensor allowed a detection limit of 19 ng L-1 of OA in PBS buffer. The matrix effect studied with spiked shellfish tissue extracts showed a good percentage of recovery and the method was also validated with certified reference mussel samples.A novel graphene-based voltammetric immunosensor for sensitive detection of okadaic acid (OA) was developed. A simple and efficient electrografting method was utilized to functionalize graphene-modified screen-printed carbon electrodes (GSPE) by the electrochemical reduction of in situ generated 4-carboxyphenyl diazonium salt in acidic aqueous solution. Next, the okadaic acid antibody was covalently immobilized on the carboxyphenyl modified graphene electrodes via carbodiimide chemistry. Square wave voltammetry (SWV) was used to investigate the stepwise assembly of the immunosensor. A competitive assay between OA and a fixed concentration of okadaic acid-ovalbumin conjugate (OA-OVA) for the immobilized antibodies was employed for the detection of okadaic acid. The decrease of the [Fe(CN)6]3-/4- reduction peak current in the square wave voltammetry for various concentrations of okadaic acid was used for establishing the calibration curve. A linear relationship between the SWV peak current difference and OA concentration was obtained up to ~5000 ng L-1. The developed immunosensor allowed a detection limit of 19 ng L-1 of OA in PBS buffer. The matrix effect studied with spiked shellfish tissue extracts showed a good percentage of recovery and the method was also validated with certified reference mussel samples. Electronic supplementary information (ESI) available. See DOI: 10.1039/c2nr32146g

Modified magnetic nanoparticles in an electrochemical method for the ochratoxin A determination in Vitis vinifera red grapes tissues.

PubMed

Fernández-Baldo, Martín A; Bertolino, Franco A; Messina, Germán A; Sanz, Maria I; Raba, Julio

2010-12-15

This work described the development and characterization of an electrochemical method using square wave voltammetry (SWV) combined with the use of modified magnetic nanoparticles (MNPs), which had shown a rapid and sensitive determination of ochratoxin A (OTA) in wine grapes (Cabernet Sauvignon, Malbec and Syrah) post-harvest tissues. The wine grapes were inoculated with Aspergillus ochraceus to obtain OTA in artificially infected samples. The OTA was directly determined using square-wave voltammetry. The current obtained is directly proportional to the concentration of OTA present in the samples. This method has been used for OTA determination in wine grapes and it was validated against a commercial ELISA test kit. The limits of detection calculated for electrochemical detection and the ELISA were 0.02 and 1.9 μg kg(-1), respectively and the coefficients of variation for accuracy and precision dates were below 5.5%. This method promises to be suitable for the detection and quantification of OTA in apparently healthy fruits post-harvest for assuring safety and quality of food as well as consumer's health. Copyright © 2010 Elsevier B.V. All rights reserved.

Electrochemical detection and degradation of ibuprofen from water on multi-walled carbon nanotubes-epoxy composite electrode.

PubMed

Motoc, Sorina; Remes, Adriana; Pop, Aniela; Manea, Florica; Schoonman, Joop

2013-04-01

This work describes the electrochemical behaviour of ibuprofen on two types of multi-walled carbon nanotubes based composite electrodes, i.e., multi-walled carbon nanotubes-epoxy (MWCNT) and silver-modified zeolite-multi-walled carbon nanotubes-epoxy (AgZMWCNT) composites electrodes. The composite electrodes were obtained using two-roll mill procedure. SEM images of surfaces of the composites revealed a homogeneous distribution of the composite components within the epoxy matrix. AgZMWCNT composite electrode exhibited the better electrical conductivity and larger electroactive surface area. The electrochemical determination of ibuprofen (IBP) was achieved using AgZMWCNT by cyclic voltammetry, differential-pulsed voltammetry, square-wave voltammetry and chronoamperometry. The IBP degradation occurred on both composite electrodes under controlled electrolysis at 1.2 and 1.75 V vs. Ag/AgCl, and IBP concentration was determined comparatively by differential-pulsed voltammetry, under optimized conditions using AgZMWCNT electrode and UV-Vis spectrophotometry methods to determine the IBP degradation performance for each electrode. AgZMWCNT electrode exhibited a dual character allowing a double application in IBP degradation process and its control.

EFFECTS OF POLYCYCLIC AROMATIC HYDROCARBON OF SAM-COATED ELECTRODES USING FERRYICYANIDE AS THE REDOX INDICATOR

EPA Science Inventory

Electrochemical responses on self-assembled monolayer (SAM)-coated polycrystalline gold electrodes were investigated using cyclic voltammetry and square wave voltammetry with a three electrode system. Experimental results show potential in the application of pyrene-imprinted SAM...

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

PubMed

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

2016-11-01

Poly(4-amino-3-hydroxynaphthalene sulfonic acid)-modified glassy carbon electrode (poly(AHNSA)/GCE) was prepared for simultaneous determination of caffeine and paracetamol using square-wave voltammetry. The method was used to study the effects of pH and scan rate on the voltammetric response of caffeine and paracetamol. Linear calibration curves in the range of 10-125μM were obtained for both caffeine and paracetamol in acetate buffer solution of pH 4.5 with a correlation coefficient of 0.9989 and 0.9986, respectively. The calculated detection limits (S/N=3) were 0.79μM for caffeine and 0.45μM for paracetamol. The effects of some interfering substances in the determination of caffeine and paracetamol were also studied and their interferences were found to be negligible which proved the selectivity of the modified electrode. The method was successfully applied for the quantitative determination of caffeine and paracetamol in Coca-Cola, Pepsi-Cola and tea samples. Copyright © 2016 Elsevier Ltd. All rights reserved.

Square-wave stripping voltammetric determination of caffeic acid on electrochemically reduced graphene oxide-Nafion composite film.

PubMed

Filik, Hayati; Çetintaş, Gamze; Avan, Asiye Aslıhan; Aydar, Sevda; Koç, Serkan Naci; Boz, İsmail

2013-11-15

An electrochemical sensor composed of Nafion-graphene nanocomposite film for the voltammetric determination of caffeic acid (CA) was studied. A Nafion graphene oxide-modified glassy carbon electrode was fabricated by a simple drop-casting method and then graphene oxide was electrochemically reduced over the glassy carbon electrode. The electrochemical analysis method was based on the adsorption of caffeic acid on Nafion/ER-GO/GCE and then the oxidation of CA during the stripping step. The resulting electrode showed an excellent electrocatalytical response to the oxidation of caffeic acid (CA). The electrochemistry of caffeic acid on Nafion/ER-GO modified glassy carbon electrodes (GCEs) were studied by cyclic voltammetry and square-wave adsorption stripping voltammetry (SW-AdSV). At optimized test conditions, the calibration curve for CA showed two linear segments: the first linear segment increased from 0.1 to 1.5 and second linear segment increased up to 10 µM. The detection limit was determined as 9.1×10(-8) mol L(-1) using SW-AdSV. Finally, the proposed method was successfully used to determine CA in white wine samples. Copyright © 2013 Elsevier B.V. All rights reserved.

Alternating current scanning electrochemical microscopy with simultaneous fast-scan cyclic voltammetry.

PubMed

Koch, Jason A; Baur, Melinda B; Woodall, Erica L; Baur, John E

2012-11-06

Fast-scan cyclic voltammetry (FSCV) is combined with alternating current scanning electrochemical microscopy (AC-SECM) for simultaneous measurements of impedance and faradaic current. Scan rates of 10-1000 V s(-1) were used for voltammetry, while a high-frequency (100 kHz), low-amplitude (10 mV rms) sine wave was added to the voltammetric waveform for the ac measurement. Both a lock-in amplifier and an analog circuit were used to measure the amplitude of the resultant ac signal. The effect of the added sine wave on the voltammetry at a carbon fiber electrode was investigated and found to have negligible effect. The combined FSCV and ac measurements were used to provide simultaneous chemical and topographical information about a substrate using a single carbon fiber probe. The technique is demonstrated in living cell culture, where cellular respiration and topography were simultaneously imaged without the addition of a redox mediator. This approach promises to be useful for the topographical and multidimensional chemical imaging of substrates.

New luminescent bioprobes Eu(lll)-phloroglucinol derivatives and their spectrofluorimetric, electrochemical interactions with nucleotides and DNA.

PubMed

Azab, Hassan Ahmed; Anwar, Zeinab M; Abdel-Salam, Enas T; el-Sayed-Sebak, Mahmoud

2012-01-01

Two new ligands derived from phloroglucinol 2-{[(4-methoxy benzoyl)oxy]} methyl benzoic acid[L1] and 2-{[(4-methyl benzoyl)oxy] methyl} benzoic acid[L2] were synthesized. The solid complex Eu(III)-L2 has been synthesised and characterized by elemental analysis, UV and IR spectra. The reaction of Eu(III) with the two synthesized ligands has been investigated in I = 0.1 mol dm(-3) p-toluene sulfonate by cyclic voltammetry and square wave voltammetry. The reaction of Eu (III)-L1 and Eu (III)-L2 binary complexes with nucleotide 5'-AMP, 5'-ADP, 5'-ATP, 5'- GMP, 5'-IMP, and 5'-CMP has been investigated using UV, fluorescence and electrochemical methods. The experimental conditions were selected such that self-association of the nucleotides and their complexes was negligibly small, that is, the monomeric complexes were studied. The interaction of the Eu(III)-L1 or L2 solid complexes with calf-thymus DNA has been investigated by fluorescence and electrochemical methods including cyclic voltammetery(CV), differential pulse polarography (DPP) and square wave voltammetry (SWV) on a glassy carbon electrode. The fluorescence intensity of Eu(III)-L2 complex was enhanced with the addition of DNA. Under optimal conditions in phosphate buffer pH 7.0 at 25 °C the linear range is 3-20 μM for calf thymus DNA (CT-DNA) and the corresponding determination limit is 1.8 μM.

Quantitative weaknesses of the Marcus-Hush theory of electrode kinetics revealed by Reverse Scan Square Wave Voltammetry: The reduction of 2-methyl-2-nitropropane at mercury microelectrodes

NASA Astrophysics Data System (ADS)

Laborda, Eduardo; Wang, Yijun; Henstridge, Martin C.; Martínez-Ortiz, Francisco; Molina, Angela; Compton, Richard G.

2011-08-01

The Marcus-Hush and Butler-Volmer kinetic electrode models are compared experimentally by studying the reduction of 2-methyl-2-nitropropane in acetonitrile at mercury microelectrodes using Reverse Scan Square Wave Voltammetry. This technique is found to be very sensitive to the electrode kinetics and to permit critical comparison of the two models. The Butler-Volmer model satisfactorily fits the experimental data whereas Marcus-Hush does not quantitatively describe this redox system.

Copper-Based Electrochemical Sensor with Palladium Electrode for Cathodic Stripping Voltammetry of Manganese

PubMed Central

2015-01-01

In this work, we report on the development of a palladium-based, microfabricated point-of-care electrochemical sensor for the determination of manganese using square wave cathodic stripping voltammetry. Heavy metals require careful monitoring, yet current methods are too complex for a point-of-care system. Voltammetry offers an attractive approach to metal detection on the microscale, but traditional carbon, gold, or platinum electrodes are difficult or expensive to microfabricate, preventing widespread use. Our sensor uses palladium working and auxiliary electrodes and integrates them with a copper-based reference electrode for simple fabrication and compatibility with microfabrication and printed circuit board processing, while maintaining competitive performance in electrochemical detection. Copper electrodes were prepared on glass substrate using a combination of microfabrication procedures followed by electrodeposition of palladium. The disposable sensor system was formed by bonding a poly(dimethylsiloxane) (PDMS) well to the glass substrate. Cathodic stripping voltammetry of manganese using our new disposable palladium-based sensors exhibited 334 nM (18.3 ppb) limit of detection in borate buffer. The sensor was used to demonstrate manganese determination in natural water samples from a pond in Burnet Woods, located in Cincinnati, OH, and the Ohio River. PMID:25476591

Copper-based electrochemical sensor with palladium electrode for cathodic stripping voltammetry of manganese.

PubMed

Kang, Wenjing; Pei, Xing; Bange, Adam; Haynes, Erin N; Heineman, William R; Papautsky, Ian

2014-12-16

In this work, we report on the development of a palladium-based, microfabricated point-of-care electrochemical sensor for the determination of manganese using square wave cathodic stripping voltammetry. Heavy metals require careful monitoring, yet current methods are too complex for a point-of-care system. Voltammetry offers an attractive approach to metal detection on the microscale, but traditional carbon, gold, or platinum electrodes are difficult or expensive to microfabricate, preventing widespread use. Our sensor uses palladium working and auxiliary electrodes and integrates them with a copper-based reference electrode for simple fabrication and compatibility with microfabrication and printed circuit board processing, while maintaining competitive performance in electrochemical detection. Copper electrodes were prepared on glass substrate using a combination of microfabrication procedures followed by electrodeposition of palladium. The disposable sensor system was formed by bonding a poly(dimethylsiloxane) (PDMS) well to the glass substrate. Cathodic stripping voltammetry of manganese using our new disposable palladium-based sensors exhibited 334 nM (18.3 ppb) limit of detection in borate buffer. The sensor was used to demonstrate manganese determination in natural water samples from a pond in Burnet Woods, located in Cincinnati, OH, and the Ohio River.

IMPACT OF POLYCYCLIC AROMATIC HYDROCARBONS OF THE ELECTROCHEMICAL RESPONSES OF A FERRICYNIDE PROBE AT TEMPLATE-MODIFIED SELF ASSEMBLED MONOLAYERS ON GOLD ELECTRODES

EPA Science Inventory

The impact of pyrene on the electrochemical response of the ferricyanide probe using Self Assembled Monolayer (SAM)-modified gold electrodes was investigated using Cyclic Voltammetry (CV) and Square Wave Voltammetry (SWV). These results suggest the feasibility of using SAMs, par...

Boron doped diamond sensor for sensitive determination of metronidazole: Mechanistic and analytical study by cyclic voltammetry and square wave voltammetry.

PubMed

Ammar, Hafedh Belhadj; Brahim, Mabrouk Ben; Abdelhédi, Ridha; Samet, Youssef

2016-02-01

The performance of boron-doped diamond (BDD) electrode for the detection of metronidazole (MTZ) as the most important drug of the group of 5-nitroimidazole was proven using cyclic voltammetry (CV) and square wave voltammetry (SWV) techniques. A comparison study between BDD, glassy carbon and silver electrodes on the electrochemical response was carried out. The process is pH-dependent. In neutral and alkaline media, one irreversible reduction peak related to the hydroxylamine derivative formation was registered, involving a total of four electrons. In acidic medium, a prepeak appears probably related to the adsorption affinity of hydroxylamine at the electrode surface. The BDD electrode showed higher sensitivity and reproducibility analytical response, compared with the other electrodes. The higher reduction peak current was registered at pH11. Under optimal conditions, a linear analytical curve was obtained for the MTZ concentration in the range of 0.2-4.2μmolL(-1), with a detection limit of 0.065μmolL(-1). Copyright © 2015 Elsevier B.V. All rights reserved.

Electrochemical approach for acute myocardial infarction diagnosis based on direct antibodies-free analysis of human blood plasma.

PubMed

Suprun, Elena V; Saveliev, Anatoly A; Evtugyn, Gennady A; Lisitsa, Alexander V; Bulko, Tatiana V; Shumyantseva, Victoria V; Archakov, Alexander I

2012-03-15

A novel direct antibodies-free electrochemical approach for acute myocardial infarction (AMI) diagnosis has been developed. For this purpose, a combination of the electrochemical assay of plasma samples with chemometrics was proposed. Screen printed carbon electrodes modified with didodecyldimethylammonium bromide were used for plasma charactrerization by cyclic (CV) and square wave voltammetry and square wave (SWV) voltammetry. It was shown that the cathodic peak in voltammograms at about -250 mV vs. Ag/AgCl can be associated with AMI. In parallel tests, cardiac myoglobin and troponin I, the AMI biomarkers, were determined in each sample by RAMP immunoassay. The applicability of the electrochemical testing for AMI diagnostics was confirmed by statistical methods: generalized linear model (GLM), linear discriminant analysis (LDA) and quadratic discriminant analysis (QDA), artificial neural net (multi-layer perception, MLP), and support vector machine (SVM), all of which were created to obtain the "True-False" distribution prediction where "True" and "False" are, respectively, positive and negative decision about an illness event. Copyright © 2011 Elsevier B.V. All rights reserved.

Application of silica fume as a new SP-extractor for trace determination of Zn(II) and Cd(II) in pharmaceutical and environmental samples by square-wave anodic stripping voltammetry

NASA Astrophysics Data System (ADS)

Ahmed, Salwa A.; Gaber, Ahmed A. Abdel; Rahim, Asmaa M. Abdel

2017-05-01

In this work, silica fume (SF) is used as a solid-phase extractor for extraction of Zn(II) and Cd(II) from aqueous solutions. Characterization of SF is performed by Fourier transform infrared, X-ray diffraction, transmission and scanning electron microscopy. The optimum experimental conditions for the two metal ions are investigated using batch and column techniques. The maximum adsorption capacity values are found to be 54.13 and 121.28 mg g-1 at the optimum pH 6.0 and 8.0 for Zn(II) and Cd(II), respectively. The equilibrium data are analyzed using the Langmuir, Freundlich, and Temkin isotherms by nonlinear regression analysis. Also, the kinetics analysis revealed that the overall adsorption process is successfully fitted with the pseudo-second-order model. The method is applied for determination of the target metal ions in pharmaceutical and environmental samples using square-wave anodic stripping voltammetry. The limit of detection (LOD) values are 0.102 and 1.43 × 10-3 mg L-1 for Zn(II) and Cd(II), respectively. The percentage recovery values are 98.8-100.5 % which indicate the success of the proposed method for determination of Zn(II) and Cd(II) without interfering effects.

Synthesis and bioelectrochemical behavior of aromatic amines.

PubMed

Shabbir, Muhammad; Akhter, Zareen; Ahmad, Iqbal; Ahmed, Safeer; Bolte, Michael; McKee, Vickie

2017-12-01

Four aromatic amines 1-amino-4-phenoxybenzene (A 1 ), 4-(4-aminophenyloxy) biphenyl (A 2 ), 1-(4-aminophenoxy) naphthalene (A 3 ) and 2-(4-aminophenoxy) naphthalene (A 4 ) were synthesized and characterized by elemental, spectroscopic (FTIR, NMR), mass spectrometric and single crystal X-ray diffraction methods. The compounds crystallized in monoclinic crystal system with space group P2 1 . Intermolecular hydrogen bonds were observed between the amine group and amine/ether acceptors of neighboring molecules. Electrochemical investigations were done using cyclic voltammetry (CV), square wave voltammetry (SWV) and differential pulse voltammetry (DPV). CV studies showed that oxidation of aromatic amines takes place at about 0.9 V (vs. Ag/AgCl) and the electron transfer (ET) process has irreversible nature. After first scan reactive intermediate were generated electrochemically and some other cathodic and anodic peaks also appeared in the succeeding scans. DPV study revealed that ET process is accompanied by one electron. DNA binding study of aromatic amines was performed by CV and UV-visible spectroscopy. These investigations revealed groove binding mode of interaction of aromatic amines with DNA. Copyright © 2017 Elsevier Inc. All rights reserved.

Determination of mercury in ambient water samples by anodic stripping voltammetry on screen-printed gold electrodes.

PubMed

Bernalte, E; Marín Sánchez, C; Pinilla Gil, E

2011-03-09

The applicability of commercial screen-printed gold electrodes (SPGEs) for the determination of Hg(II) in ambient water samples by square wave anodic stripping voltammetry has been demonstrated. Electrode conditioning procedures, chemical and instrumental variables have been optimized to develop a reliable method capable of measuring dissolved mercury in the low ng mL(-1) range (detection limit 1.1 ng mL(-1)), useful for pollution monitoring or screening purposes. The proposed method was tested with the NIST 1641d Mercury in Water Standard Reference Material (recoveries 90.0-110%) and the NCS ZC 76303 Mercury in Water Certified Reference Material (recoveries 82.5-90.6%). Waste water samples from industrial origin and fortified rain water samples were assayed for mercury by the proposed method and by a reference ICP-MS method, with good agreement. Screen printing technology thus opens a useful way for the construction of reliable electrochemical sensors for decentralized or even field Hg(II) testing. Copyright © 2011 Elsevier B.V. All rights reserved.

Development and Optimization of Voltammetric Methods for Real Time Analysis of Electrorefiner Salt with High Concentrations of Actinides and Fission Products

DOE Office of Scientific and Technical Information (OSTI.GOV)

Simpson, Michael F.; Phongikaroon, Supathorn; Zhang, Jinsuo

This project addresses the problem of achieving accurate material control and accountability (MC&A) around pyroprocessing electrorefiner systems. Spent nuclear fuel pyroprocessing poses a unique challenge with respect to reprocessing technology in that the fuel is never fully dissolved in the process fluid. In this case, the process fluid is molten, anhydrous LiCl-KCl salt. Therefore, there is no traditional input accountability tank. However, electrorefiners (ER) accumulate very large quantities of fissile nuclear material (including plutonium) and should be well safeguarded in a commercial facility. Idaho National Laboratory (INL) currently operates a pyroprocessing facility for treatment of spent fuel from Experimental Breedermore » Reactor-II with two such ER systems. INL implements MC&A via a mass tracking model in combination with periodic sampling of the salt and other materials followed by destructive analysis. This approach is projected to be insufficient to meet international safeguards timeliness requirements. A real time or near real time monitoring method is, thus, direly needed to support commercialization of pyroprocessing. A variety of approaches to achieving real time monitoring for ER salt have been proposed and studied to date—including a potentiometric actinide sensor for concentration measurements, a double bubbler for salt depth and density measurements, and laser induced breakdown spectroscopy (LIBS) for concentration measurements. While each of these methods shows some promise, each also involves substantial technical complexity that may ultimately limit their implementation. Yet another alternative is voltammetry—a very simple method in theory that has previously been tested for this application to a limited extent. The equipment for a voltammetry system consists of off-the-shelf components (three electrodes and a potentiostat), which results in substantial benefits relative to cost and robustness. Based on prior knowledge of electrochemical reduction potentials for each of the species of interest, voltammetry can be used to quantify concentrations of a variety of elemental species—including uranium, plutonium, minor actinides, and rare earths. Various methods have been tested by other researchers to date—including cyclic voltammetry, square wave voltammetry, normal pulse voltammetry, etc. In most cases, it has been observed that there is a very limited concentration range for which the output can be readily correlated with concentration in the salt. Furthermore, testing to date has been limited to simple ternary salts with only a single element being quantified. While incomplete for application to MC&A for pyroprocessing, these results lead us to believe that voltammetry can be optimized based on salt properties and fundamental electrochemical rate processes to yield a highly accurate and robust method. This project is divided into four tasks jointly executed by three university research groups. This includes experimental measurement of key physical data on the systems of interest, development of a predictive voltammetry model, experimental validation of the voltammetry model, and design/verification of an optimized measurement method. This project supports the goals of the US-ROK Joint Fuel Cycle Study in addition to the NA-24 Office of the National Nuclear Security Agency and the International Atomic Energy Agency (IAEA).« less

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

PubMed Central

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

Electrochemical mechanism of tin membrane electrodeposition under ultrasonic waves.

PubMed

Nan, Tianxiang; Yang, Jianguang; Chen, Bing

2018-04-01

Tin was electrodeposited from chloride solutions using a membrane cell under ultrasonic waves. Cyclic voltammetry (CV), linear sweep voltammetry (LSV), chronoamperometry (CHR), and chronopotentiometry were applied to investigate the electrochemical mechanism of tin electrodeposition under ultrasonic field. Chronoamperometry curves showed that the initial process of tin electrodeposition followed the diffusion controlled three-dimensional nucleation and grain growth mechanism. The analysis of the cyclic voltammetry and linear sweep voltammetry diagrams showed that the application of ultrasound can change the tin membrane electro-deposition reaction from diffusion to electrochemical control, and the optimum parameters for tin electrodeposition were H + concentration 3.5 mol·L -1 , temperature 35 °C and ultrasonic power 100 W. The coupling ultrasonic field played a role in refining the grain in this process. The growth of tin crystals showed no orientation preferential, and the tin deposition showed a tendency to form a regular network structure after ultrasonic coupling. While in the absence of ultrasonic coupling, the growth of tin crystals has a high preferential orientation, and the tin deposition showed a tendency to form tin whiskers. Ultrasonic coupling was more favorable for obtaining a more compact and smoother cathode tin layer. Copyright © 2017 Elsevier B.V. All rights reserved.

Electrochemical sensing of ammonium ion at the water/1,6-dichlorohexane interface.

PubMed

Ribeiro, José A; Silva, F; Pereira, Carlos M

2012-01-15

In this work, ion transfer and facilitated ion transfer of ammonium ion by a lipophilic cyclodextrin is investigated at the water/1,6-dichlorohexane micro-interface, using electrochemical approaches (cyclic voltammetry, differential pulse voltammetry and square wave voltammetry). The association constant has been obtained for the complex between ammonium ion and the cyclodextrin. Experimental conditions for the analytical determination of ammonium ion were established and a detection limit of 0.12 μM was obtained. The amperometric sensor gave a current response proportional to the ammonium ion concentration in the range from 4.2 to 66 μM. Copyright © 2011 Elsevier B.V. All rights reserved.

Microelectrode voltammetry of multi-electron transfers complicated by coupled chemical equilibria: a general theory for the extended square scheme.

PubMed

Laborda, Eduardo; Gómez-Gil, José María; Molina, Angela

2017-06-28

A very general and simple theoretical solution is presented for the current-potential-time response of reversible multi-electron transfer processes complicated by homogeneous chemical equilibria (the so-called extended square scheme). The expressions presented here are applicable regardless of the number of electrons transferred and coupled chemical processes, and they are particularized for a wide variety of microelectrode geometries. The voltammetric response of very different systems presenting multi-electron transfers is considered for the most widely-used techniques (namely, cyclic voltammetry, square wave voltammetry, differential pulse voltammetry and steady state voltammetry), studying the influence of the microelectrode geometry and the number and thermodynamics of the (electro)chemical steps. Most appropriate techniques and procedures for the determination of the 'interaction' between successive transfers are discussed. Special attention is paid to those situations where homogeneous chemical processes, such as protonation, complexation or ion association, affect the electrochemical behaviour of the system by different stabilization of the oxidation states.

Poly arginine-graphene quantum dots as a biocompatible and non-toxic nanocomposite: Layer-by-layer electrochemical preparation, characterization and non-invasive malondialdehyde sensory application in exhaled breath condensate.

PubMed

Hasanzadeh, Mohammad; Mokhtari, Fozieh; Shadjou, Nasrin; Eftekhari, Aziz; Mokhtarzadeh, Ahad; Jouyban-Gharamaleki, Vahid; Mahboob, Soltanali

2017-06-01

This study reports on the electropolymerization of a low toxic and biocompatible polymer with entitle poly arginine-graphene quantum dots (PARG-GQDs) as a novel strategy for surface modification of glassy carbon (GC) surface and preparation a new interface for biomedical application. The fabrication of PARG-GQDs on GCE was performed using Layer-by-layer regime. Scanning electron microscopy (SEM) was confirmed dispersion of GQDs on the surface of PARG which lead to increase of surface coverage of PARG. The redox behavior of prepared sensor was then characterized by cyclic voltammetry (CV), differential pulse voltammetry (DPV) and chronoamperometry (CHA), square wave voltammetry (SWV), linear sweep voltammetry (LSV). The electroactivity of PARG-GQDs coating towards detection and determination of malondialdehyde (MDA) as one of the most common biomarkers of oxidative stress, was then studied. Then, application of prepared sensor for the detection of MDA in exhaled breath condensate (EBC) is described. Electrochemical based sensor shows the lower limit of quantification (LLOQ) were 0.329nanomolar. This work is the first report on the integration of GQDs to poly amino acids. Further development can lead to monitoring of MDA or other exhaled breath biomarkers by GQDs functionalized poly amino acids in EBC using electrochemical methods. Copyright © 2017. Published by Elsevier B.V.

Characterization of an electrochemical mercury sensor using alternating current, cyclic, square wave and differential pulse voltammetry.

PubMed

Guerreiro, Gabriela V; Zaitouna, Anita J; Lai, Rebecca Y

2014-01-31

Here we report the characterization of an electrochemical mercury (Hg(2+)) sensor constructed with a methylene blue (MB)-modified and thymine-containing linear DNA probe. Similar to the linear probe electrochemical DNA sensor, the resultant sensor behaved as a "signal-off" sensor in alternating current voltammetry and cyclic voltammetry. However, depending on the applied frequency or pulse width, the sensor can behave as either a "signal-off" or "signal-on" sensor in square wave voltammetry (SWV) and differential pulse voltammetry (DPV). In SWV, the sensor showed "signal-on" behavior at low frequencies and "signal-off" behavior at high frequencies. In DPV, the sensor showed "signal-off" behavior at short pulse widths and "signal-on" behavior at long pulse widths. Independent of the sensor interrogation technique, the limit of detection was found to be 10nM, with a linear dynamic range between 10nM and 500nM. In addition, the sensor responded to Hg(2+) rather rapidly; majority of the signal change occurred in <20min. Overall, the sensor retains all the characteristics of this class of sensors; it is reagentless, reusable, sensitive, specific and selective. This study also highlights the feasibility of using a MB-modified probe for real-time sensing of Hg(2+), which has not been previously reported. More importantly, the observed "switching" behavior in SWV and DPV is potentially generalizable and should be applicable to most sensors in this class of dynamics-based electrochemical biosensors. Copyright © 2013 Elsevier B.V. All rights reserved.

Voltammetric determination of tartaric acid in wines by electrocatalytic oxidation on a cobalt(II)-phthalocyanine-modified electrode associated with multiway calibration.

PubMed

Lourenço, Anabel S; Nascimento, Raphael F; Silva, Amanda C; Ribeiro, Williame F; Araujo, Mario C U; Oliveira, Severino C B; Nascimento, Valberes B

2018-05-30

The electrocatalytic oxidation of tartaric acid on a carbon paste electrode modified with cobalt (II)-phthalocyanine was demonstrated and applied to the development of a highly sensitive, simple, fast and inexpensive voltammetric sensor to determine tartaric acid. The electrochemical behavior of the modified electrode was investigated by cyclic and square wave voltammetry, and the effect of experimental variables, such as dispersion and loading of cobalt (II)-phthalocyanine, together with optimum conditions for sensing the analyte by square wave voltammetry were assessed. In addition, the absence of a significant memory effect combined with the ease of electrode preparation led to the development of a sensitive and direct method to determine tartaric acid in wines. Interferences from other low molecular weight organic acids commonly present in wines were circumvented by using a multiway calibration technique, successfully obtaining the second order advantage by modeling voltammetric data with unfolded partial least square with residual bilinearization (U-PLS/RBL). A linear response range between 10 and 100 μmol L -1 (r = 0.9991), a relative prediction error of 4.55% and a recovery range from 96.41 to 102.43% were obtained. The proposed method is non-laborious, since it does not use sample pretreatment such as filtration, extraction, pre-concentration or cleanup procedures. Copyright © 2018 Elsevier B.V. All rights reserved.

Quantitative Determining of Ultra-Trace Aluminum Ion in Environmental Samples by Liquid Phase Microextraction Assisted Anodic Stripping Voltammetry.

PubMed

Zhang, Liuyang; Luo, Jinju; Shen, Xinyu; Li, Chunya; Wang, Xian; Nie, Bei; Fang, Huaifang

2018-05-10

Direct detecting of trace amount Al(III) in aqueous solution by stripping voltammetry is often frustrated by its irreversible reduction, resided at −1.75 V (vs. Ag/AgCl reference), which is in a proximal potential of proton reduction. Here, we described an electroanalytical approach, combined with liquid phase microextraction (LPME) using ionic liquid (IL), to quantitatively assess trace amount aluminum in environmental samples. The Al(III) was caged by 8-hydroxyquinoline, forming a superb hydrophobic metal⁻chelate, which sequentially transfers and concentrates in the bottom layer of IL-phase during LPME. The preconcentrated Al(III) was further analyzed by a square-wave anodic stripping voltammetry (SW-ASV). The resulting Al-deposited electrodes were characterized by scanning electron microscopy and powder X-ray diffraction, showing the intriguing amorphous nanostructures. The method developed provides a linear calibration ranging from 0.1 to 1.2 ng L −1 with a correlation coefficient of 0.9978. The LOD attains as low as 1 pmol L −1 , which reaches the lowest report for Al(III) detection using electroanalytical techniques. The applicable methodology was implemented for monitoring Al(III) in commercial distilled water.

LabVIEW-based sequential-injection analysis system for the determination of trace metals by square-wave anodic and adsorptive stripping voltammetry on mercury-film electrodes.

PubMed

Economou, Anastasios; Voulgaropoulos, Anastasios

2003-01-01

The development of a dedicated automated sequential-injection analysis apparatus for anodic stripping voltammetry (ASV) and adsorptive stripping voltammetry (AdSV) is reported. The instrument comprised a peristaltic pump, a multiposition selector valve and a home-made potentiostat and used a mercury-film electrode as the working electrodes in a thin-layer electrochemical detector. Programming of the experimental sequence was performed in LabVIEW 5.1. The sequence of operations included formation of the mercury film, electrolytic or adsorptive accumulation of the analyte on the electrode surface, recording of the voltammetric current-potential response, and cleaning of the electrode. The stripping step was carried out by applying a square-wave (SW) potential-time excitation signal to the working electrode. The instrument allowed unattended operation since multiple-step sequences could be readily implemented through the purpose-built software. The utility of the analyser was tested for the determination of copper(II), cadmium(II), lead(II) and zinc(II) by SWASV and of nickel(II), cobalt(II) and uranium(VI) by SWAdSV.

LabVIEW-based sequential-injection analysis system for the determination of trace metals by square-wave anodic and adsorptive stripping voltammetry on mercury-film electrodes

PubMed Central

Economou, Anastasios; Voulgaropoulos, Anastasios

2003-01-01

The development of a dedicated automated sequential-injection analysis apparatus for anodic stripping voltammetry (ASV) and adsorptive stripping voltammetry (AdSV) is reported. The instrument comprised a peristaltic pump, a multiposition selector valve and a home-made potentiostat and used a mercury-film electrode as the working electrodes in a thin-layer electrochemical detector. Programming of the experimental sequence was performed in LabVIEW 5.1. The sequence of operations included formation of the mercury film, electrolytic or adsorptive accumulation of the analyte on the electrode surface, recording of the voltammetric current-potential response, and cleaning of the electrode. The stripping step was carried out by applying a square-wave (SW) potential-time excitation signal to the working electrode. The instrument allowed unattended operation since multiple-step sequences could be readily implemented through the purpose-built software. The utility of the analyser was tested for the determination of copper(II), cadmium(II), lead(II) and zinc(II) by SWASV and of nickel(II), cobalt(II) and uranium(VI) by SWAdSV. PMID:18924623

New redox-active layer create via epoxy-amine reaction - The base of genosensor for the detection of specific DNA and RNA sequences of avian influenza virus H5N1.

PubMed

Malecka, Kamila; Stachyra, Anna; Góra-Sochacka, Anna; Sirko, Agnieszka; Zagórski-Ostoja, Włodzimierz; Dehaen, Wim; Radecka, Hanna; Radecki, Jerzy

2015-03-15

This paper concerns the development of a redox-active monolayer and its application for the construction of an electrochemical genosensor designed for the detection of specific DNA and RNA oligonucleotide sequences related to the avian influenza virus (AIV) type H5N1. This new redox layer was created on a gold electrode surface step by step. Cyclic Voltammetry, Osteryoung Square-Wave Voltammetry and Differential Pulse Voltammetry were used for its characterization. This new redox-active layer was applied for the construction of the DNA biosensor. The NH2-NC3 probe (20-mer) was covalently attached to the gold electrode surface via a "click" reaction between the amine and an epoxide group. The hybridization process was monitored using the Osteryoung Square-Wave Voltammetry. The 20-mer DNA and ca. 280-mer RNA oligonucleotides were used as the targets. The constructed genosensor was capable to determine complementary oligonucleotide sequences with a detection limit in the pM range. It is able to distinguish the different position of the part RNA complementary to the DNA probe. The genosensor was very selective. The 20-mer DNA as well as the 280-mer RNA oligonucleotides without a complementary sequence generated a weak signal. Copyright © 2014 Elsevier B.V. All rights reserved.

Cyclic voltammetry deposition of copper nanostructure on MWCNTs modified pencil graphite electrode: An ultra-sensitive hydrazine sensor.

PubMed

Heydari, Hamid; Gholivand, Mohammad B; Abdolmaleki, Abbas

2016-09-01

In this study, Copper (Cu) nanostructures (CuNS) were electrochemically deposited on a film of multiwall carbon nanotubes (MWCNTs) modified pencil graphite electrode (MWCNTs/PGE) by cyclic voltammetry method to fabricate a CuNS-MWCNTs composite sensor (CuNS-MWCNT/PGE) for hydrazine detection. Scanning electron microscopy (SEM) and Energy-dispersive X-ray spectroscopy (EDX) were used for the characterization of CuNS on the MWCNTs matrix. The composite of CuNS-MWCNTs was characterized with cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). The preliminary studies showed that the proposed sensor have a synergistic electrocatalytic activity for the oxidation of hydrazine in phosphate buffer. The catalytic currents of square wave voltammetry had a linear correlation with the hydrazine concentration in the range of 0.1 to 800μM with a low detection limit of 70nM. Moreover, the amperometric oxidation current exhibited a linear correlation with hydrazine concentration in the concentration range of 50-800μM with the detection limit of 4.3μM. The proposed electrode was used for the determination of hydrazine in real samples and the results were promising. Empirical results also indicated that the sensor had good reproducibility, long-term stability, and the response of the sensor to hydrazine was free from interferences. Moreover, the proposed sensor benefits from simple preparation, low cost, outstanding sensitivity, selectivity, and reproducibility for hydrazine determination. Copyright © 2016. Published by Elsevier B.V.

Anodic stripping voltammetry with gold electrodes as an alternative method for the routine determination of mercury in fish. Comparison with spectroscopic approaches.

PubMed

Giacomino, Agnese; Ruo Redda, Andrea; Squadrone, Stefania; Rizzi, Marco; Abete, Maria Cesarina; La Gioia, Carmela; Toniolo, Rosanna; Abollino, Ornella; Malandrino, Mery

2017-04-15

The applicability to the determination of mercury in tuna of square wave anodic stripping voltammetry (SW-ASV) conducted at both solid gold electrode (SGE) and a gold nanoparticle-modified glassy carbon electrode (AuNPs-GCE) was demonstrated. Mercury content in two certified materials and in ten samples of canned tuna was measured. The performances of the electrodes were compared with one another as well as with two spectroscopic techniques, namely cold vapour atomic absorption spectroscopy (CV-AAS) and a direct mercury analyser (DMA). The results found pointed out that both SW-ASV approaches were suitable and easy-to-use method to monitor mercury concentration in tunas, since they allowed accurate quantification at concentration values lower than the maximum admissible level in this matrix ([Hg]=1mg/kg wet weight,ww ). In particular, mercury detection at the AuNPs-GCE showed a LOQ in fish-matrix of 0.1μg/l, corresponding to 0.06mg/kg ww , with performance comparable to that of DMA. Copyright © 2016 Elsevier Ltd. All rights reserved.

Voltammetric pH sensing using carbon electrodes: glassy carbon behaves similarly to EPPG.

PubMed

Lu, Min; Compton, Richard G

2014-09-21

Developing and building on recent work based on a simple sensor for pH determination using unmodified edge plane pyrolytic graphite (EPPG) electrodes, we present a voltammetric method for pH determination using a bare unmodified glassy carbon (GC) electrode. By exploiting the pH sensitive nature of quinones present on carbon edge-plane like sites within the GC, we show how GC electrodes can be used to measure pH. The electro-reduction of surface quinone groups on the glassy carbon electrode was characterised using cyclic voltammetry (CV) and optimised with square-wave voltammetry (SWV) at 298 K and 310 K. At both temperatures, a linear correlation was observed, corresponding to a 2 electron, 2 proton Nernstian response over the aqueous pH range 1.0 to 13.1. As such, unmodified glassy carbon electrodes are seen to be pH dependent, and the Nernstian response suggests its facile use for pH sensing. Given the widespread use of glassy carbon electrodes in electroanalysis, the approach offers a method for the near-simultaneous measurement and monitoring of pH during such analyses.

Thermal, structural and electrochemical properties of new aliphatic-aromatic imine with piperazine moieties blended with titanium dioxide

NASA Astrophysics Data System (ADS)

Różycka, Anna; Fryń, Patryk; Iwan, Agnieszka; Bogdanowicz, Krzysztof Artur; Filapek, Michal; Górska, Natalia; Dąbczyński, Paweł; Rysz, Jakub; Pociecha, Damian; Hreniak, Agnieszka; Marzec, Monika

2018-02-01

A new piperazine imine, (7E)-N-((4-((E)-(4-hexadecylphenylimino)methyl)piperazin-1-yl)methylene)-4-dodecylbenzenamine, has been synthesized by the condensation of 1,4-piperazinedicarboxaldehyde with 4-hexadecylaniline. The imine was characterized by cyclic voltammetry, Fourier transform middle-infrared absorption spectroscopy and X-ray diffraction. Thermal properties of imine was analyzed by differential scanning calorimetry method during first and second heating scan at 10 and 20 °C/min. Texture of imine was investigated by polarized optical microscopy and atomic force microscopy. Furthermore, imine was blended with titanium dioxide in anatase form and fully characterized by the same methods. Piperazine imine and its mixture with titanium dioxide exhibited only a transition from crystal to isotropic state. Imine exhibits two-step reduction wave attributed to one-electron transfer in each step as was found by cyclic voltammetry. Both titanium dioxide and poly(3-hexylthiophene) change the electrochemical properties of piperazine imine, however, in different ways. Studied imine blended with titanium dioxide exhibited higher value of energy band gap than pure piperazine imine and lower Eg than pure poly(3-hexylthiophene).

Fully printed flexible and disposable wireless cyclic voltammetry tag.

PubMed

Jung, Younsu; Park, Hyejin; Park, Jin-Ah; Noh, Jinsoo; Choi, Yunchang; Jung, Minhoon; Jung, Kyunghwan; Pyo, Myungho; Chen, Kevin; Javey, Ali; Cho, Gyoujin

2015-01-29

A disposable cyclic voltammetry (CV) tag is printed on a plastic film by integrating wireless power transmitter, polarized triangle wave generator, electrochemical cell and signage through a scalable gravure printing method. By proximity of 13.56 MHz RF reader, the printed CV tag generates 320 mHz of triangular sweep wave from +500 mV to -500 mV which enable to scan a printed electrochemical cell in the CV tag. By simply dropping any specimen solution on the electrochemical cell in the CV tag, the presence of solutes in the solution can be detected and shown on the signage of the CV tag in five sec. 10 mM of N,N,N',N'-tetramethyl-p-phenylenediamine (TMPD) was used as a standard solute to prove the working concept of fully printed disposable wireless CV tag. Within five seconds, we can wirelessly diagnose the presence of TMPD in the solution using the CV tag in the proximity of the 13.56 MHz RF reader. This fully printed and wirelessly operated flexible CV tag is the first of its kind and marks the path for the utilization of inexpensive and disposable wireless electrochemical sensor systems for initial diagnose hazardous chemicals and biological molecules to improve public hygiene and health.

Fully printed flexible and disposable wireless cyclic voltammetry tag

PubMed Central

Jung, Younsu; Park, Hyejin; Park, Jin-Ah; Noh, Jinsoo; Choi, Yunchang; Jung, Minhoon; Jung, Kyunghwan; Pyo, Myungho; Chen, Kevin; Javey, Ali; Cho, Gyoujin

2015-01-01

A disposable cyclic voltammetry (CV) tag is printed on a plastic film by integrating wireless power transmitter, polarized triangle wave generator, electrochemical cell and signage through a scalable gravure printing method. By proximity of 13.56 MHz RF reader, the printed CV tag generates 320 mHz of triangular sweep wave from +500 mV to −500 mV which enable to scan a printed electrochemical cell in the CV tag. By simply dropping any specimen solution on the electrochemical cell in the CV tag, the presence of solutes in the solution can be detected and shown on the signage of the CV tag in five sec. 10 mM of N,N,N′,N′-tetramethyl-p-phenylenediamine (TMPD) was used as a standard solute to prove the working concept of fully printed disposable wireless CV tag. Within five seconds, we can wirelessly diagnose the presence of TMPD in the solution using the CV tag in the proximity of the 13.56 MHz RF reader. This fully printed and wirelessly operated flexible CV tag is the first of its kind and marks the path for the utilization of inexpensive and disposable wireless electrochemical sensor systems for initial diagnose hazardous chemicals and biological molecules to improve public hygiene and health. PMID:25630250

Fully printed flexible and disposable wireless cyclic voltammetry tag

NASA Astrophysics Data System (ADS)

Jung, Younsu; Park, Hyejin; Park, Jin-Ah; Noh, Jinsoo; Choi, Yunchang; Jung, Minhoon; Jung, Kyunghwan; Pyo, Myungho; Chen, Kevin; Javey, Ali; Cho, Gyoujin

2015-01-01

A disposable cyclic voltammetry (CV) tag is printed on a plastic film by integrating wireless power transmitter, polarized triangle wave generator, electrochemical cell and signage through a scalable gravure printing method. By proximity of 13.56 MHz RF reader, the printed CV tag generates 320 mHz of triangular sweep wave from +500 mV to -500 mV which enable to scan a printed electrochemical cell in the CV tag. By simply dropping any specimen solution on the electrochemical cell in the CV tag, the presence of solutes in the solution can be detected and shown on the signage of the CV tag in five sec. 10 mM of N,N,N',N'-tetramethyl-p-phenylenediamine (TMPD) was used as a standard solute to prove the working concept of fully printed disposable wireless CV tag. Within five seconds, we can wirelessly diagnose the presence of TMPD in the solution using the CV tag in the proximity of the 13.56 MHz RF reader. This fully printed and wirelessly operated flexible CV tag is the first of its kind and marks the path for the utilization of inexpensive and disposable wireless electrochemical sensor systems for initial diagnose hazardous chemicals and biological molecules to improve public hygiene and health.

Electrochemical study of ricin at glassy carbon electrode.

PubMed

Ribeiro, Williame F; da Costa, Daniel J E; Lourenço, Anabel S; Lopes, Ilanna C; de Medeiros, Everaldo P; Salazar-Banda, Giancarlo R; do Nascimento, Valberes B; de Araújo, Mário C U

2013-08-21

Ricin, Ricinus communis agglutinin 60 - RCA 60, is a deadly phytotoxic protein which inhibits ribosomes (class II), and there is no known effective antidote in living organisms. Ricin is composed of two polypeptide chains, A and B, linked covalently by a single disulfide bond. The analytical methods for the detection of RCA 60 are commonly laborious, expensive, require skilled labor, and involve sophisticated equipment. Aimed at the development of electroanalytical methods for RCA 60 detection, here we studied the electrochemical oxidation of RCA 60 on a glassy carbon (GC) electrode over a wide pH range, using cyclic voltammetry, differential pulse voltammetry (DPV) and square wave voltammetry (SWV). Two quasi-reversible electrochemical RCA 60 oxidation peaks were identified on the GC electrode by SWV. For values of 2.2 ≤ pH ≤ 10.2, DPV studies revealed that the peak potentials, EP1 and EP2, display a linear dependence with pH and the reaction mechanism involves the transfer of 2H⁺/2e⁻ (peak 1) and 1H⁺/1e⁻ (peak 2). The first and second RCA 60 oxidation steps may correspond to the oxidation of cysteine and tyrosine-tryptophan residues, respectively. The oxidation product of the second RCA 60 oxidation step appears at 7.0 ≤ pH ≤ 11.8. For pH ≥ 10.2, both processes are pH independent, resulting in a pKa of ca. 10.2. A third RCA 60 oxidation peak only appears at acidic pH. RCA 60 samples extracted from different castor seed cultivars showed similar electrochemical behavior, enabling the implementation of an analytical voltammetric method.

Fabrication strategies, sensing modes and analytical applications of ratiometric electrochemical biosensors.

PubMed

Jin, Hui; Gui, Rijun; Yu, Jianbo; Lv, Wei; Wang, Zonghua

2017-05-15

Previously developed electrochemical biosensors with single-electric signal output are probably affected by intrinsic and extrinsic factors. In contrast, the ratiometric electrochemical biosensors (RECBSs) with dual-electric signal outputs have an intrinsic built-in correction to the effects from system or background electric signals, and therefore exhibit a significant potential to improve the accuracy and sensitivity in electrochemical sensing applications. In this review, we systematically summarize the fabrication strategies, sensing modes and analytical applications of RECBSs. First, the different fabrication strategies of RECBSs were introduced, referring to the analytes-induced single- and dual-dependent electrochemical signal strategies for RECBSs. Second, the different sensing modes of RECBSs were illustrated, such as differential pulse voltammetry, square wave voltammetry, cyclic voltammetry, alternating current voltammetry, electrochemiluminescence, and so forth. Third, the analytical applications of RECBSs were discussed based on the types of target analytes. Finally, the forthcoming development and future prospects in the research field of RECBSs were also highlighted. Copyright © 2017 Elsevier B.V. All rights reserved.

Development of a sequential injection-square wave voltammetry method for determination of paraquat in water samples employing the hanging mercury drop electrode.

PubMed

dos Santos, Luciana B O; Infante, Carlos M C; Masini, Jorge C

2010-03-01

This work describes the development and optimization of a sequential injection method to automate the determination of paraquat by square-wave voltammetry employing a hanging mercury drop electrode. Automation by sequential injection enhanced the sampling throughput, improving the sensitivity and precision of the measurements as a consequence of the highly reproducible and efficient conditions of mass transport of the analyte toward the electrode surface. For instance, 212 analyses can be made per hour if the sample/standard solution is prepared off-line and the sequential injection system is used just to inject the solution towards the flow cell. In-line sample conditioning reduces the sampling frequency to 44 h(-1). Experiments were performed in 0.10 M NaCl, which was the carrier solution, using a frequency of 200 Hz, a pulse height of 25 mV, a potential step of 2 mV, and a flow rate of 100 µL s(-1). For a concentration range between 0.010 and 0.25 mg L(-1), the current (i(p), µA) read at the potential corresponding to the peak maximum fitted the following linear equation with the paraquat concentration (mg L(-1)): i(p) = (-20.5 ± 0.3)C (paraquat) - (0.02 ± 0.03). The limits of detection and quantification were 2.0 and 7.0 µg L(-1), respectively. The accuracy of the method was evaluated by recovery studies using spiked water samples that were also analyzed by molecular absorption spectrophotometry after reduction of paraquat with sodium dithionite in an alkaline medium. No evidence of statistically significant differences between the two methods was observed at the 95% confidence level.

Lead detection using micro/nanocrystalline boron-doped diamond by square-wave anodic stripping voltammetry.

PubMed

Arantes, Tatiane M; Sardinha, André; Baldan, Mauricio R; Cristovan, Fernando H; Ferreira, Neidenei G

2014-10-01

Monitoring heavy metal ion levels in water is essential for human health and safety. Electroanalytical techniques have presented important features to detect toxic trace heavy metals in the environment due to their high sensitivity associated with their easy operational procedures. Square-wave voltammetry is a powerful electrochemical technique that may be applied to both electrokinetic and analytical measurements, and the analysis of the characteristic parameters of this technique also enables the mechanism and kinetic evaluation of the electrochemical process under study. In this work, we present a complete optimized study on the heavy metal detection using diamond electrodes. It was analyzed the influence of the morphology characteristics as well as the doping level on micro/nanocrystalline boron-doped diamond films by means of square-wave anodic stripping voltammetry (SWASV) technique. The SWASV parameters were optimized for all films, considering that their kinetic response is dependent on the morphology and/or doping level. The films presented reversible results for the Lead [Pb (II)] system studied. The Pb (II) analysis was performed in ammonium acetate buffer at pH 4.5, varying the lead concentration in the range from 1 to 10 μg L(-1). The analytical responses were obtained for the four electrodes. However, the best low limit detection and reproducibility was found for boron doped nanocrystalline diamond electrodes (BDND) doped with 2000 mg L(-1) in B/C ratio. Copyright © 2014 Elsevier B.V. All rights reserved.

Non-conductive nanomaterial enhanced electrochemical response in stripping voltammetry: The use of nanostructured magnesium silicate hollow spheres for heavy metal ions detection.

PubMed

Xu, Ren-Xia; Yu, Xin-Yao; Gao, Chao; Jiang, Yu-Jing; Han, Dong-Dong; Liu, Jin-Huai; Huang, Xing-Jiu

2013-08-06

Nanostructured magnesium silicate hollow spheres, one kind of non-conductive nanomaterials, were used in heavy metal ions (HMIs) detection with enhanced performance for the first time. The detailed study of the enhancing electrochemical response in stripping voltammetry for simultaneous detection of ultratrace Cd(2+), Pb(2+), Cu(2+) and Hg(2+) was described. Electrochemical properties of modified electrodes were characterized by cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). The operational parameters which have influence on the deposition and stripping of metal ions, such as supporting electrolytes, pH value, and deposition time were carefully studied. The anodic stripping voltammetric performance toward HMIs was evaluated using square wave anodic stripping voltammetry (SWASV) analysis. The detection limits achieved (0.186nM, 0.247nM, 0.169nM and 0.375nM for Cd(2+), Pb(2+), Cu(2+) and Hg(2+)) are much lower than the guideline values in drinking water given by the World Health Organization (WHO). In addition, the interference and stability of the modified electrode were also investigated under the optimized conditions. An interesting phenomenon of mutual interference between different metal ions was observed. Most importantly, the sensitivity of Pb(2+) increased in the presence of certain concentrations of other metal ions, such as Cd(2+), Cu(2+) and Hg(2+) both individually and simultaneously. The proposed electrochemical sensing method is thus expected to open new opportunities to broaden the use of SWASV in analysis for detecting HMIs in the environment. Copyright © 2013 Elsevier B.V. All rights reserved.

Biosensors for hepatitis B virus detection.

PubMed

Yao, Chun-Yan; Fu, Wei-Ling

2014-09-21

A biosensor is an analytical device used for the detection of analytes, which combines a biological component with a physicochemical detector. Recently, an increasing number of biosensors have been used in clinical research, for example, the blood glucose biosensor. This review focuses on the current state of biosensor research with respect to efficient, specific and rapid detection of hepatitis B virus (HBV). The biosensors developed based on different techniques, including optical methods (e.g., surface plasmon resonance), acoustic wave technologies (e.g., quartz crystal microbalance), electrochemistry (amperometry, voltammetry and impedance) and novel nanotechnology, are also discussed.

Simultaneous voltammetric determination of prednisone and prednisolone in human body fluids.

PubMed

Goyal, Rajendra N; Bishnoi, Sunita

2009-08-15

A sensitive, rapid and reliable electrochemical method based on voltammetry at single wall carbon nanotube (SWNT) modified edge plane pyrolytic graphite electrode (EPPGE) is proposed for the simultaneous determination of prednisolone and prednisone in human body fluids and pharmaceutical preparations. The electrochemical response of both the drugs was evaluated by osteryoung square wave voltammetry (OSWV) in phosphate buffer medium of pH 7.2. The modified electrode exhibited good electrocatalytic properties towards prednisone and prednisolone reduction with a peak potential of approximately -1230 and approximately -1332 mV respectively. The concentration versus peak current plots were linear for both the analytes in the range 0.01-100 microM and the detection limit (3 sigma/slope) observed for prednisone and prednisolone were 0.45 x 10(-8), 0.90 x 10(-8)M, respectively. The results of the quantitative estimation of prednisone and prednisolone in biological fluids were also compared with HPLC and the results were in good agreement.

Pulse-voltammetric glucose detection at gold junction electrodes.

PubMed

Rassaei, Liza; Marken, Frank

2010-09-01

A novel glucose sensing concept based on the localized change or "modulation" in pH within a symmetric gold-gold junction electrode is proposed. A paired gold-gold junction electrode (average gap size ca. 500 nm) is prepared by simultaneous bipotentiostatic electrodeposition of gold onto two closely spaced platinum disk electrodes. For glucose detection in neutral aqueous solution, the potential of the "pH-modulator" electrode is set to -1.5 V vs saturated calomel reference electrode (SCE) to locally increase the pH, and simultaneously, either cyclic voltammetry or square wave voltammetry experiments are conducted at the sensor electrode. A considerable improvement in the sensor electrode response is observed when a normal pulse voltammetry sequence is applied to the modulator electrode (to generate "hydroxide pulses") and the glucose sensor electrode is operated with fixed bias at +0.5 V vs SCE (to eliminate capacitive charging currents). Preliminary data suggest good linearity for the glucose response in the medically relevant 1-10 mM concentration range (corresponding to 0.18-1.8 g L(-1)). Future electroanalytical applications of multidimensional pulse voltammetry in junction electrodes are discussed.

Novel electrochemical biosensor based on PVP capped CoFe2O4@CdSe core-shell nanoparticles modified electrode for ultra-trace level determination of rifampicin by square wave adsorptive stripping voltammetry.

PubMed

Asadpour-Zeynali, Karim; Mollarasouli, Fariba

2017-06-15

This work introduces a new electrochemical sensor based on polyvinyl pyrrolidone capped CoFe 2 O 4 @CdSe core-shell modified electrode for a rapid detection and highly sensitive determination of rifampicin (RIF) by square wave adsorptive stripping voltammetry. The new PVP capped CoFe 2 O 4 @CdSe with core-shell nanostructure was synthesized by a facile synthesis method for the first time. PVP can act as a capping and etching agent for protection of the outer surface nanoparticles and formation of a mesoporous shell, respectively. Another important feature of this work is the choice of the ligand (1,10-phenanthroline) for precursor cadmium complex that works as a chelating agent in order to increase optical and electrical properties and stability of prepared nanomaterial. The nanoparticles have been characterized by field emission scanning electron microscopy (FESEM), transmission electron microscope (TEM), energy dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), UV-vis, photoluminescence (PL) spectroscopy, FT-IR, and cyclic voltammetry techniques. The PL spectroscopy study of CoFe 2 O 4 @CdSe has shown significant PL quenching by the formation of CoFe 2 O 4 core inside CdSe, this shows that CoFe 2 O 4 NPs are efficient electron acceptors with the CdSe. It is clearly observed that the biosensor can significantly enhance electrocatalytic activity towards the oxidation of RIF, under the optimal conditions. The novelty of this work arises from the new synthesis method for the core-shell of CoFe 2 O 4 @CdSe. Then, the novel electrochemical biosensor was fabricated for ultra-trace level determination of rifampicin with very low detection limit (4.55×10 -17 M) and a wide linear range from 1.0×10 -16 to 1.0×10 -7 M. The fabricated biosensor showed high sensitivity and selectivity, good reproducibility and stability. Therefore, it was successfully applied for the determination of ultra-trace RIF amounts in biological and pharmaceutical samples with satisfactory recovery data. Copyright © 2016 Elsevier B.V. All rights reserved.

Determination of tryptamine in foods using square wave adsorptive stripping voltammetry.

PubMed

Costa, Daniel J E; Martínez, Ana M; Ribeiro, Williame F; Bichinho, Kátia M; Di Nezio, María Susana; Pistonesi, Marcelo F; Araujo, Mario C U

2016-07-01

Tryptamine, a biogenic amine, is an indole derivative with an electrophilic substituent at the C3 position of the pyrrole ring of the indole moiety. The electrochemical oxidation of tryptamine was investigated using glassy carbon electrode (GCE), and focusing on trace level determination in food products by square wave adsorptive stripping voltammetry (SWAdSV). The electrochemical responses of tryptamine were evaluated using differing voltammetric techniques over a wide pH range, a quasi-reversible electron-transfer to redox system represented by coupled peaks P1-P3, and an irreversible reaction for peak P2 were demonstrated. The proton and electron counts associated with the oxidation reactions were estimated. The nature of the mass transfer process was predominantly diffusion-limited for the oxidation process of P1, the most selective and sensitive analytical response (acetate buffer solution pH 5.3), being used for the development of SWAdSV method, under optimum conditions. The excellent response allowed the development of an electroanalytical method with a linear response range of from 4.7-54.5)×10(-)(8)molL(-1), low detection limit (0.8×10(-)(9)molL(-)(1)), and quantification limit (2.7×10(-9)molL(-1)), and acceptable levels of repeatability (3.6%), and reproducibility (3.8%). Tryptamine content was determined in bananas, tomatoes, cheese (mozzarella and gorgonzola), and cold meats (chicken sausage and pepperoni sausage), yielding recoveries above 90%, with excellent analytical performance using simple and low cost instrumentation. Copyright © 2016 Elsevier B.V. All rights reserved.

Eletrochemical reduction of patulin and 5-hydroxymethylfurfural in both neutral and acid non-aqueous media. Their electroanalytical determination in apple juices.

PubMed

Damián Chanique, Gerardo; Heraldo Arévalo, Alejandro; Alicia Zon, María; Fernández, Héctor

2013-07-15

The electro-reduction of patulin mycotoxin and 5-hydroxymethylfurfural at glassy carbon electrodes in acetonitrile +0.1 mol L(-1) tetrabutylammonium perchlorate, in both the absence and the presence of different aliquots of trifluoroacetic acid is reported. 5-hydroxymethylfurfural is the most common interference in the determination of patulin in products derived from apples. The electrochemical techniques were cyclic and square wave voltammetries, and controlled potential bulk electrolysis. The number of electrons exchanged in the patulin electro-reduction of n=1 could be inferred from controlled potential bulk electrolysis measurements. Ultraviolet-visible and infrared spectroscopies were used to identify patulin electro-reduction product/s. A value of (2.1±0.1)×10(-5) cm(2) s(-1) for the patulin diffusion coefficient was calculated from convoluted cyclic voltammograms. A method based on square wave voltammetry was developed for the quantitative determination of patulin in both fresh, and commercial apple juices in the presence of 5-hydroxymethylfurfural. Calibration curves obtained from solutions of the commercial reagent, and commercial apple juices were linear in the range from 3.0×10(-7) to 2.2×10(-5) mol L(-1). The lowest concentration measured experimentally for a signal to noise ratio of 3:1 was 3×10(-7) mol L(-1) (45 ppb) and a recovery percent of 84% was determined for commercial apple juices. This electroanalytical methodology appears as a good screening method for the determination of patulin in apple juices. Copyright © 2013 Elsevier B.V. All rights reserved.

Simultaneous voltammetric determination of dopamine and epinephrine in human body fluid samples using a glassy carbon electrode modified with nickel oxide nanoparticles and carbon nanotubes within a dihexadecylphosphate film.

PubMed

Figueiredo-Filho, Luiz C S; Silva, Tiago A; Vicentini, Fernando C; Fatibello-Filho, Orlando

2014-06-07

A simple and highly selective electrochemical method was developed for the single or simultaneous determination of dopamine (DA) and epinephrine (EP) in human body fluids using a glassy carbon electrode modified with nickel oxide nanoparticles and carbon nanotubes within a dihexadecylphosphate film using square-wave voltammetry (SWV) or differential-pulse voltammetry (DPV). Using DPV with the proposed electrode, a separation of ca. 360 mV between the peak reduction potentials of DA and EP present in binary mixtures was obtained. The analytical curves for the simultaneous determination of dopamine and epinephrine showed an excellent linear response, ranging from 7.0 × 10(-8) to 4.8 × 10(-6) and 3.0 × 10(-7) to 9.5 × 10(-6) mol L(-1) for DA and EP, respectively. The detection limits for the simultaneous determination of DA and EP were 5.0 × 10(-8) mol L(-1) and 8.2 × 10(-8) mol L(-1), respectively. The proposed method was successfully applied in the simultaneous determination of these analytes in human body fluid samples of cerebrospinal fluid, human serum and lung fluid.

Portable Lock-in Amplifier-Based Electrochemical Method to Measure an Array of 64 Sensors for Point-of-Care Applications.

PubMed

Hrdý, Radim; Kynclová, Hana; Klepáčová, Ivana; Bartošík, Martin; Neužil, Pavel

2017-09-05

We present a portable lock-in amplifier-based electrochemical sensing system. The basic unit (cluster) consists of four electrochemical cells (EC), each containing one pseudoreference electrode (PRE) and one working electrode (WE). All four ECs are simultaneously interrogated, each at different frequencies, with square wave pulses superposed on a sawtooth signal for cyclic voltammetry (CV). Lock-in amplification provides independent read-out of four signals, with excellent noise suppression. We expanded a single cluster system into an array of 16 clusters by using electronic switches. The chip with an array of ECs was fabricated using planar technology with a gap between a WE and a PRE of ≈2 μm, which results in partial microelectrode-type behavior. The basic electrode characterization was performed with the model case using a ferricyanide-ferrocyanide redox couple (Fe 2+ /Fe 3+ ) reaction, performing CV and differential pulse voltammetry (DPV). We then used this system to perform cyclic lock-in voltammetry (CLV) to measure concurrently responses of the four ECs. We repeated this method with all 64 ECs on the chip. The standard deviation of a peak oxidation and reduction current in a single channel consisting of 13 ECs was ≈7.46% and ≈5.6%, respectively. The four-EC configuration in each measured spot allows determination of nonperforming ECs and, thus, to eliminate potential false results. This system is built in a portable palm-size format suitable for point-of-care applications. It can perform either individual or multiple measurements of active compounds, such as biomarkers.

Universal mobile electrochemical detector designed for use in resource-limited applications

PubMed Central

Nemiroski, Alex; Christodouleas, Dionysios C.; Hennek, Jonathan W.; Kumar, Ashok A.; Maxwell, E. Jane; Fernández-Abedul, Maria Teresa; Whitesides, George M.

2014-01-01

This paper describes an inexpensive, handheld device that couples the most common forms of electrochemical analysis directly to “the cloud” using any mobile phone, for use in resource-limited settings. The device is designed to operate with a wide range of electrode formats, performs on-board mixing of samples by vibration, and transmits data over voice using audio—an approach that guarantees broad compatibility with any available mobile phone (from low-end phones to smartphones) or cellular network (second, third, and fourth generation). The electrochemical methods that we demonstrate enable quantitative, broadly applicable, and inexpensive sensing with flexibility based on a wide variety of important electroanalytical techniques (chronoamperometry, cyclic voltammetry, differential pulse voltammetry, square wave voltammetry, and potentiometry), each with different uses. Four applications demonstrate the analytical performance of the device: these involve the detection of (i) glucose in the blood for personal health, (ii) trace heavy metals (lead, cadmium, and zinc) in water for in-field environmental monitoring, (iii) sodium in urine for clinical analysis, and (iv) a malarial antigen (Plasmodium falciparum histidine-rich protein 2) for clinical research. The combination of these electrochemical capabilities in an affordable, handheld format that is compatible with any mobile phone or network worldwide guarantees that sophisticated diagnostic testing can be performed by users with a broad spectrum of needs, resources, and levels of technical expertise. PMID:25092346

Simultaneous voltammetry detection of dopamine and uric acid in human serum and urine with a poly(procaterol hydrochloride) modified glassy carbon electrode.

PubMed

Kong, Dexian; Zhuang, Qizhao; Han, Yejian; Xu, Lanping; Wang, Zeming; Jiang, Lili; Su, Jinwei; Lu, Chun-Hua; Chi, Yuwu

2018-08-01

In the present study, procaterol hydrochloride (ProH) was successfully electropolymerized onto a glass carbon electrode (GCE) with simply cyclic voltammetry scans to construct a poly(procaterol hydrochloride) (p-ProH) membrane modified electrode. Compared with the bare GCE, much higher oxidation peak current responses and better peak potentials separation could be obtained for the simultaneous oxidation of dopamine (DA) and uric acid (UA), owning to the excellent electrocatalytic ability of the p-ProH membrane. And it's based on that a square wave voltammetry (SWV) method was developed to selective and simultaneous measurement of DA and UA. Under the optimum conditions, the linear dependence of oxidation peak current on analyte concentrations were found to be 1.0-100 μmol/L and 2-100 μmol/L, giving detection limits of 0.3 μmol/L and 0.5 μmol/L for DA and UA, separately. The as prepared modified electrode shows simplicity in construction with the merits of good reproducibility, high stability, passable selectivity and nice sensitivity. Finally, the proposed p-ProH membrane modified electrode was successfully devoted to the detection of DA and UA in biological fluids such as human serum and urine with acceptable results. Copyright © 2018 Elsevier B.V. All rights reserved.

Modified Carbon Nanotube Paste Electrode for Voltammetric Determination of Carbidopa, Folic Acid, and Tryptophan

PubMed Central

Esfandiari Baghbamidi, Sakineh; Beitollahi, Hadi; Karimi-Maleh, Hassan; Soltani-Nejad, Somayeh; Soltani-Nejad, Vahhab; Roodsaz, Sara

2012-01-01

A simple and convenient method is described for voltammetric determination of carbidopa (CD), based on its electrochemical oxidation at a modified multiwall carbon nanotube paste electrode. Under optimized conditions, the proposed method exhibited acceptable analytical performances in terms of linearity (over the concentration range from 0.1 to 700.0 μM), detection limit (65.0 nM), and reproducibility (RSD = 2.5%) for a solution containing CD. Also, square wave voltammetry (SWV) was used for simultaneous determination of CD, folic acid (FA), and tryptophan (TRP) at the modified electrode. To further validate its possible application, the method was used for the quantification of CD, FA, and TRP in urine samples. PMID:22666634

Facile and quantitative electrochemical detection of yeast cell apoptosis

NASA Astrophysics Data System (ADS)

Yue, Qiulin; Xiong, Shiquan; Cai, Dongqing; Wu, Zhengyan; Zhang, Xin

2014-03-01

An electrochemical method based on square wave anodic stripping voltammetry (SWASV) was developed to detect the apoptosis of yeast cells conveniently and quantitatively through the high affinity between Cu2+ and phosphatidylserine (PS) translocated from the inner to the outer plasma membrane of the apoptotic cells. The combination of negatively charged PS and Cu2+ could decrease the electrochemical response of Cu2+ on the electrode. The results showed that the apoptotic rates of cells could be detected quantitatively through the variations of peak currents of Cu2+ by SWASV, and agreed well with those obtained through traditional flow cytometry detection. This work thus may provide a novel, simple, immediate and accurate detection method for cell apoptosis.

Tungsten oxide-Au nanosized film composites for glucose oxidation and sensing in neutral medium

PubMed Central

Gougis, Maxime; Ma, Dongling; Mohamedi, Mohamed

2015-01-01

In this work, we report for the first time the use of tungsten oxide (WOx) as catalyst support for Au toward the direct electrooxidation of glucose. The nanostructured WOx/Au electrodes were synthesized by means of laser-ablation technique. Both micro-Raman spectroscopy and transmission electron microscopy showed that the produced WOx thin film is amorphous and made of ultrafine particles of subnanometer size. X-ray diffraction and X-ray photoelectron spectroscopy revealed that only metallic Au was present at the surface of the WOx/Au composite, suggesting that the WOx support did not alter the electronic structure of Au. The direct electrocatalytic oxidation of glucose in neutral medium such as phosphate buffered saline (pH 7.2) solution has been investigated with cyclic voltammetry, chronoamperometry, and square-wave voltammetry. Sensitivity as high as 65.7 μA cm−2 mM−1 up to 10 mM of glucose and a low detection limit of 10 μM were obtained with square-wave voltammetry. This interesting analytical performance makes the laser-fabricated WOx/Au electrode potentially promising for implantable glucose fuel cells and biomedical analysis as the evaluation of glucose concentration in biological fluids. Finally, owing to its unique capabilities proven in this work, it is anticipated that the laser-ablation technique will develop as a fabrication tool for chip miniature-sized sensors in the near future. PMID:25931820

Disposable DNA biosensor with the carbon nanotubes-polyethyleneimine interface at a screen-printed carbon electrode for tests of DNA layer damage by quinazolines.

PubMed

Galandová, Júlia; Ovádeková, Renáta; Ferancová, Adriana; Labuda, Ján

2009-06-01

A screen-printed carbon working electrode within a commercially available screen-printed three-electrode assembly was modified by using a composite of multiwalled carbon nanotubes (MWCNT) dispersed in polyethylenimine (PEI) followed by covering with the calf thymus dsDNA layer. Several electrochemical methods were used to characterize the biosensor and to evaluate damage to the surface-attached DNA: square wave voltammetry of the [Ru(bpy)(3)](2+) redox indicator and mediator of the guanine moiety oxidation, cyclic voltammetry and electrochemical impedance spectroscopy in the presence of the [Fe(CN)(6)](3-/4-) indicator in solution. Due to high electroconductivity and large surface area of MWCNT and positive charge of PEI, the MWCNT-PEI composite is an advantageous platform for the DNA immobilization by the polyelectrolyte complexation and its voltammetric and impedimetric detection. In this respect, the MWCNT-PEI interface exhibited better properties than the MWCNT-chitosan one reported from our laboratory previously. A deep DNA layer damage at incubation of the biosensor in quinazoline solution was found, which depends on the quinazoline concentration and incubation time.

Voltammetric determination of homocysteine using multiwall carbon nanotube paste electrode in the presence of chlorpromazine as a mediator.

PubMed

Gholami-Orimi, Fathali; Taleshi, Farshad; Biparva, Pourya; Karimi-Maleh, Hassan; Beitollahi, Hadi; Ebrahimi, Hamid R; Shamshiri, Mohamad; Bagheri, Hasan; Fouladgar, Masoud; Taherkhani, Ali

2012-01-01

We propose chlorpromazine (CHP) as a new mediator for the rapid, sensitive, and highly selective voltammetric determination of homocysteine (Hcy) using multiwall carbon nanotube paste electrode (MWCNTPE). The experimental results showed that the carbon nanotube paste electrode has a highly electrocatalytic activity for the oxidation of Hcy in the presence of CHP as a mediator. Cyclic voltammetry, double potential step chronoamperometry, and square wave voltammetry (SWV) are used to investigate the suitability of CHP at the surface of MWCNTPE as a mediator for the electrocatalytic oxidation of Hcy in aqueous solutions. The kinetic parameters of the system, including electron transfer coefficient, and catalytic rate constant were also determined using the electrochemical approaches. In addition, SWV was used for quantitative analysis. SWV showed wide linear dynamic range (0.1-210.0 μM Hcy) with a detection limit of 0.08 μM Hcy. Finally, this method was also examined as a selective, simple, and precise electrochemical sensor for the determination of Hcy in real samples.

Voltammetric Determination of Homocysteine Using Multiwall Carbon Nanotube Paste Electrode in the Presence of Chlorpromazine as a Mediator

PubMed Central

Gholami-Orimi, Fathali; Taleshi, Farshad; Biparva, Pourya; Karimi-Maleh, Hassan; Beitollahi, Hadi; Ebrahimi, Hamid R.; Shamshiri, Mohamad; Bagheri, Hasan; Fouladgar, Masoud; Taherkhani, Ali

2012-01-01

We propose chlorpromazine (CHP) as a new mediator for the rapid, sensitive, and highly selective voltammetric determination of homocysteine (Hcy) using multiwall carbon nanotube paste electrode (MWCNTPE). The experimental results showed that the carbon nanotube paste electrode has a highly electrocatalytic activity for the oxidation of Hcy in the presence of CHP as a mediator. Cyclic voltammetry, double potential step chronoamperometry, and square wave voltammetry (SWV) are used to investigate the suitability of CHP at the surface of MWCNTPE as a mediator for the electrocatalytic oxidation of Hcy in aqueous solutions. The kinetic parameters of the system, including electron transfer coefficient, and catalytic rate constant were also determined using the electrochemical approaches. In addition, SWV was used for quantitative analysis. SWV showed wide linear dynamic range (0.1–210.0 μM Hcy) with a detection limit of 0.08 μM Hcy. Finally, this method was also examined as a selective, simple, and precise electrochemical sensor for the determination of Hcy in real samples. PMID:22675657

Electrochemical studies of quinine in surfactant media using hanging mercury drop electrode: a cyclic voltammetric study.

PubMed

Dar, Riyaz Ahmad; Brahman, Pradeep Kumar; Tiwari, Sweety; Pitre, Krishna Sadashiv

2012-10-01

The electrochemical behavior of quinine was investigated by cyclic voltammetry (CV) and square wave voltammetry (SWV) using surfactant. The reduction peak current of quinine increases remarkably in presence of 1% CTAB. Its electrochemical behavior is quasi-reversible in the Britton-Robinson buffers of pH 10.38 by exhibiting the well-defined single cathodic and anodic waves and the ratio of I(p)(a)/I(p)(c) approaching one at the scan rate of 500 mVs(-1). On the basis of CV, SWV and Coulometry, electrochemical reduction mechanism of quinine has been proposed which has shown that protonation occurs on the nitrogen of the quinoline moiety. Linearity was obtained when the peak currents (I(p)) were plotted against concentrations of quinine in the range of 30.0-230.0 ng mL(-1) with a detection limit of 0.132 ng mL(-1) in SWV and 90.0-630.0 ng mL(-1) with a detection limit of 0.238 ng mL(-1) in DPV. Fast and sensitive SWV has been applied for the quantitative analysis of quinine in bark of Cinchona sp. and in soft drinks and a good recovery was obtained. The accuracy and precision of the method are determined and validated statistically. No interferences from other food additives were observed. The relative standard deviation for intraday and interday assay was 0.89 and 0.73% (n=3) respectively. Copyright © 2012 Elsevier B.V. All rights reserved.

Electrochemical magneto immunosensor based on endogenous β-galactosidase enzyme to determine enterotoxicogenic Escherichia coli F4 (K88) in swine feces using square wave voltammetry.

PubMed

Viviana Tarditto, Lorena; Alicia Zon, María; García Ovando, Hugo; Roberto Vettorazzi, Nelio; Javier Arévalo, Fernando; Fernández, Héctor

2017-11-01

Diseases caused by enterotoxicogenic Escherichia coli F4 (K88) (ETEC F4) are a problem in swine production establishments. Due to the high rate of mortality and morbidity of E. coli infections, a rapid and accurate diagnosis is important in order to choose an appropriate treatment to reduce the economic impact. Therefore, an electrochemical magneto-immunosensor (EMI) was developed to detect and quantify ETEC F4 in swine feces samples through a direct non-competitive immunoassay. ETEC F4 was selectively captured by immunomagnetic separation. The detection principle was based on the activity of β-galactosidase endogenous enzyme (β-gal), which hydrolyses the p-aminophenyl-β-D-galactopyranoside (p-APG) producing p-aminophenol (p-AP), which was oxidized on a carbon screen printed electrode (CSPE) using square wave voltammetry (SWV). All parameters related to construction and electrochemical responses were optimized. The total analysis time to quantify ETEC F4 using the EMI was less than 2h and the limit of detection (LOD) was 33CFUmL -1 . The perceptual relative error (%E r ) was 20%. The magneto-immunosensor was validated versus conventional method of culture and plate count, obtaining a very good agreement. The EMI is simple, fast and economical to detect and quantify ETEC F4 in swine feces samples, being thus a valuable tool in swine production. Copyright © 2017 Elsevier B.V. All rights reserved.

Electrochemical Sensors Based on Screen-Printed Electrodes: The Use of Phthalocyanine Derivatives for Application in VFA Detection

PubMed Central

Ndiaye, Amadou L.; Delile, Sébastien; Brunet, Jérôme; Varenne, Christelle; Pauly, Alain

2016-01-01

Here, we report on the use of electrochemical methods for the detection of volatiles fatty acids (VFAs), namely acetic acid. We used tetra-tert-butyl phthalocyanine (PcH2-tBu) as the sensing material and investigated its electroanalytical properties by means of cyclic voltammetry (CV) and square wave voltammetry (SWV). To realize the electrochemical sensing system, the PcH2-tBu has been dropcast-deposited on carbon (C) orgold (Au)screen-printed electrodes (SPEs) and characterized by cyclic voltammetry and scanning electron microscopy (SEM). The SEM analysis reveals that the PcH2-tBu forms mainly aggregates on the SPEs. The modified electrodes are used for the detection of acetic acid and present a linear current increase when the acetic acid concentration increases. The Cmodified electrode presents a limit of detection (LOD) of 25.77 mM in the range of 100 mM–400 mM, while the Aumodified electrode presents an LOD averaging 40.89 mM in the range of 50 mM–300 mM. When the experiment is realized in a buffered condition, theCmodified electrode presents a lower LOD, which averagesthe 7.76 mM. A pronounced signal decay attributed to an electrode alteration is observed in the case of the gold electrode. This electrode alteration severely affects the coating stability. This alteration is less perceptible in the case of the carbon electrode. PMID:27598214

Analytical solutions of the planar cyclic voltammetry process for two soluble species with equal diffusivities and fast electron transfer using the method of eigenfunction expansions

DOE Office of Scientific and Technical Information (OSTI.GOV)

Samin, Adib; Lahti, Erik; Zhang, Jinsuo, E-mail: zhang.3558@osu.edu

Cyclic voltammetry is a powerful tool that is used for characterizing electrochemical processes. Models of cyclic voltammetry take into account the mass transport of species and the kinetics at the electrode surface. Analytical solutions of these models are not well-known due to the complexity of the boundary conditions. In this study we present closed form analytical solutions of the planar voltammetry model for two soluble species with fast electron transfer and equal diffusivities using the eigenfunction expansion method. Our solution methodology does not incorporate Laplace transforms and yields good agreement with the numerical solution. This solution method can be extendedmore » to cases that are more general and may be useful for benchmarking purposes.« less

MEASURING METAL SULFIDE COMPLEXES IN OXIC RIVER WATERS WITH SQUARE WAVE VOLTAMMETRY. (R825395)

EPA Science Inventory

A sulfide identification protocol was developed to quantify specific metal
sulfides that could exist in river water. Using a series of acid additions,
nitrogen purges, and voltammetric analyses, metal sulfides were identified and
semiquantified in three specific gr...

Mercury-Free Analysis of Lead in Drinking Water by Anodic Stripping Square Wave Voltammetry

ERIC Educational Resources Information Center

Wilburn, Jeremy P.; Brown, Kyle L.; Cliffel, David E.

2007-01-01

The analysis of drinking water for lead, which has well-known health effects, is presented as an instructive example for undergraduate chemistry students. It allows the students to perform an experiment and evaluate to monitor risk factors and common hazard of everyday life.

Determination of picloram in natural waters employing sequential injection square wave voltammetry using the hanging mercury drop electrode.

PubMed

Dos Santos, Luciana B O; Masini, Jorge C

2007-05-15

This paper describes the development of a sequential injection analysis method to automate the determination of picloram by square wave voltammetry exploiting the concept of monosegmented flow analysis to perform in-line sample conditioning and standard addition. To perform these tasks, an 800muL monosegment is formed, composed by 400muL of sample and 400muL of conditioning/standard solution, in medium of 0.10molL(-1) H(2)SO(4). Homogenization of the monosegment is achieved by three flow reversals. After homogenization the mixture zone is injected toward the flow cell, which is adapted to the capillary of a hanging drop mercury electrode, at a flow rate of 50muLs(-1). After a suitable delay time, the potential is scanned from -0.5 to -1.0V versus Ag/AgCl at frequency of 300Hz and pulse height of 25mV. The linear dynamic range is observed for picloram concentrations between 0.10 and 2.50mgL(-1) fitting to the linear equation I(p)=(-2.19+/-0.03)C(picloram)+(0.096+/-0.039), with R(2)=0.9996, for which the slope is given in muALmg(-1). The detection and quantification limits are 0.036 and 0.12mgL(-1), respectively. The sampling frequency is 37h(-1) when the standard addition protocol is followed, but can be increased to 41h(-1) if the protocol to obtain in-line external calibration curve is used for quantification. The method was applied for determination of picloram in spiked water samples and the accuracy was evaluated by comparison with high performance liquid chromatography using molecular absorption at 220nm for detection. No evidences of statistically significant differences between the two methods were observed.

Substituent Inductive Effects on the Electrochemical Oxidation of Flavonoids Studied by Square Wave Voltammetry and Ab Initio Calculations.

PubMed

Arroyo-Currás, Netzahualcóyotl; Rosas-García, Víctor M; Videa, Marcelo

2016-10-27

Flavonoids are natural products commonly found in the human diet that show antioxidant, anti-inflammatory and anti-hepatotoxic activities. These nutraceutical properties may relate to the electrochemical activity of flavonoids. To increase the understanding of structure-electrochemical activity relations and the inductive effects that OH substituents have on the redox potential of flavonoids, we carried out square-wave voltammetry experiments and ab initio calculations of eight flavonoids selected following a systematic variation in the number of hydroxyl substituents and their location on the flavan backbone: three flavonols, three anthocyanidins, one anthocyanin and the flavonoid backbone flavone. We compared the effect that the number of -OH groups in the ring B of flavan has on the oxidation potential of the flavonoids considered, finding linear correlations for both flavonols and anthocyanidins ( R 2 = 0.98 ). We analyzed the effects that position and number of -OH substituents have on electron density distributions via ab initio quantum chemical calculations. We present direct correlations between structural features and oxidation potentials that provide a deeper insight into the redox chemistry of these molecules.

Determination of Benzyl-hexadecyldimethylammonium 1,4-Bis(2-ethylhexyl)sulfosuccinate Vesicle Permeability by Using Square Wave Voltammetry and an Enzymatic Reaction.

PubMed

Cobo Solis, Airam K; Correa, N Mariano; Molina, Patricia G

2017-10-31

This report describes the studies performed to determine the permeability coefficient value (P) of 1-naphthyl phosphate (1-NP) through the benzyl-hexadecyldimethylammonium 1,4-bis(2-ethylhexyl)sulfosuccinate (AOT-BHD) vesicle bilayer. 1-NP was added in the external phase and must cross the bilayer of the vesicle to react with the encapsulated enzyme (alkaline phosphatase) to yield 1-naphtholate (NPh - ), the product of the enzymatic hydrolysis. This product is electrochemically detected, at basic pH value, by a square wave voltammetry technique, which can be a good alternative over the spectroscopic one, to measure the vesicle solutions because scattering (due to its turbidity) does not make any influence in the electrochemical signal. The experimental data allow us to propose a mathematical model, and a value of P = (1.00 ± 0.15) × 10 -9 cm s -1 was obtained. Also, a value of P = (2.0 ± 0.5) × 10 -9 cm s -1 was found by using an independent technique, ultraviolet-visible spectroscopy, for comparison. It is evident that the P values obtained from both the techniques are comparable (within the experimental error of both techniques) under the same experimental conditions. This study constitutes the first report of the 1-NP permeability determination in this new vesicle. We want to highlight the importance of the introduction of a new method and the electrochemical response of the product generated through an enzymatic reaction that occurs in the inner aqueous phase of the vesicle, where the enzyme is placed.

Electrochemical and nonenzymatic glucose biosensor based on MDPA/MWNT/PGE nanocomposite.

PubMed

Surucu, Ozge; Abaci, Serdar

2017-09-01

The nonenzymatic detection of glucose has been widely investigated in a variety of fields ranging from biomedical applications to ecological approaches. Among these fields, electrochemical methods have great advantages such as high electrocatalytic ability, high sensitivity, good selectivity and low-cost for the electrooxidation of glucose. Future trends on glucose sensing are nanostructured electrodes depending upon the development of nanotechnology. In this study, an electrochemical and nonenzymatic glucose sensor based on (E)-4-((5-methylthiazole-2-yl)diazenyl)-N-phenylaniline (MDPA)/multi-walled carbon nanotube (MWNT)/pencil graphite electrode (PGE) was performed. Electrochemical measurements were obtained using cyclic voltammetry and square wave voltammetry techniques, and characterization of surfaces was carried out using scanning electron microscope and electrochemical impedance spectroscopy techniques. The modification of PGE was made using MDPA and MWNT, and 10 cycles coating was used to prepare the proposed electrode. The effects of scan rate and pH on the peak potential and the peak current were determined. The limit of detection and linear range were calculated using various concentrations of glucose. The interference study was made using coexisting substances including metal ions such as Al 3+ , Cu 2+ , Fe 3+ and ascorbic acid. Copyright © 2017 Elsevier B.V. All rights reserved.

Electrochemistry and Spectroelectrochemistry of the Pu (III/IV) and (IV/VI) Couples in Nitric Acid Systems

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lines, Amanda M.; Adami, Susan R.; Casella, Amanda J.

The solution chemistry of Pu in nitric acid is explored via electrochemistry and spectroelectrochemistry. By utilizing and comparing these techniques, an improved understanding of Pu behavior and its dependence on nitric acid concentration can be achieved. Here the Pu (III/IV) couple is characterized using cyclic voltammetry, square wave voltammetry, and a spectroelectrochemical Nernst step. Results indicate the formal reduction potential of the couple shifts negative with increasing acid concentration and reversible electrochemistry is no longer attainable above 6 M HNO3. Spectroelectrochemistry is also used to explore the irreversible oxidation of Pu(IV) to Pu(VI) and shine light on the mechanism andmore » acid dependence of the redox reaction.« less

E-DNA sensor of Mycobacterium tuberculosis based on electrochemical assembly of nanomaterials (MWCNTs/PPy/PAMAM).

PubMed

Miodek, Anna; Mejri, Nawel; Gomgnimbou, Michel; Sola, Christophe; Korri-Youssoufi, Hafsa

2015-09-15

Two-step electrochemical patterning methods have been employed to elaborate composite nanomaterials formed with multiwalled carbon nanotubes (MWCNTs) coated with polypyrrole (PPy) and redox PAMAM dendrimers. The nanomaterial has been demonstrated as a molecular transducer for electrochemical DNA detection. The nanocomposite MWCNTs-PPy has been formed by wrapping the PPy film on MWCNTs during electrochemical polymerization of pyrrole on the gold electrode. The MWCNTs-PPy layer was modified with PAMAM dendrimers of fourth generation (PAMAM G4) with covalent bonding by electro-oxidation method. Ferrocenyl groups were then attached to the surface as a redox marker. The electrochemical properties of the nanomaterial (MWCNTs-PPy-PAMAM-Fc) were studied using both square wave voltammetry and cyclic voltammetry to demonstrate efficient electron transfer. The nanomaterial shows high performance in the electrochemical detection of DNA hybridization leading to a variation in the electrochemical signal of ferrocene with a detection limit of 0.3 fM. Furthermore, the biosensor demonstrates ability for sensing DNA of rpoB gene of Mycobacterium tuberculosis in real PCR samples. Developed biosensor was suitable for detection of sequences with a single nucleotide polymorphism (SNP) T (TCG/TTG), responsible for resistance of M. tuberculosis to rifampicin drug, and discriminating them from wild-type samples without such mutation. This shows potential of such systems for further application in pathogens diagnostic and therapeutic purpose.

MICROFABRICATED ARRAY OF IRIDIUM MICRODISKS AS A SUBSTRATE FOR DIRECT DETERMINATION OF CU2+ OR HG2+USING SQUARE WAVE ANODIC STRIPPING VOLTAMMETRY. (R825511C022)

EPA Science Inventory

The perspectives, information and conclusions conveyed in research project abstracts, progress reports, final reports, journal abstracts and journal publications convey the viewpoints of the principal investigator and may not represent the views and policies of ORD and EPA. Concl...

Brain extracellular glucose assessed by voltammetry throughout the rat sleep-wake cycle.

PubMed

Netchiporouk, L; Shram, N; Salvert, D; Cespuglio, R

2001-04-01

In the present study, cortical extracellular levels of glucose were monitored for the first time throughout the sleep-wake states of the freely moving rat. For this purpose, polygraphic recordings (electroencephalogram of the fronto-occipital cortices and electromyogram of the neck muscles) were achieved in combination with differential normal pulse voltammetry (DNPV) using a specific glucose sensor. Data obtained reveal that the basal extracellular glucose concentration in the conscious rat is 0.59 +/- 0.3 m M while under chloral hydrate anaesthesia (0.4 g/kg, i.p.) it increases up to 180% of its basal concentration. Regarding the sleep-wake cycle, the existence of spontaneous significant variations in the mean glucose level during slow-wave sleep (SWS = +13%) and paradoxical sleep (PS = -11%) compared with the waking state (100%) is also reported. It is to be noticed that during long periods of active waking, glucose level tends towards a decrease that becomes significant after 15 min (active waking = -32%). On the contrary, during long episodes of slow-wave sleep, it tends towards an increase which becomes significant after 12 min (SWS = +28%). It is suggested that voltammetric techniques using enzymatic biosensors are useful tools allowing direct glucose measurements in the freely moving animal. On the whole, paradoxical sleep is pointed out as a state highly dependent on the availability of energy and slow-wave sleep as a period of energy saving.

Voltammetric studies of antimony ions in soda-lime-silica glass melts up to 1873 K.

PubMed

Yamashita, H; Yamaguchi, S; Nishimura, R; Maekawa, T

2001-01-01

The half wave potential of reduction of Sb5+ in 16Na2O x 10CaO x 74SiO2 glass melts was examined by differential pulse voltammetry up to 1873 K. The half wave potential shifted to the positive direction with an increase in temperature. The results indicate that the equilibrium of Sb5+/Sb3+ shifted to negative direction with an increase in temperature. The half wave potential shifted to positive direction (48 mV at 1473 K) when the atmosphere over the melts changed from pure oxygen gas to air, in agreement with the theoretical prediction. The reversibility of Pt:O2 reference electrode is confirmed.

Cyclic voltammetry using silver as cathode material: a simple method for determining electro and chemical features and solubility values of CO2 in ionic liquids.

PubMed

Reche, Irene; Gallardo, Iluminada; Guirado, Gonzalo

2015-01-28

A report is presented on the use of cyclic voltammetry using silver as a working electrode. The combined electrocatalytic properties of silver and ionic liquids allow cyclic voltammetry to be turned into an ideal tool for the rapid and accurate access to diffusion coefficient values and solubility values of carbon dioxide in ionic liquids under standard conditions.

Voltammetry Method Evaluation

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hoyt, N.; Pereira, C.; Willit, J.

2016-07-29

The purpose of the ANL MPACT Voltammetry project is to evaluate the suitability of previously developed cyclic voltammetry techniques to provide electroanalytical measurements of actinide concentrations in realistic used fuel processing scenarios. The molten salts in these scenarios are very challenging as they include high concentrations of multiple electrochemically active species, thereby creating a variety of complications. Some of the problems that arise therein include issues related to uncompensated resistance, cylindrical diffusion, and alloying of the electrodeposited metals. Improvements to the existing voltammetry technique to account for these issues have been implemented, resulting in good measurements of actinide concentrations acrossmore » a wide range of adverse conditions.« less

A graphene-based electrochemical sensor for sensitive detection of paracetamol

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kang, Xinhuang; Wang, Jun; Wu, Hong

2010-05-15

An electrochemical sensor based on the electrocatalytic activity of functionalized graphene for sensitive detection of paracetamol is presented. The electrochemical behaviors of paracetamol on graphene-modified glassy carbon electrodes (GCEs) were investigated by cyclic voltammetry and square-wave voltammetry. The results showed that the graphene-modified electrode exhibited excellent electrocatalytic activity to paracetamol. A quasi-reversible redox process of paracetamol at the modified electrode was obtained, and the over-potential of paracetamol decreased significantly compared with that at the bare GCE. Such electrocatalytic behavior of graphene is attributed to its unique physical and chemical properties, e.g., subtle electronic characteristics, attractive π–π interaction, and strong adsorptivemore » capability. The sensor shows great promise for simple, sensitive, and quantitative detection of paracetamol.« less

Development of a cyclic voltammetry method for the detection of Clostridium novyi in black disease.

PubMed

Liu, L L; Jiang, D N; Xiang, G M; Liu, C; Yu, J C; Pu, X Y

2014-03-17

Black disease is an acute disease of sheep and cattle. The pathogen is the obligate anaerobe, Clostridium novyi. Due to difficulties of anaerobic culturing in the country or disaster sites, a simple, rapid, and sensitive method is required. In this study, an electrochemical method, the cyclic voltammetry method, basing on loop-mediated isothermal amplification (LAMP), electrochemical ion bonding (positive dye, methylene blue), was introduced. DNA extracted from C. novyi specimens was amplified through the LAMP reaction. Then the products combined were with methylene blue, which lead to a reduction in the oxidation peak current (ipA) and the reduction peak current (ipC) of the cyclic voltammetry. The changes of ipA/ipC were real-time measured by special designed electrode, so the DNA was quantitatively detected. The results displayed that this electrochemical detection of C. novyi could be completed in 1-2 h with the lowest bacterial concentration of 10(2) colony forming units/mL, and high accuracy (96.5%), sensitivity (96%), and specificity (97%) compared to polymerase chain reation. The cyclic voltammetry method was a simple and fast method, with high sensitivity and high specificity, and has great potential to be a usable molecular tool for fast diagnosis of Black disease.

Molecularly imprinted polymer solid-phase extraction coupled to square wave voltammetry at carbon fibre microelectrodes for the determination of fenbendazole in beef liver.

PubMed

Guzmán-Vázquez de Prada, A; Loaiza, Oscar A; Serra, B; Morales, D; Martínez-Ruiz, P; Reviejo, A J; Pingarrón, J M

2007-05-01

A molecularly imprinted polymer was developed and used for solid-phase extraction (MISPE) of the antihelmintic fenbendazole in beef liver samples. Detection of the analyte was accomplished using square wave voltammetry (SWV) at a cylindrical carbon fibre microelectrode (CFME). A mixture of MeOH/HAc (9:1) was employed both as eluent in the MISPE system and as working medium for electrochemical detection of fenbendazole. The limit of detection was 1.9x10(-7) mol L-1 (57 microg L-1), which was appropriate for the determination of fenbendazole at the maximum residue level permitted by the European Commission (500 microg kg-1 in liver). Given that the SW voltammetric analysis could not be directly performed in the sample extract as a consequence of interference from some sample components, a sample clean-up with a MIP for selectively retaining fenbendazole was performed. The MIP was synthesized using a 1:8:22 template/methacrylic acid/ethylene glycol dimethacrylate ratio. A Britton-Robinson Buffer of pH 9.0 was selected for retaining fenbendazole in the MIP cartridges, and an eluent volume of 5.0 mL at a flow rate of 2.0 mL min-1 was chosen in the elution step. Cross-reactivity with the MIP was observed for other benzimidazoles. The synthesized MIP exhibited a good selectivity for benzimidazoles with respect to other veterinary drugs. The applicability of the MISPE-SWV method was tested with beef liver samples, spiked with fenbendazole at 5,000 and 500 microg kg-1. Results obtained for ten different liver samples yielded mean recoveries of (95+/-12)% and (96+/-11)% for the upper and lower concentration level, respectively.

Multiple Strategy Bio-Detection Sensor Platforms Made From Carbon and Polymer Materials

DTIC Science & Technology

2006-01-31

strands for detection purposes using the cyclic voltammetry (impedance) method. 6. Design of an actual set (Au patttern) to best detect the DNA binding. 7...chronoamperometry and cyclic voltammetry are used for electropolymerization. When chronoamperometry is used, the applied potential was kept at 0.8V, and the...others remained constant. When cyclic voltammetry is used, the scan rate is kept at 1OOmV/s with a scan range from -0.4V tol.OV. The thickness or the

Voltammetric behavior of Mammeisin (MA) at a glassy carbon electrode and its interaction with Bovine Serum Albumin (BSA).

PubMed

Leuna, Jules-Blaise Mabou; Sop, Sergeot Kungo; Makota, Suzanne; Njanja, Evangeline; Ebelle, Thiery Christophe; Azebaze, Anatole Guy; Ngameni, Emmanuel; Nassi, Achille

2018-02-01

The electrochemical oxidation of Mammeisin (MA) was studied in a solution containing acetone and 0.1M phosphate buffer +0.1M KCl (pH=5.3) at a glassy carbon electrode (GCE), using cyclic (CV) and square wave voltammetry (SWV). MA showed a quasi-reversible process, which is pH dependent and that involves the exchange of two electrons and two protons. The oxidation product was adsorbed by the electrode surface to form a film that blocks active sites over repetitive cyclic. Moreover, the interaction of MA and bovine serum albumin (BSA) was studied by CV and SWV at different pHs (5.4, 7.2, 9.5). As a result of the affinity binding with BSA, electrochemically inactive complex was formed. In addition, the oxidation potential of MA in the presence of BSA depends on the pH. The diffusion coefficients of both free and bound MA were estimated from the cyclic voltammetry data using the method developed by Randles-Sevich (D f =9.85×10 -5 cm 2 s -1 and D b =1.27×10 -9 cm 2 s -1 ) and the binding constant of MA-BSA complex, K=3.47×10 2 Lmol -1 , was obtained. Copyright © 2017. Published by Elsevier B.V.

Cyclic Voltammetry.

ERIC Educational Resources Information Center

Evans, Dennis H.; And Others

1983-01-01

Cyclic voltammetry is a simple experiment that has become popular in chemical research because it can provide useful information about redox reactions in a form which is easily obtained and interpreted. Discusses principles of the method and illustrates its use in the study of four electrode reactions. (Author/JN)

Characterization of inclusion complexes of organic ions with hydrophilic hosts by ion transfer voltammetry with solvent polymeric membranes.

PubMed

Olmos, José Manuel; Laborda, Eduardo; Ortuño, Joaquín Ángel; Molina, Ángela

2017-03-01

The quantitative characterization of inclusion complexes formed in aqueous phase between organic ions and hydrophilic hosts by ion-transfer voltammetry with solvent polymeric membrane ion sensors is studied, both in a theoretical and experimental way. Simple analytical solutions are presented for the determination of the binding constant of the complex from the variation with the host concentration of the electrochemical signal. These solutions are valid for any voltammetric technique and for solvent polymeric membrane ion sensors comprising one polarisable interface (1PI) and also, for the first time, two polarisable interfaces (2PIs). Suitable experimental conditions and data analysis procedures are discussed and applied to the study of the interactions of a common ionic liquid cation (1-octyl-3-metyl-imidazolium) and an ionisable drug (clomipramine) with two hydrophilic cyclodextrins: α-cyclodextrin and 2-hydroxypropyl-β-cyclodextrin. The experimental study is performed via square wave voltammetry with 2PIs and 1PI solvent polymeric membranes and in both cases the electrochemical experiments enable the detection of inclusion complexes and the determination of the corresponding binding constant. Copyright © 2016 Elsevier B.V. All rights reserved.

Direct Quantification of Cd2+ in the Presence of Cu2+ by a Combination of Anodic Stripping Voltammetry Using a Bi-Film-Modified Glassy Carbon Electrode and an Artificial Neural Network.

PubMed

Zhao, Guo; Wang, Hui; Liu, Gang

2017-07-03

Abstract : In this study, a novel method based on a Bi/glassy carbon electrode (Bi/GCE) for quantitatively and directly detecting Cd 2+ in the presence of Cu 2+ without further electrode modifications by combining square-wave anodic stripping voltammetry (SWASV) and a back-propagation artificial neural network (BP-ANN) has been proposed. The influence of the Cu 2+ concentration on the stripping response to Cd 2+ was studied. In addition, the effect of the ferrocyanide concentration on the SWASV detection of Cd 2+ in the presence of Cu 2+ was investigated. A BP-ANN with two inputs and one output was used to establish the nonlinear relationship between the concentration of Cd 2+ and the stripping peak currents of Cu 2+ and Cd 2+ . The factors affecting the SWASV detection of Cd 2+ and the key parameters of the BP-ANN were optimized. Moreover, the direct calibration model (i.e., adding 0.1 mM ferrocyanide before detection), the BP-ANN model and other prediction models were compared to verify the prediction performance of these models in terms of their mean absolute errors (MAEs), root mean square errors (RMSEs) and correlation coefficients. The BP-ANN model exhibited higher prediction accuracy than the direct calibration model and the other prediction models. Finally, the proposed method was used to detect Cd 2+ in soil samples with satisfactory results.

Fullerene-C60-modified electrode as a sensitive voltammetric sensor for detection of nandrolone--an anabolic steroid used in doping.

PubMed

Goyal, Rajendra N; Gupta, Vinod K; Bachheti, Neeta

2007-07-30

The electrochemical behaviour of nandrolone is investigated by cyclic, differential pulse and square-wave voltammetry in phosphate buffer system at fullerene-C60-modified electrode. The modified electrode shows an excellent electrocatalytic activity towards the oxidation of nandrolone resulting in a marked lowering in the peak potential and considerable improvement of the peak current as compared to the electrochemical activity at the bare glassy carbon electrode. The oxidation process is shown to be irreversible and diffusion-controlled. A linear range of 50 microM to 0.1 nM is obtained along with a detection limit and sensitivity of 0.42 nM and 0.358 nA nM(-1), respectively, in square-wave voltammetric technique. A diffusion coefficient of 4.13x10(-8) cm2 s(-1) was found for nandrolone using chronoamperometry. The effect of interferents, stability and reproducibility of the proposed method were also studied. The described method was successfully employed for the determination of nandrolone in human serum and urine samples. A cross-validation of observed results by GC-MS indicates that the results are in good agreement with each other.

Sensitive voltammetric determination of thymol in essential oil of Carum copticum seeds using boron-doped diamond electrode.

PubMed

Stanković, Dalibor M

2015-10-01

Essential oil of Carum copticum seeds, obtained from a local shop, was extracted and content of thymol was analyzed using square-wave voltammetry at boron-doped diamond electrode. The effect of various parameters, such as pH of supporting electrolyte and square-wave voltammetric parameters (modulation amplitude and frequency), was examined. In Britton-Robinson buffer solution (pH 4), thymol provided a single and oval-shaped irreversible oxidation peak at +1.13 V versus silver/silver chloride potassium electrode (3M). Under optimal experimental conditions, a plot of peak height against concentration of thymol was found to be linear over the range of 4 to 100μM consisting of two linear ranges: from 4 to 20μM (R(2)=0.9964) and from 20 to 100μM (R(2)=0.9993). The effect of potential interferences such as p-cymene and γ-terpinene (major components in essential oil of C. copticum seeds) was evaluated. Thus, the proposed method displays a sufficient selectivity toward thymol with a detection limit of 3.9μM, and it was successfully applied for the determination of thymol in essential oil of C. copticum seeds. The Prussian blue method was used for validation of the proposed electroanalytical method. Copyright © 2015 Elsevier Inc. All rights reserved.

Determination of total and electrolabile copper in agricultural soil by using disposable modified-carbon screen-printed electrodes.

PubMed

Faucher, Stéphane; Cugnet, Cyril; Authier, Laurent; Lespes, Gaëtane

2014-02-01

The objective of the study is to evaluate modified-carbon screen-printed working electrodes (SPE) combined with square wave anodic stripping voltammetry (SWASV) to determine electrolabile and total copper in soils with the perspective to assess the environmental hazard resulting from copper anthropogenic contamination. The voltammetric method was investigated using a mineralized certified reference soil such that it can be assumed that the copper was totally under electrolabile form in the solution of mineralized soil. In optimal conditions, a copper recovery of 97% and a relative standard deviation (RSD) of 9% were found. The limits of detection and quantification for copper were 0.4 and 1.3 μg L(-1), respectively. Finally, the method was applied on soil leachates, which allowed evaluating the cupric transfer from the soil to the leachates and quantifying the electrolabile copper part in leachates.

Adsorptive Stripping Voltammetry of Environmental Indicators: Determination of Zinc in Algae

ERIC Educational Resources Information Center

Collado-Sanchez, C.; Hernandez-Brito, J. J.; Perez-Pena, J.; Torres-Padron, M. E.; Gelado-Caballero, M. D.

2005-01-01

A method for sample preparation and for the determination of average zinc content in algae using adsorptive stripping voltammetry are described. The students gain important didactic advantages through metal determination in environmental matrices, which include carrying out clean protocols for sampling and handling, and digesting samples using…

Comparative study of the antioxidant capacity and polyphenol content of Douro wines by chemical and electrochemical methods.

PubMed

Rebelo, M J; Rego, R; Ferreira, M; Oliveira, M C

2013-11-01

A comparative study of the antioxidant capacity and polyphenols content of Douro wines by chemical (ABTS and Folin-Ciocalteau) and electrochemical methods (cyclic voltammetry and differential pulse voltammetry) was performed. A non-linear correlation between cyclic voltammetric results and ABTS or Folin-Ciocalteau data was obtained if all types of wines (white, muscatel, ruby, tawny and red wines) are grouped together in the same correlation plot. In contrast, a very good linear correlation was observed between the electrochemical antioxidant capacity determined by differential pulse voltammetry and the radical scavenging activity of ABTS. It was also found that the antioxidant capacity of wines evaluated by the electrochemical methods (expressed as gallic acid equivalents) depend on background electrolyte of the gallic acid standards, type of electrochemical signal (current or charge) and electrochemical technique. Copyright © 2013 Elsevier Ltd. All rights reserved.

Square Wave Voltammetry of TNT at Gold Electrodes Modified with Self-Assembled Monolayers Containing Aromatic Structures

PubMed Central

Trammell, Scott A.; Zabetakis, Dan; Moore, Martin; Verbarg, Jasenka; Stenger, David A.

2014-01-01

Square wave voltammetry for the reduction of 2,4,6-trinitrotoluene (TNT) was measured in 100 mM potassium phosphate buffer (pH 8) at gold electrodes modified with self-assembled monolayers (SAMs) containing either an alkane thiol or aromatic ring thiol structures. At 15 Hz, the electrochemical sensitivity (µA/ppm) was similar for all SAMs tested. However, at 60 Hz, the SAMs containing aromatic structures had a greater sensitivity than the alkane thiol SAM. In fact, the alkane thiol SAM had a decrease in sensitivity at the higher frequency. When comparing the electrochemical response between simulations and experimental data, a general trend was observed in which most of the SAMs had similar heterogeneous rate constants within experimental error for the reduction of TNT. This most likely describes a rate limiting step for the reduction of TNT. However, in the case of the alkane SAM at higher frequency, the decrease in sensitivity suggests that the rate limiting step in this case may be electron tunneling through the SAM. Our results show that SAMs containing aromatic rings increased the sensitivity for the reduction of TNT when higher frequencies were employed and at the same time suppressed the electrochemical reduction of dissolved oxygen. PMID:25549081

Cyclic voltammetry of apple fruits: Memristors in vivo.

PubMed

Volkov, Alexander G; Nyasani, Eunice K; Tuckett, Clayton; Blockmon, Avery L; Reedus, Jada; Volkova, Maya I

2016-12-01

A memristor is a resistor with memory that exhibits a pinched hysteretic relationship in cyclic voltammetry. Recently, we have found memristors in the electrical circuitry of plants and seeds. There are no publications in literature about the possible existence of memristors and electrical differentiators in fruits. Here we found that the electrostimulation of Golden Delicious or Arkansas Black apple fruits by bipolar periodic waves induces hysteresis loops with pinched points in cyclic voltammograms at low frequencies between 0.1MHz and 1MHz. At high frequencies of 1kHz, the pinched hysteresis loop transforms to a non-pinched hysteresis loop instead of a single line I=V/R for ideal memristors because the amplitude of electrical current depends on capacitance of a fruit's tissue and electrodes, frequency and direction of scanning. Electrostimulation of electrical circuits in apple fruits by periodic voltage waves also induces electrotonic potential propagation due to cell-to-cell electrical coupling with electrical differentiators. A differentiator is an electrical circuit in which the output of the circuit is approximately directly proportional to the rate of change of the input. The information gained from electrostimulation can be used to elucidate and to observe electrochemical and electrophysiological properties of electrical circuits in fruits. Copyright © 2016 Elsevier B.V. All rights reserved.

Electrochemical and spectroelectrochemical study on novel non-peripherally tetra 1,2,4-triazole substituted phthalocyanines

NASA Astrophysics Data System (ADS)

Demirbaş, Ümit; Akyüz, Duygu; Akçay, Hakkı Türker; Koca, Atıf; Bekircan, Olcay; Kantekin, Halit

2018-03-01

In the present study novel tetra 4-(4-fluorophenyl)-5-(4-methoxyphenyl)-4H-1,2,4-triazole-3-thio substituted non-peripherally metal free (4), zinc(II) (5), lead (II) (6) and copper(II) (7) phthalocyanines were synthesized. The obtained novel compounds were characterized by a combination of FT-IR, 1H NMR, UV-Vis and MALDI-TOF techniques. The redox properties of the complexes have been investigated via cyclic voltammetry, square wave voltammetry and in situ spectroelectrochemistry. The compounds displayed ring-based, reversible and/or quasi-reversible reduction and oxidation processes and aggregation of the complexes influenced the redox character of the processes. The color changes during the redox processes of metallo phthalocyanine were recorded by in-situ spectroelectrochemical measurements. In situ UV-vis spectroelectrochemical measurements, which was associated with color change of the complexes, showed their applicability in the fields of the electrochemical technologies.

Electrochemical characterization of gelatinized starch dispersions: voltammetry and electrochemical impedance spectroscopy on platinum surface.

PubMed

Hernandez-Jaimes, C; Lobato-Calleros, C; Sosa, E; Bello-Pérez, L A; Vernon-Carter, E J; Alvarez-Ramirez, J

2015-06-25

The electrochemical properties of gelatinized starch dispersions (GSD; 5% w/w) from different botanical sources were studied using cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) tests over a platinum surface. The phenomenological modelling of EIS data using equivalent circuits indicated that after gelatinization the electrical resistance was determined mainly by the resistance of insoluble material (i.e., ghosts). Sonication of the GSD disrupted the ghost microstructure, and produced an increase in electrical conductivity by reducing the resistance of the insoluble material. The CV data showed three oxidation peaks at potentials where glucose solutions displayed oxidation waves. It is postulated that hydrolysis at the bulk and electrocatalyzed oxidation on the Pt-surface are reactions involved in the starch transformation. Starches peak intensity increased with the amylose content, suggesting that the amylose-rich matrix played an important role in the charge transfer in the electrolytic system. Copyright © 2015 Elsevier Ltd. All rights reserved.

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

NASA Astrophysics Data System (ADS)

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

2016-03-01

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

Electrochemical Determination of Food Preservative Nitrite with Gold Nanoparticles/p-Aminothiophenol-Modified Gold Electrode.

PubMed

Üzer, Ayşem; Sağlam, Şener; Can, Ziya; Erçağ, Erol; Apak, Reşat

2016-08-02

Due to the negative impact of nitrate and nitrite on human health, their presence exceeding acceptable levels is not desired in foodstuffs. Thus, nitrite determination at low concentrations is a major challenge in electroanalytical chemistry, which can be achieved by fast, cheap, and safe electrochemical sensors. In this work, the working electrode (Au) was functionalized with p-aminothiophenol (p-ATP) and modified with gold nanoparticles (Au-NPs) to manufacture the final (Au/p-ATP-Aunano) electrode in a two-step procedure. In the first step, p-ATP was electropolymerized on the electrode surface to obtain a polyaminothiophenol (PATP) coating. In the second step, Au/p-ATP-Aunano working electrode was prepared by coating the surface with the use of HAuCl₄ solution and cyclic voltammetry. Determination of aqueous nitrite samples was performed with the proposed electrode (Au/p-ATP-Aunano) using square wave voltammetry (SWV) in pH 4 buffer medium. Characteristic peak potential of nitrite samples was 0.76 V, and linear calibration curves of current intensity versus concentration was linear in the range of 0.5-50 mg·L(-1) nitrite with a limit of detection (LOD) of 0.12 mg·L(-1). Alternatively, nitrite in sausage samples could be colorimetrically determined with high sensitivity by means of p-ATP‒modified gold nanoparticles (AuNPs) and naphthylethylene diamine as coupling agents for azo-dye formation due to enhanced charge-transfer interactions with the AuNPs surface. The slopes of the calibration lines in pure NO₂(-) solution and in sausage sample solution, to which different concentrations of NO₂(-) standards were added, were not significantly different from each other, confirming the robustness and interference tolerance of the method. The proposed voltammetric sensing method was validated against the colorimetric nanosensing method in sausage samples.

Tuning Electron-Transfer Properties in 5,10,15,20-Tetra(1'-hexanoylferrocenyl)porphyrins as Prospective Systems for Quantum Cellular Automata and Platforms for Four-Bit Information Storage.

PubMed

Erickson, Nathan R; Holstrom, Cole D; Rhoda, Hannah M; Rohde, Gregory T; Zatsikha, Yuriy V; Galloni, Pierluca; Nemykin, Victor N

2017-04-17

Metal-free (1) and zinc (2) 5,10,15,20-tetra(1'-hexanoylferrocenyl)porphyrins were prepared using an acid-catalyzed tetramerization reaction between pyrrole and 1'-(1-hexanoyl)ferrocencarboxaldehyde. New organometallic compounds were characterized by combination of 1 H, 13 C, and variable-temperature NMR, UV-vis, magnetic circular dichroism, and high-resolution electrospray ionization mass spectrometry methods. The redox properties of 1 and 2 were probed by electrochemical (cyclic voltammetry and differential pulse voltammetry), spectroelectrochemical, and chemical oxidation approaches coupled with UV-vis-near-IR and Mössbauer spectroscopy. Electrochemical data recorded in the dichloromethane/TBA[B(C 6 F 5 ) 4 ] system (TBA[B(C 6 F 5 ) 4 ] is a weakly coordinating tetrabutylammonium tetrakis(pentafluorophenyl)borate electrolyte) are suggestive of "1e - + 1e - + 2e - " oxidation sequence for four ferrocene groups in 1 and 2, which followed by oxidation process centered at the porphyrin core. The separation between all ferrocene-centered oxidation electrochemical waves is very large (510-660 mV). The nature of mixed-valence [1] n+ and [2] n+ (n = 1 or 2) complexes was probed by the spectroelectrochemical and chemical oxidation methods. Analysis of the intervalence charge-transfer band in [1] + and [2] + is suggestive of the Class II (in Robin-Day classification) behavior of all mixed-valence species, which correlate well with Mössbauer data. Density functional theory-polarized continuum model (DFT-PCM) and time-dependent (TD) DFT-PCM methods were applied to correlate redox and optical properties of organometallic complexes 1 and 2 with their electronic structures.

The natural diatomite from caldiran-van (Turkey): electroanalytical application to antimigraine compound naratriptan at modified carbon paste electrode.

PubMed

Calışkan, Necla; Sögüt, Eda; Saka, Cafer; Yardım, Yavuz; Sentürk, Zuhre

2010-09-01

This paper is the first report describing the characterization of local diatomite of Caldiran-Van region (Eastern Anatolia, Turkey). Special attention was paid to the ability of its electroanalytical performance at modified electrodes and to the potential application of diatomite-modified electrode. For this purpose, the determination of Naratriptan which is a novel oral triptan (5-hydroxytryptamine receptor agonist) in migraine treatment, by means of a carbon paste electrode modified with 10% (w/w) of diatomite was studied using cyclic and square-wave voltammetry. The experimental conditions that affect the electrode reaction process were studied in terms of pH of the supporting electrolyte, scan rate, accumulation variables, modifier composition and square-wave parameters. Using square-wave stripping mode, the drug yielded a well-defined voltammetric response in Britton-Robinson buffer, pH 4.0 at 0.84 V (vs. Ag/AgCl) (a pre-concentration step being carried out with an open circuit at 120 s). The process could be used to determine Naratriptan concentrations in the range 5x10(-7)-9x10(-7) M, with a detection limit of 1.25x10(-7) M (46.5 mug L(-1)). The applicability of the method to spiked human urine samples was illustrated.

Voltammetry as a Tool for Characterization of CdTe Quantum Dots

PubMed Central

Sobrova, Pavlina; Ryvolova, Marketa; Hubalek, Jaromir; Adam, Vojtech; Kizek, Rene

2013-01-01

Electrochemical detection of quantum dots (QDs) has already been used in numerous applications. However, QDs have not been well characterized using voltammetry, with respect to their characterization and quantification. Therefore, the main aim was to characterize CdTe QDs using cyclic and differential pulse voltammetry. The obtained peaks were identified and the detection limit (3 S/N) was estimated down to 100 fg/mL. Based on the convincing results, a new method for how to study stability and quantify the dots was suggested. Thus, the approach was further utilized for the testing of QDs stability. PMID:23807507

Determination of cobalt in vegetable animal foodstuffs by differential pulse adsorptive voltammetry using alpha-benzil dioxime.

PubMed

Giroussi, S; Voulgaropoulos, A; Ayiannidis, A K; Golimowski, J; Janicki, M

1995-12-22

A selective and sensitive voltammetric method for the determination of cobalt in vegetable animal foodstuffs is developed. The method is based on the use of alpha-benzil dioxime (alpha-BD) as a chelating agent for differential pulse adsorptive stripping voltammetry (DPASV) and is free from zinc interferences. The influence of pH, time and alpha-BD concentration on the peak resolution and height are discussed. The method was successfully applied in some typical vegetable animal foodstuffs with R.S.D. < 6%.

A simple, fast and accurate in-situ method to measure the rate of transport of redox species through membranes for lithium batteries

NASA Astrophysics Data System (ADS)

Meddings, Nina; Owen, John R.; Garcia-Araez, Nuria

2017-10-01

Lithium ion conducting membranes are important to protect the lithium metal electrode and act as a barrier to crossover species such as polysulphides in Li-S systems, redox mediators in Li-O2 cells or dissolved cathode species or electrolyte oxidation products in high voltage Li-ion batteries. We present an in-situ method for measuring permeability of membranes to crossover redox species. The method employs a 'Swagelok' cell design equipped with a glassy carbon working electrode, in which redox species are placed initially in the counter electrode compartment only. Permeability through the membrane, which separates working and counter electrodes, is determined using a square wave voltammetry technique that allows the concentration of crossover redox species to be evaluated over time with very high precision. We test the method using a model and well-behaved electrochemical system to demonstrate its sensitivity, reproducibility and reliability relative to alternative approaches. This new method offers advantages in terms of small electrolyte volume, and simple, fast, quantitative and in-situ measurement.

A sensitive, selective and rapid determination of lead(II) ions in real-life samples using an electrochemically reduced graphene oxide-graphite reinforced carbon electrode.

PubMed

Hamsawahini, Kunashegaran; Sathishkumar, Palanivel; Ahamad, Rahmalan; Yusoff, Abdull Rahim Mohd

2015-11-01

In this study, a sensitive and cost-effective electrochemically reduced graphene oxide (ErGO) on graphite reinforced carbon (GRC) was developed for the detection of lead (Pb(II)) ions present in the real-life samples. A film of graphene oxide (GO) was drop-casted on GRC and their electrochemical properties were investigated using cyclic voltammetry (CV), amperometry and square wave voltammetry (SWV). Factors influencing the detection of Pb(II) ions, such as grades of GRC, constant applied cathodic potential (CACP), concentration of hydrochloric acid and drop-casting drying time were optimised. GO is irreversibly reduced in the range of -0.7 V to -1.6 V vs Ag/AgCl (3 M) in acidic condition. The results showed that the reduction behaviour of GO contributed to the high sensitivity of Pb(II) ions detection even at nanomolar level. The ErGO-GRC showed the detection limit of 0.5 nM and linear range of 3-15 nM in HCl (1 M). The developed electrode has potential to be a good candidate for the determination of Pb(II) ions in different aqueous system. The proposed method gives a good recovery rate of Pb(II) ions in real-life water samples such as tap water and river water. Copyright © 2015 Elsevier B.V. All rights reserved.

Embedded Disposable Functionalized Electrochemical Biosensor with a 3D-Printed Flow Cell for Detection of Hepatic Oval Cells (HOCs).

PubMed

Damiati, Samar; Peacock, Martin; Leonhardt, Stefan; Damiati, Laila; Baghdadi, Mohammed A; Becker, Holger; Kodzius, Rimantas; Schuster, Bernhard

2018-02-14

Hepatic oval cells (HOCs) are considered the progeny of the intrahepatic stem cells that are found in a small population in the liver after hepatocyte proliferation is inhibited. Due to their small number, isolation and capture of these cells constitute a challenging task for immunosensor technology. This work describes the development of a 3D-printed continuous flow system and exploits disposable screen-printed electrodes for the rapid detection of HOCs that over-express the OV6 marker on their membrane. Multiwall carbon nanotube (MWCNT) electrodes have a chitosan film that serves as a scaffold for the immobilization of oval cell marker antibodies (anti-OV6-Ab), which enhance the sensitivity of the biomarker and makes the designed sensor specific for oval cells. The developed sensor can be easily embedded into the 3D-printed flow cell to allow cells to be exposed continuously to the functionalized surface. The continuous flow is intended to increase capture of most of the target cells in the specimen. Contact angle measurements were performed to characterize the nature and quality of the modified sensor surface, and electrochemical measurements (cyclic voltammetry (CV) and square wave voltammetry (SWV)) were performed to confirm the efficiency and selectivity of the fabricated sensor to detect HOCs. The proposed method is valuable for capturing rare cells and could provide an effective tool for cancer diagnosis and detection.

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

PubMed

Kumaravel, Ammasai; Chandrasekaran, Maruthai

2015-07-15

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

Electrochemical methods for monitoring of environmental carcinogens.

PubMed

Barek, J; Cvacka, J; Muck, A; Quaiserová, V; Zima, J

2001-04-01

The use of modern electroanalytical techniques, namely differential pulse polarography, differential pulse voltammetry on hanging mercury drop electrode or carbon paste electrode, adsorptive stripping voltammetry and high performance liquid chromatography with electrochemical detection for the determination of trace amounts of carcinogenic N-nitroso compounds, azo compounds, heterocyclic compounds, nitrated polycyclic aromatic hydrocarbons and aromatic and heterocyclic amines is discussed. Scope and limitations of these methods are described and some practical applications based on their combination with liquid-liquid or solid phase extraction are given.

Investigation of interaction between magnetic silica particles and lambda phage DNA fragment.

PubMed

Smerkova, Kristyna; Dostalova, Simona; Vaculovicova, Marketa; Kynicky, Jindrich; Trnkova, Libuse; Kralik, Miroslav; Adam, Vojtech; Hubalek, Jaromir; Provaznik, Ivo; Kizek, Rene

2013-12-01

Nucleic acids belong to the most important molecules and therefore the understanding of their properties, function and behavior is crucial. Even though a range of analytical and biochemical methods have been developed for this purpose, one common step is essential for all of them - isolation of the nucleic acid from the from complex sample matrix. The use of magnetic particles for the separation of nucleic acids has many advantages over other isolation methods. In this study, an isolation procedure for extraction of DNA was optimized. Each step of the isolation process including washing, immobilization and elution was optimized and therefore the efficiency was increased from 1.7% to 28.7% and the total time was shortened from 75 to 30min comparing to the previously described method. Quantification of the particular parameter influence was performed by square-wave voltammetry using hanging drop mercury electrode. Further, we compared the optimized method with standard chloroform extraction and applied on isolation of DNA from Staphylococcus aureus and Escherichia coli. Copyright © 2013 Elsevier B.V. All rights reserved.

Development and Use of a Cyclic Voltammetry Simulator to Introduce Undergraduate Students to Electrochemical Simulations

ERIC Educational Resources Information Center

Brown, Jay H.

2015-01-01

Cyclic voltammetry (CV) is a popular technique for the study of electrochemical mechanisms because the method can provide useful information on the redox couple. The technique involves the application of a potential ramp on an unstirred solution while the current is monitored, and then the ramp is reversed for a return sweep. CV is sometimes…

Voltammetric Determination of Penicillamine Using a Carbon Paste Electrode Modified with Multiwall Carbon Nanotubes In the Presence of Methyldopa as a Mediator.

PubMed

Safari, Fardin; Keyvanfard, Mohsen; Karimi-Maleh, Hassan; Alizad, Khadijeh

2017-01-01

A multiwall carbon nanotubes-modified carbon paste electrode (MWCNTs/MCPE) was fabricated and used to study the electrooxidation of penicillamine (PA) by electrochemical methods in the presence of methyldopa (MDOP) as a homogeneous mediator. The electrochemical oxidation of PA on the new sensor has been carefully studied. The kinetic parameters such as electron transfer coefficient, α, and catalytic reaction rate constant, K / h , were also determined using electrochemical approaches. The electrocatalytic oxidation peak current of PA showed a linear dependent on the PA concentrations and linear calibration curves were obtained in the ranges of 0.2-250.0 µM of PA concentration with square wave voltammetry (SWV) method. The detection limit (3σ) was determined as 0.1 µM. This sensor was also examined as a fast, selective, simple and precise new sensor for voltammetric determination of PA in real samples such as drug and urine.

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

PubMed

Amare, Meareg; Abicho, Samuel; Admassie, Shimelis

2014-01-01

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

Voltammetric Determination of Penicillamine Using a Carbon Paste Electrode Modified with Multiwall Carbon Nanotubes In the Presence of Methyldopa as a Mediator

PubMed Central

Safari, Fardin; Keyvanfard, Mohsen; Karimi-Maleh, Hassan; Alizad, Khadijeh

2017-01-01

A multiwall carbon nanotubes-modified carbon paste electrode (MWCNTs/MCPE) was fabricated and used to study the electrooxidation of penicillamine (PA) by electrochemical methods in the presence of methyldopa (MDOP) as a homogeneous mediator. The electrochemical oxidation of PA on the new sensor has been carefully studied. The kinetic parameters such as electron transfer coefficient, α, and catalytic reaction rate constant, K/h, were also determined using electrochemical approaches. The electrocatalytic oxidation peak current of PA showed a linear dependent on the PA concentrations and linear calibration curves were obtained in the ranges of 0.2-250.0 µM of PA concentration with square wave voltammetry (SWV) method. The detection limit (3σ) was determined as 0.1 µM. This sensor was also examined as a fast, selective, simple and precise new sensor for voltammetric determination of PA in real samples such as drug and urine. PMID:29201090

Multistep Oxidation of Diethynyl Oligophenylamine-Bridged Diruthenium and Diiron Complexes.

PubMed

Zhang, Jing; Guo, Shen-Zhen; Dong, Yu-Bao; Rao, Li; Yin, Jun; Yu, Guang-Ao; Hartl, František; Liu, Sheng Hua

2017-01-17

Homo-dinuclear nonlinear complexes [{M(dppe)Cp*} 2 {μ-(-C≡C) 2 X}] (dppe = 1,2-bis(diphenylphosphino)ethane; Cp* = η 5 -C 5 Me 5 ; X = triphenylamine (TPA), M = Ru (1a) and Fe (1b); X = N,N,N',N'-tetraphenylphenylene-1,4-diamine (TPPD), M = Ru (2a)) were prepared and characterized by 1 H, 13 C, and 31 P NMR spectroscopy and single-crystal X-ray diffraction (1a, 2a). Attempts to prepare the diiron analogue of 2a were not successful. Experimental data obtained from cyclic voltammetry, square wave voltammetry, UV-vis-NIR (NIR = near-infrared) spectro-electrochemistry, and very informative IR spectro-electrochemistry in the C≡C stretching region, combined with density functional theory calculations, afford to make an emphasizing assessment of the close association between the metal-ethynyl termini and the oligophenylamine bridge core as well as their respective involvement in sequential one-electron oxidations of these complexes. The anodic behavior of the homo-bimetallic complexes depends strongly both on the metal center and the length of the oligophenylamine bridge core. The poorly separated first two oxidations of diiron complex 1b are localized on the electronically nearly independent Fe termini. In contrast, diruthenium complex 1a exhibits a significantly delocalized character and a marked electronic communication between the ruthenium centers through the diethynyl-TPA bridge. The ruthenium-ethynyl halves in 2a, separated by the doubly extended and more flexible TPPD bridge core, show a lower degree of electronic coupling, resulting in close-lying first two anodic waves and the NIR electronic absorption of [2a] + with an indistinctive intervalence charge transfer character. Finally, the third anodic waves in the voltammetric responses of the homo-bimetallic complexes are associated with the concurrent exclusive oxidation of the TPA or TPPD bridge cores.

Biophysical and electrochemical properties of Self-assembled noncovalent SWNT/DNA hybrid and electroactive nanostructure

NASA Astrophysics Data System (ADS)

Mirzapoor, Aboulfazl; Ranjbar, Bijan

2017-09-01

DNA self-assembled hybrid nanostructures are widely used in recent research in nanobiotechnology. Combination of DNA with carbon based nanoparticles such as single-walled carbon nanotube (SWNT), multi-walled carbon nanotube (MWNT) and carbon quantum dot were applied in important biological applications. Many examples of biosensors, nanowires and nanoelectronic devices, nanomachine and drug delivery systems are fabricated by these hybrid nanostructures. In this study, a new hybrid nanostructure has been fabricated by noncovalent interactions between single or double stranded DNA and SWNT nanoparticles and biophysical properties of these structures were studied comparatively. Biophysical properties of hybrid nanostructures studied by circular dichroism, UV-vis and fluorescence spectroscopy techniques. Also, electrochemical properties studied by cyclic voltammetry, linear sweep voltammetry, square wave voltammetry, choronoamperometry and impedance spectroscopy (EIS). Results revealed that the biophysical and electrochemical properties of SWNT/DNA hybrid nanostructures were different compare to ss-DNA, ds-DNA and SWNT singly. Circular dichroism results showed that ss-DNA wrapped around the nanotubes through π-π stacking interactions. The results indicated that after adding SWNT to ss-DNA and ds-DNA intensity of CD and UV-vis spectrum peaks were decreased. Electrochemical experiments indicated that the modification of single-walled carbon nanotubes by ss-DNA improves the electron transfer rate of hybrid nanostructures. It was demonstrated SWNT/DNA hybrid nanostructures should be a good electroactive nanostructure that can be used for electrochemical detection or sensing.

Direct Electrochemical Preparation of Cobalt, Tungsten, and Tungsten Carbide from Cemented Carbide Scrap

NASA Astrophysics Data System (ADS)

Xiao, Xiangjun; Xi, Xiaoli; Nie, Zuoren; Zhang, Liwen; Ma, Liwen

2017-02-01

A novel process of preparing cobalt, tungsten, and tungsten carbide powders from cemented carbide scrap by molten salt electrolysis has been investigated in this paper. In this experiment, WC-6Co and NaCl-KCl salt were used as sacrificial anode and electrolyte, respectively. The dissolution potential of cobalt and WC was determined by linear sweep voltammetry to be 0 and 0.6 V ( vs Ag/AgCl), respectively. Furthermore, the electrochemical behavior of cobalt and tungsten ions was investigated by a variety of electrochemical techniques. Results of cyclic voltammetry (CV) and square-wave voltammetry show that the cobalt and tungsten ions existed as Co2+ and W2+ on melts, respectively. The effect of applied voltage, electrolysis current, and electrolysis times on the composition of the product was studied. Results showed that pure cobalt powder can be obtained when the electrolysis potential is lower than 0.6 V or during low current and short times. Double-cathode and two-stage electrolysis was utilized for the preparation of cobalt, tungsten carbide, and tungsten powders. Additionally, X-ray diffraction results confirm that the product collected at cathodes 1 and 2 is pure Co and WC, respectively. Pure tungsten powder was obtained after electrolysis of the second part. Scanning electron microscope results show that the diameters of tungsten, tungsten carbide, and cobalt powder are smaller than 100, 200, and 200 nm, respectively.

Electrochemical Sensors for In Situ Phosphate and Nitrate Measurements in Seawater

NASA Astrophysics Data System (ADS)

Romanytsia, I.; Chen Legrand, D.; Barus, C.; Striebig, N.; Garcon, V.

2016-02-01

Monitoring the evolution of concentrations of dissolved inorganic nutrients, like phosphate and nitrate, provides insights on the oceanic biogeochemical cycles. This long term monitoring is key to investigate how changing oceanic conditions will alter biogeochemical cycles. We report here the latest development and analytical method to measure phosphate and nitrate concentrations in seawater without any addition of liquid reagents. We propose to use a derivative electrochemical method such as Square Wave Voltammetry (SWV) to detect phosphomolybdic complex and nitrate as this method offers a higher sensitivity than classical cyclic voltammetry and avoids the need of stirring the solution like for chronoamperometry technique. Phosphate is a non-electroactive species and its determination is performed by measuring its corresponding phosphomolybdic complex formed in situ after oxidation of two molybdenum electrodes placed into two different compartments connected with a proton-exchange membrane. [1]. All the SWV parameters such as step potential, amplitude and frequency have been determined to detect phosphomolybdic complex as fast as possible and with the lowest limit of detection. Depending on the frequency used, two calibration curves have been obtained for two phosphate concentration ranges: 0.07-1.06 µM (250 Hz) and 0.5-6 µM (2.5 Hz). We are currently working to adapt those parameters to laboratory prototype and results obtained will be presented. On the other hand, nitrate can be detected directly on gold electrode modified with silver nanoparticles (AgNPs) where the nitrate reduction process can be easily measured at -0.97 V [2]. This method allows to obtain good calibration curves with a detection limit of 10 nM, very short measuring time (2.8 s) and long life time of the modified electrode (minimum 47 days storage in seawater). [1] Jonca et al., Electrochimica Acta 88 (2013) 165-169 [2] Fajerwerg et al., Electrochem. Commun. 12 (2010) 1439-1441

Electrochemically driven catalysis of Rhizobium sp. NT-26 arsenite oxidase with its native electron acceptor cytochrome c552.

PubMed

Kalimuthu, Palraj; Heath, Matthew D; Santini, Joanne M; Kappler, Ulrike; Bernhardt, Paul V

2014-01-01

We describe the catalytic voltammograms of the periplasmic arsenite oxidase (Aio) from the chemolithoautotrophic bacterium Rhizobium sp. str. NT-26 that oxidizes arsenite to arsenate. Electrochemistry of the enzyme was accomplished using its native electron transfer partner, cytochrome c552 (cyt c552), as a mediator. The protein cyt c552 adsorbed on a mercaptoundecanoic acid (MUA) modified Au electrode exhibited a stable, reversible one-electron voltammetric response at +275mV vs NHE (pH6). In the presence of arsenite and Aio the voltammetry of cyt c552 is transformed from a transient response to an amplified sigmoidal (steady state) wave consistent with an electro-catalytic system. Digital simulation was performed using a single set of parameters for all catalytic voltammetries obtained at different sweep rates and various substrate concentrations. The obtained kinetic constants from digital simulation provide new insight into the kinetics of the NT-26 Aio catalytic mechanism. © 2013.

The Cathodic Behavior of Ti(III) Ion in a NaCl-2CsCl Melt

NASA Astrophysics Data System (ADS)

Song, Yang; Jiao, Shuqiang; Hu, Liwen; Guo, Zhancheng

2016-02-01

The cathodic behavior of Ti(III) ions in a NaCl-2CsCl melt was investigated by cyclic voltammetry, chronopotentiometry, and square wave voltammetry with a tungsten electrode being the working electrode at different temperatures. The results show that the cathodic behavior of Ti(III) ion consists of two irreversible steps: Ti3+ + e = Ti2+ and Ti2+ + 2 e = Ti. The diffusion coefficient for the Ti(III) ion in the NaCl-2CsCl eutectic is 1.26 × 10-5 cm2 s-1 at 873 K (600 °C), increases to be 5.57 × 10-5 cm2 s-1 at 948K (675°C), and further rises to 10.8 × 10-5 cm2 s-1 at 1023 (750 °C). Moreover, galvanostatic electrolysis performed on a titanium electrode further presents the feasibility of electrodepositing metallic titanium in the molten NaCl-2CsCl-TiCl3 system.

Determination of allura red in some food samples by adsorptive stripping voltammetry.

PubMed

Alghamdi, Ahmad H

2005-01-01

Square wave (SW) voltammetry was used to explore the adsorption properties of the food additive dye Allura Red on a hanging mercury drop electrode (HMDE). By using the adsorptive stripping voltammetric approach, we developed a sensitive electroanalytical method for the determination of this azo dye. A well-developed voltammetric peak probably related to the cathodic reduction of the azo moiety was obtained in pH 9 Britton-Robinson (B-R) buffer at 613 mV. Cyclic voltammetric studies indicated that the reduction process was irreversible and primarily controlled by adsorption. The adsorptive voltammetric signal was evaluated with respect to various experimental conditions; the optimized values were supporting electrolyte, B-R buffer; pH 11; accumulation time, 180 s; accumulation potential, 0.0 V; scan rate, 900 mV/s; pulse amplitude, 75 mV; and SW frequency, 90 Hz. Adsorptive voltammetric peak current showed a linear response for Allura Red in the concentration range of 2.5 x 10(-8) to 2.0 x 10(-7) mol/L (r = 0.998). The limit of detection was 8.5 x 10(-9) mol/L (4.2 ng/mL), the precision in terms of relative standard deviation was 1.3%, and the mean recovery was 102%. Possible interferences by several substances usually present in food products such as food additive azo dyes (E110, E102), gelatin, natural and artificial sweeteners, preservatives, and antioxidants were also evaluated. The proposed electrochemical procedure was successfully applied to the determination of this food dye in commercially available candy and a soft drink. The results were compared by statistical evaluation with those obtained by a reference spectrophotometric method.

Embedded Disposable Functionalized Electrochemical Biosensor with a 3D-Printed Flow Cell for Detection of Hepatic Oval Cells (HOCs)

PubMed Central

Peacock, Martin; Leonhardt, Stefan; Damiati, Laila; Baghdadi, Mohammed A.; Schuster, Bernhard

2018-01-01

Hepatic oval cells (HOCs) are considered the progeny of the intrahepatic stem cells that are found in a small population in the liver after hepatocyte proliferation is inhibited. Due to their small number, isolation and capture of these cells constitute a challenging task for immunosensor technology. This work describes the development of a 3D-printed continuous flow system and exploits disposable screen-printed electrodes for the rapid detection of HOCs that over-express the OV6 marker on their membrane. Multiwall carbon nanotube (MWCNT) electrodes have a chitosan film that serves as a scaffold for the immobilization of oval cell marker antibodies (anti-OV6-Ab), which enhance the sensitivity of the biomarker and makes the designed sensor specific for oval cells. The developed sensor can be easily embedded into the 3D-printed flow cell to allow cells to be exposed continuously to the functionalized surface. The continuous flow is intended to increase capture of most of the target cells in the specimen. Contact angle measurements were performed to characterize the nature and quality of the modified sensor surface, and electrochemical measurements (cyclic voltammetry (CV) and square wave voltammetry (SWV)) were performed to confirm the efficiency and selectivity of the fabricated sensor to detect HOCs. The proposed method is valuable for capturing rare cells and could provide an effective tool for cancer diagnosis and detection. PMID:29443890

Molecularly imprinted polymer nanoparticles-based electrochemical sensor for determination of diazinon pesticide in well water and apple fruit samples.

PubMed

Motaharian, Ali; Motaharian, Fatemeh; Abnous, Khalil; Hosseini, Mohammad Reza Milani; Hassanzadeh-Khayyat, Mohammad

2016-09-01

In this research, an electrochemical sensor based on molecularly imprinted polymer (MIP) nanoparticles for selective and sensitive determination of diazinon (DZN) pesticides was developed. The nanoparticles of diazinon imprinted polymer were synthesized by suspension polymerization and then used for modification of carbon paste electrode (CPE) composition in order to prepare the sensor. Cyclic voltammetry (CV) and square wave voltammetry (SWV) methods were applied for electrochemical measurements. The obtained results showed that the carbon paste electrode modified by MIP nanoparticles (nano-MIP-CP) has much higher adsorption ability for diazinon than the CPE based non-imprinted polymer nanoparticles (nano-NIP-CP). Under optimized extraction and analysis conditions, the proposed sensor exhibited excellent sensitivity (95.08 μA L μmol(-1)) for diazinon with two linear ranges of 2.5 × 10(-9) to 1.0 × 10(-7) mol L(-1) (R (2) = 0.9971) and 1.0 × 10(-7) to 2.0 × 10(-6) mol L(-1) (R (2) = 0.9832) and also a detection limit of 7.9 × 10(-10) mol.L(-1). The sensor was successfully applied for determination of diaznon in well water and apple fruit samples with recovery values in the range of 92.53-100.86 %. Graphical abstract Procedure for preparation of electrochemical sensor based on MIP nanoparticles for determination of diazinon.

Electrochemical oxidation and electroanalytical determination of xylitol at a boron-doped diamond electrode.

PubMed

Lourenço, Anabel S; Sanches, Fátima A C; Magalhães, Renata R; Costa, Daniel J E; Ribeiro, Williame F; Bichinho, Kátia M; Salazar-Banda, Giancarlo R; Araújo, Mário C U

2014-02-01

Xylitol is a reduced sugar with anticariogenic properties used by insulin-dependent diabetics, and which has attracted great attention of the pharmaceutical, cosmetics, food and dental industries. The detection of xylitol in different matrices is generally based on separation techniques. Alternatively, in this paper, the application of a boron-doped diamond (BDD) electrode allied to differing voltammetric techniques is presented to study the electrochemical behavior of xylitol, and to develop an analytical methodology for its determination in mouthwash. Xylitol undergoes two oxidation steps in an irreversible diffusion-controlled process (D=5.05 × 10(-5)cm(2)s(-1)). Differential pulse voltammetry studies revealed that the oxidation mechanism for peaks P1 (3.4 ≤ pH ≤ 8.0), and P2 (6.0 ≤ pH ≤ 9.0) involves transfer of 1H(+)/1e(-), and 1e(-) alone, respectively. The oxidation process P1 is mediated by the (•)OH generated at the BDD hydrogen-terminated surface. The maximum peak current was obtained at a pH of 7.0, and the electroanalytical method developed, (employing square wave voltammetry) yielded low detection (1.3 × 10(-6) mol L(-1)), and quantification (4.5 × 10(-6) mol L(-1)) limits, associated with good levels of repeatability (4.7%), and reproducibility (5.3%); thus demonstrating the viability of the methodology for detection of xylitol in biological samples containing low concentrations. © 2013 Elsevier B.V. All rights reserved.

Cyclic Voltammetric Wave-Shapes for Microdisk Electrodes: Coupled Effects of Solution Resistance, Double-Layer Capacitance, and Finite Electrochemical Kinetics

DTIC Science & Technology

1991-05-01

vaveshapea. While the use of high scan rates enhances the effect of electrode kinetics upon the voltametry , the deleterious coupled influence of pa 20...waveshapes. While the use of high scan rates enhances the effect of electrode kinetics upon the voltametry , the deleterious coupled influence of P...2 1 󈧚 Aoki et al have in- 23 vestigated linear sweep voltammetry at microdisks in the reversible case, and Zoski and co-workers have developed

Electrochemical behavior of phytochelatins and related peptides at the hanging mercury drop electrode in the presence of cobalt(II) ions.

PubMed

Dorcák, Vlastimil; Sestáková, Ivana

2006-01-01

Direct current voltammetry and differential pulse voltammetry have been used to investigate the electrochemical behaviour of two phytochelatins: heptapeptide (gamma-Glu-Cys)3-Gly and pentapeptide (gamma-Glu-Cys)2-Gly, tripeptide glutathione gamma-Glu-Cys-Gly and its fragments: dipeptides Cys-Gly and gamma-Glu-Cys at the hanging mercury drop electrode in the presence of cobalt(II) ions. Most interesting results were obtained with direct current voltammetry in the potential region of -0.80 V up to -1.80 V. Differential pulse voltammetry of the same solutions of Co(II) with peptides gives more complicated voltammograms with overlapping peaks, probably in connection with the influence of adsorption at slow scan rates necessarily used in this method. However, in using Brdicka catalytic currents for analytical purposes, differential pulse voltammograms seem to be more helpful. Presented investigations have shown that particularly the prewave of cobalt(II) allows distinguishing among phytochelatins, glutathione, and its fragments.

Conditioning of renewable silver amalgam film electrode for the characterization of clothianidin and its determination in selected samples by adsorptive square-wave voltammetry.

PubMed

Brycht, Mariola; Skrzypek, Sławomira; Guzsvány, Valéria; Berenji, Janoš

2013-12-15

A new square-wave adsorptive stripping voltammetric (SWAdSV) method was developed for the determination of the neonicotinoid insecticide clothianidin (Clo), based on its reduction at a renewable silver amalgam film electrode (Hg(Ag)FE). The key point of the procedure is the pretreatment of the Hg(Ag)FE by applying the appropriate conditioning potential (-1.70 V vs. Ag/AgCl reference electrode). Under the optimized voltammetric conditions, such pretreatment resulted in the peak for the Clo reduction in Britton-Robinson buffer pH 9.0 at about -0.60 V, which was used for the analytical purpose. The developed SWAdSV procedure made it possible to determine Clo in the concentration range of 6.0×10(-7)-7.0×10(-6) mol L(-1) (LOD=1.8×10(-7) mol L(-1), LOQ=6.0×10(-7) mol L(-1)) and 7.0×10(-6)-4.0×10(-5) mol L(-1) (LOD=1.3×10(-6) mol L(-1), LOQ=4.2×10(-6) mol L(-1)). The repeatability, precision, and the recovery of the method were determined. The effect of common interfering pesticides was also investigated. Standard addition method was successfully applied and validated for the determination of Clo in spiked Warta River water, corn seeds samples, and in corn seeds samples treated with the commercial formulation PONCHO 600 FS. © 2013 Elsevier B.V. All rights reserved.

Polytetrafluorethylene film-based liquid-three phase micro extraction coupled with differential pulse voltammetry for the determination of atorvastatin calcium.

PubMed

Ensafi, Ali A; Khoddami, Elaheh; Rezaei, Behzad

2013-01-01

In this paper, we describe a new combination method based on polytetrafluorethylene (PTFE) film-based liquid three-phase micro extraction coupled with differential pulse voltammetry (DPV) for the micro extraction and quantification of atorvastatin calcium (ATC) at the ultra-trace level. Different factors affecting the liquid-three phases micro extraction of atorvastatin calcium, including organic solvent, pH of the donor and acceptor phases, concentration of salt, extraction time, stirring rate and electrochemical factors, were investigated, and the optimal extraction conditions were established. The final stable signal was achieved after a 50 min extraction time, which was used for analytical applications. An enrichment factor of 21 was achieved, and the relative standard deviation (RSD) of the method was 4.5% (n = 4). Differential pulse voltammetry exhibited two wide linear dynamic ranges of 20.0-1000.0 pmol L(-1) and 0.001-11.0 µmol L(-1) of ATC. The detection limit was found to be 8.1 pmol L(-1) ATC. Finally, the proposed method was used as a new combination method for the determination of atorvastatin calcium in real samples, such as human urine and plasma.

Electrochemical detection of phenolic estrogenic compounds at clay modified carbon paste electrode

NASA Astrophysics Data System (ADS)

Belkamssa, N.; Ouattara, L.; Kawachi, A.; Tsujimura, M.; Isoda, H.; Chtaini, A.; Ksibi, M.

2015-04-01

A simple and sensitive electroanalytical method was developed to determine the Endocrine Disrupting chemical 4-tert-octylphenol on clay modified carbon paste electrode (Clay/CPE). The electrochemical response of the proposed electrode was studied by means of cyclic and square wave voltammetry. It has found that the oxidation of 4-tert-octylphenol on the clay/CPE displayed a well-defined oxidation peak. Under these optimal conditions, a linear relation between concentrations of 4-tert-octylphenol current response was obtained over range of 7.26×10-6 to 3.87×10-7 with a detection and quantification limit of 9.2×10-7 M and 3.06×10-6 M, respectively. The correlation coefficient is 0.9963. The modified electrode showed suitable sensitivity, high stability and an accurate detection of 4-tert-octylphenol. The modified electrode also relevant suitable selectivity for various phenolic estrogenic compounds.

An ambient stable core-substituted perylene bisimide dianion: isolation and single crystal structure analysis† †Electronic supplementary information (ESI) available: Synthesis, spectroelectrochemistry, UV-vis, electrochemistry, X-ray diffraction, NMR and mass spectra. CCDC 1032959. For ESI and crystallographic data in CIF or other electronic format see DOI: 10.1039/c4sc03671a Click here for additional data file. Click here for additional data file.

PubMed Central

Seifert, Sabine; Schmidt, David

2015-01-01

Here we report the first example of an isolable, ambient stable perylene bisimide (PBI) dianion which was synthesized by catalytic reduction of a highly electron deficient PBI derivative. The remarkable stability of this unprecedented dianion in air for months facilitated its complete characterization by different methods, including single crystal X-ray analysis. Furthermore, solvent dependent cyclic and square wave voltammetry studies revealed that the formation of PBI dianions is preferred in more polar solvents, whereas the generation of PBI radical anions should be favoured in less polar solvents. PMID:28717450

Determination of low levels of cadmium ions by the under potential deposition on a self-assembled monolayer on gold electrode.

PubMed

Noyhouzer, Tomer; Mandler, Daniel

2011-01-17

The electrochemical determination of low levels of Cd using a self-assembled monolayer (SAM) modified Au electrode is reported. Determination was based on the stripping of Cd, which was deposited by under potential deposition (UPD). A series of short alkanethiol SAMs bearing different end groups, i.e., sulfonate, carboxylate and ammonium, were examined. Lowest level of detection (ca. 50 ngL(-1)) was achieved with a 3-mercaptopropionic acid (MPA) monolayer using subtractive anodic square wave voltammetry (SASV). Additional surface methods, namely, reductive desorption and X-ray photoelectron spectroscopy, were applied to determine the interfacial structure of the electrodeposited Cd on the modified electrodes. We conclude that the deposited Cd forms a monoatomic layer, which bridges between the gold surface and the alkanethiol monolayer associating with both the gold and the sulfur atoms. Copyright © 2010 Elsevier B.V. All rights reserved.

Conditions and chemometrics for the determination of heavy metals in natural and waste waters by stripping voltammetry with UV irradiation

DOE Office of Scientific and Technical Information (OSTI.GOV)

Volkova, V.N.; Zakharova, E.A.; Khustenko, L.A.

The number of supporting electrolytes for stripping voltammetry with photochemical oxygen deactivation was broadened. The following agents are recommended: formic, lactic, tartaric, citric, and malonic acids at pH 2-4; salts of lactic, tartaric, and citric acids at pH 6-7; and salts of lactic, tartaric, citric, and glutaric acids at pH 12-14. A rapid method was developed for simultaneously determining Zn, Cd, Pb, and Cu in a 0.5 M formic acid supporting electrolyte. The method is chemometrically sound and cost-effective.

Evaluation of seven cosubstrates in the quantification of horseradish peroxidase enzyme by square wave voltammetry.

PubMed

Kergaravat, Silvina V; Pividori, Maria Isabel; Hernandez, Silvia R

2012-01-15

The electrochemical detection for horseradish peroxidase-cosubstrate-H(2)O(2) systems was optimized. o-Phenilendiamine, phenol, hydroquinone, pyrocatechol, p-chlorophenol, p-aminophenol and 3,3'-5,5'-tetramethylbenzidine were evaluated as cosubstrates of horseradish peroxidase (HRP) enzyme. Therefore, the reaction time, the addition sequence of the substrates, the cosubstrate:H(2)O(2) ratio and the electrochemical techniques were elected by one-factor optimization assays while the buffer pH, the enzymatic activity and cosubstrate and H(2)O(2) concentrations for each system were selected simultaneously by response surface methodology. Then, the calibration curves for seven horseradish peroxidase-cosubstrate-H(2)O(2) systems were built and the analytic parameters were analyzed. o-Phenilendiamine was selected as the best cosubstrate for the HRP enzyme. For this system the reaction time of 60s, the phosphate buffer pH 6.0, and the concentrations of 2.5×10(-4)molL(-1) o-phenilendiamine and of 1.25×10(-4)molL(-1) H(2)O(2) were chosen as the optimal conditions. In these conditions, the calibration curve of horseradish peroxidase by square wave voltammetry showed a linearity range from 9.5×10(-11) to 1.9×10(-8)molL(-1) and the limit of detection of 3.8×10(-11)molL(-1) with RSD% of 0.03% (n=3). Copyright © 2011 Elsevier B.V. All rights reserved.

Simultaneous determination of L-ascorbic acid, dopamine and uric acid with gold nanoparticles-β-cyclodextrin-graphene-modified electrode by square wave voltammetry.

PubMed

Tian, Xianqing; Cheng, Changming; Yuan, Hongyan; Du, Juan; Xiao, Dan; Xie, Shunping; Choi, Martin M F

2012-05-15

Graphene decorated with gold nanoparticles (AuNPs-β-CD-Gra) has been synthesized by in situ thermal reduction of graphene oxide and HAuCl(4) with β-cyclodextrin (β-CD) under alkaline condition. The AuNPs-β-CD-Gra product was well characterized by infrared spectroscopy, X-ray powder diffraction, scanning electron microscopy, high-resolution transmission electron microscopy, and selected area electron diffraction. This material was used to fabricate an AuNPs-β-CD-Gra-modified glassy carbon electrode (GCE) which showed excellent electro-oxidation of l-ascorbic acid (AA), dopamine (DA) and uric acid (UA) in 0.10 M NaH(2)PO(4)-HCl buffer solution (pH 2.0) by square wave voltammetry (SWV). Three well-resolved oxidation peaks of AA and DA and UA were obtained. The AuNPs-β-CD-Gra/GCE exhibits linear responses to AA, DA and UA in the ranges 30-2000, 0.5-150 and 0.5-60 μM, respectively. The detection limits (based on S/N=3 and preconcentration time=3.0 min) for AA, DA and UA are 10, 0.15 and 0.21 μM, respectively. The AuNPs-β-CD-Gra/GCE has been successfully applied to determine UA in human urine with satisfactory results. Our work provides a simple, convenient and green route to synthesize AuNPs on Gra which is potentially useful in electroanalysis. Copyright © 2012 Elsevier B.V. All rights reserved.

Electrochemical Determination of Food Preservative Nitrite with Gold Nanoparticles/p-Aminothiophenol-Modified Gold Electrode

PubMed Central

Üzer, Ayşem; Sağlam, Şener; Can, Ziya; Erçağ, Erol; Apak, Reşat

2016-01-01

Due to the negative impact of nitrate and nitrite on human health, their presence exceeding acceptable levels is not desired in foodstuffs. Thus, nitrite determination at low concentrations is a major challenge in electroanalytical chemistry, which can be achieved by fast, cheap, and safe electrochemical sensors. In this work, the working electrode (Au) was functionalized with p-aminothiophenol (p-ATP) and modified with gold nanoparticles (Au-NPs) to manufacture the final (Au/p-ATP-Aunano) electrode in a two-step procedure. In the first step, p-ATP was electropolymerized on the electrode surface to obtain a polyaminothiophenol (PATP) coating. In the second step, Au/p-ATP-Aunano working electrode was prepared by coating the surface with the use of HAuCl4 solution and cyclic voltammetry. Determination of aqueous nitrite samples was performed with the proposed electrode (Au/p-ATP-Aunano) using square wave voltammetry (SWV) in pH 4 buffer medium. Characteristic peak potential of nitrite samples was 0.76 V, and linear calibration curves of current intensity versus concentration was linear in the range of 0.5–50 mg·L−1 nitrite with a limit of detection (LOD) of 0.12 mg·L−1. Alternatively, nitrite in sausage samples could be colorimetrically determined with high sensitivity by means of p-ATP‒modified gold nanoparticles (AuNPs) and naphthylethylene diamine as coupling agents for azo-dye formation due to enhanced charge-transfer interactions with the AuNPs surface. The slopes of the calibration lines in pure NO2− solution and in sausage sample solution, to which different concentrations of NO2− standards were added, were not significantly different from each other, confirming the robustness and interference tolerance of the method. The proposed voltammetric sensing method was validated against the colorimetric nanosensing method in sausage samples. PMID:27490543

Trace level and highly selective determination of urea in various real samples based upon voltammetric analysis of diacetylmonoxime-urea reaction product on the carbon nanotube/carbon paste electrode.

PubMed

Alizadeh, Taher; Ganjali, Mohammad Reza; Rafiei, Faride

2017-06-29

In this study an innovative method was introduced for selective and precise determination of urea in various real samples including urine, blood serum, soil and water. The method was based on the square wave voltammetry determination of an electroactive product, generated during diacetylmonoxime reaction with urea. A carbon paste electrode, modified with multi-walled carbon nanotubes (MWCNTs) was found to be an appropriate electrochemical transducer for recording of the electrochemical signal. It was found that the chemical reaction conditions influenced the analytical signal directly. The calibration graph of the method was linear in the range of 1 × 10 -7 - 1 × 10 -2  mol L -1 . The detection limit was calculated to be 52 nmol L -1 . Relative standard error of the method was also calculated to be 3.9% (n = 3). The developed determination procedure was applied for urea determination in various real samples including soil, urine, plasma and water samples. Copyright © 2017 Elsevier B.V. All rights reserved.

Design of a dual-mode electrochemical measurement and analysis system.

PubMed

Yang, Jr-Fu; Wei, Chia-Ling; Wu, Jian-Fu; Liu, Bin-Da

2013-01-01

A dual-mode electrochemical measurement and analysis system is proposed. This system includes a dual-mode chip, which was designed and fabricated by using TSMC 0.35 µm 3.3 V/5 V 2P4M mixed-signal CMOS process. Two electrochemical measurement and analysis methods, chronopotentiometry and voltammetry, can be performed by using the proposed chip and system. The proposed chip and system are verified successfully by performing voltammetry and chronopotentiometry on solutions.

A pipette-based calibration system for fast-scan cyclic voltammetry with fast response times.

PubMed

Ramsson, Eric S

2016-01-01

Fast-scan cyclic voltammetry (FSCV) is an electrochemical technique that utilizes the oxidation and/or reduction of an analyte of interest to infer rapid changes in concentrations. In order to calibrate the resulting oxidative or reductive current, known concentrations of an analyte must be introduced under controlled settings. Here, I describe a simple and cost-effective method, using a Petri dish and pipettes, for the calibration of carbon fiber microelectrodes (CFMs) using FSCV.

Synthesis and characterization of graphene quantum dots-silver nanocomposites

NASA Astrophysics Data System (ADS)

Vandana, M.; Ashokkumar, S. P.; Vijeth, H.; Niranjana, M.; Yesappa, L.; Devendrappa, H.

2018-04-01

A facile microwave assisted hydrothermal method is used to synthesise glucose derived water soluble crystalline graphene quantum dots (GQDs) andcitrate reduction method was used to synthesized silver nanoparticles (SNPs). The formation of graphene quantum dots-silver nanocomposites (GSC) was synthesized through a simple refluxing process and characterised using Fourier Transform Infrared (FT-IR) to study the chemical interaction, Surface morphology using FESEM, Optical properties were studied using UV-Visible spectroscopy. The absorption band shows at 249, 306 and 447 nm confirms the formation of GQDs and GSC. The electrochemical performance of GSC tested to determine the oxidation/reduction processes by cyclic voltammetry and linear sweep voltammetry.

Determination of trace mercury in water based on N-octylpyridinium ionic liquids preconcentration and stripping voltammetry.

PubMed

Li, Zhenhan; Xia, Shanhong; Wang, Jinfen; Bian, Chao; Tong, Jianhua

2016-01-15

A novel method for determination of trace mercury in water is developed. The method is performed by extracting mercury firstly with ionic liquids (ILs) and then detecting the concentration of mercury in organic media with anodic stripping voltammetry. Liquid-liquid extraction of mercury(II) ions by four ionic liquids with N-octylpyridinium cations ([OPy](+)) was studied. N-octylpyridinium tetrafluoroborate and N-octylpyridinium trifluoromethylsulfonate were found to be efficient and selective extractant for mercury. Temperature controlled dispersive liquid phase microextraction (TC-DLPME) technique was utilized to improve the performance of preconcentration. After extraction, precipitated IL was diluted by acetonitrile buffer and mercury was detected by differential pulse stripping voltammetry (DPSV) with gold disc electrode. Mercury was enriched by 17 times while interfering ions were reduced by two orders of magnitude in the organic media under optimum condition. Sensitivity and selectivity for electrochemical determination of mercury were improved by using the proposed method. Tap, pond and waste water samples were analyzed with recoveries ranging from 81% to 107% and detection limit of 0.05 μg/L. Copyright © 2015 Elsevier B.V. All rights reserved.

Electrochemistry and electrocatalysis of myoglobin immobilized in sulfonated graphene oxide and Nafion films.

PubMed

Chen, Guiying; Sun, Hong; Hou, Shifeng

2016-06-01

In this study, sulfonated graphene oxide (SGO) was synthesized and characterized by Fourier transform infrared (FT-IR) spectroscopy and X-ray photoelectron spectroscopy (XPS). It was used to make Mb-SGO-Nafion composite films by coating myoglobin (Mb) on the glassy carbon electrodes (GCE). Positions of the Soret absorption bands suggested that Mb retained its native conformation in the films. Mb-SGO-Nafion film modified electrode showed a pair of well-defined and nearly reversible cyclic voltammetry peaks at around -0.39 V versus saturated calomel electrode (SCE) in pH 7.0 buffers, characteristic of heme Fe(III)/Fe(II) redox couples. Electrochemical parameters such as electron transfer rate constant (ks) and formal potential (E(o')) were estimated by fitting the data of square-wave voltammetry with nonlinear regression analysis. Experimental data demonstrated that the electron transfer between Mb and electrode was greatly facilitated and showed good electrocatalytic properties toward various substrates, such as H2O2 and NaNO2, with significant lowering of reduction overpotential. Copyright © 2016. Published by Elsevier Inc.

Electrodeposited nitrogen-doped graphene/carbon nanotubes nanocomposite as enhancer for simultaneous and sensitive voltammetric determination of caffeine and vanillin.

PubMed

Jiang, Lin; Ding, Yaping; Jiang, Feng; Li, Li; Mo, Fan

2014-06-23

A nitrogen-doped graphene/carbon nanotubes (NGR-NCNTs) nanocomposite was employed into the study of the electrochemical sensor via electrodeposition for the first time. The morphology and structure of NGR-NCNTs nanocomposite were investigated by scanning electron microscopy (SEM) and transmission electron microscopy (TEM), respectively. Meanwhile, the electrochemical performance of the glassy carbon electrode (GCE) modified with electrodeposited NGR-NCNTs (ENGR-NCNTs/GCE) towards caffeine (CAF) and vanillin (VAN) determination was demonstrated by cyclic voltammetry (CV) and square wave voltammetry (SWV). Under optimal condition, ENGR-NCNTs/GCE exhibited a wide linearity of 0.06-50 μM for CAF and 0.01-10 μM for VAN with detection limits of 0.02 μM and 3.3×10(-3) μM, respectively. Furthermore, the application of the proposed sensor in food products was proven to be practical and reliable. The desirable results show that the ENGR-NCNTs nanocomposite has promising potential in electrocatalytic biosensor application. Copyright © 2014 Elsevier B.V. All rights reserved.

Electrocatalytic effect of polyvinyl pyrrolidone capped platinum nanoparticles electrodeposited on platinum electrode for ammonia oxidation

NASA Astrophysics Data System (ADS)

Mayedwa, Noluthando; Matinise, Nolubabalo; Mongwaketsi, Nametso; Maaza, Malik

2018-05-01

The aim of this work was to study structural and kinetic parameters as well as the mechanism of platinum nanoparticles (PtNP) reduced with sodium borohydride (NaBH4) and capped with polyvinyl pyrrolidone (PVP). The nanoparticles were supported on Pt electrode for ammonia oxidation in fuel cell application. X-ray diffraction (XRD) was used to study structural composition and high resolution transmission electron microscopy (HRTEM) was used for morphological study of the nanoalloy. The electrocatalysts were studied in alkaline solution of potassium hydroxide (KOH) by cyclic voltammetry (CV), square wave voltammetry (SWV) and electrochemical impedance spectroscopy (EIS). CV showed that the ammonia oxidation over potential for PtNP was -431 mV and with exchange current density of 1.726 × 10-4 A. EIS showed that the charge transfer resistance (Rct) of PtNP was the lowest (Rct = 1.943 × 106 Ω) compared to that of bare Pt working electrode (2.0604 × 106 Ω), indicating that the Pt nanoparticles have good conductivity and played an important role in accelerating the transfer of electrons.

Synthesis of ZnO nanorods and their application in the construction of a nanostructure-based electrochemical sensor for determination of levodopa in the presence of carbidopa.

PubMed

Molaakbari, Elahe; Mostafavi, Ali; Beitollahi, Hadi; Alizadeh, Reza

2014-09-07

A novel carbon paste electrode modified with ZnO nanorods and 5-(4'-amino-3'-hydroxy-biphenyl-4-yl)-acrylic acid (3,4'-AAZCPE) was fabricated. The electrochemical study of the modified electrode, as well as its efficiency for the electrocatalytic oxidation of levodopa, is described. The electrode was employed to study the electrocatalytic oxidation of levodopa, using cyclic voltammetry (CV), chronoamperometry (CHA), and square-wave voltammetry (SWV) as diagnostic techniques. It has been found that the oxidation of levodopa at the surface of the modified electrode occurs at a potential of about 370 mV less positive than that of an unmodified carbon paste electrode. The SWV results exhibit a linear dynamic range from 1.0 × 10(-7) M to 7.0 × 10(-5) M and a detection limit of 3.5 × 10(-8) M for levodopa. In addition, this modified electrode was used for the simultaneous determination of levodopa and carbidopa. Finally, the modified electrode was used for the determination of levodopa and carbidopa in some real samples.

Linear scan voltammetric indirect determination of Al(III) by the catalytic cathodic response of norepinephrine at the hanging mercury drop electrode.

PubMed

Zhang, Fuping; Ji, Ming; Xu, Quan; Yang, Li; Bi, Shuping

2005-09-01

The biological effects of aluminum (Al) have received much attention in recent years. Al is of basic relevance as concern with its reactivity and bioavailability. In this paper, the electrochemical behaviors of norepinephrine (NE) in the absence and presence of Al(III) at the hanging mercury drop electrode have been studied and applied to the practical analysis. Highly selective catalytic cathodic peak of NE is yielded by linear scan voltammetry (LSV) at -1.32 V (vs. SCE). A linear relationship holds between the cathodic peak current and the Al(III) concentration. It has been successfully applied to the determination of Al(III) in real waters and synthetic biological samples with satisfying results, which are in accordance with those obtained by ICP-AES method. The electrochemical properties and the mechanisms of the peaks in the presence and absence of Al(III) have been explored. The results show that they are irreversible adsorptive hydrogen catalytic waves. These studies not only enrich the methods of determining Al, but also lay foundations of further understanding of the mechanisms of neurodementia.

Voltammetric detection of the α-dicarbonyl compound: methylglyoxal as a flavoring agent in wine and beer.

PubMed

Chatterjee, Sanghamitra; Chen, Aicheng

2012-11-02

A simple, rapid and highly selective method for the determination of the most abundant α-dicarbonyl compound in wine and beer has been developed for the first time by employing square wave voltammetry. A novel electrochemical sensor, based on the electrodeposition of platinum nanoparticles onto single wall carbon nanotubes that were cast on a glassy carbon electrode (GCE) substrate, is presented in this paper. This modified electrode exhibited excellent catalytic activity in the electroreduction of methylglyoxal, showing much higher peak currents than those measured on an unmodified GCE. The effects of different experimental and instrumental parameters, such as solution pH and square wave frequency, were examined. The reduction peak current showed a linear range of from 0.1×10(-6) to 100×10(-6)M with a 0.9979 correlation coefficient; and a low detection limit of 2.8×10(-9)M was also obtained. The proposed methodology was successfully applied to the quantitative analysis of methylglyoxal in wine and beer samples. The developed sensor possesses advantageous properties such as a high active surface area, stability, and rapid electron transfer rate, which cumulatively demonstrate high performance toward the electrocatalytic reduction and detection of methylglyoxal. Copyright © 2012 Elsevier B.V. All rights reserved.

Determination of glucose in human urine by cyclic voltammetry method using gold electrode

NASA Astrophysics Data System (ADS)

Riyanto; Supwatul Hakim, Muh.

2018-01-01

This study has been the determination of glucose in human urine by cyclic voltammetry method using gold electrode. The gold electrode was prepared using gold wire with purity 99.99%, size 1.0 mm by length and wide respectively, connected with silver wire using silver conductive paint. The effect of electrolyte, pH and glucose concentration has been determined to produce the optimum method. The research showed the KNO3 is a good electrolyte for determination of glucose in human urine using gold electrode. The effect of glucose concentration have the coefficient correlation is R2 = 0.994. The results of the recovery using addition method showed at range95-105%. As a conclusion isa gold electrode is a good electrode for electrochemical sensors to the determination of glucose in human urine.

Electrochemistry and analytical determination of lysergic acid diethylamide (LSD) via adsorptive stripping voltammetry.

PubMed

Merli, Daniele; Zamboni, Daniele; Protti, Stefano; Pesavento, Maria; Profumo, Antonella

2014-12-01

Lysergic acid diethylamide (LSD) is hardly detectable and quantifiable in biological samples because of its low active dose. Although several analytical tests are available, routine analysis of this drug is rarely performed. In this article, we report a simple and accurate method for the determination of LSD, based on adsorptive stripping voltammetry in DMF/tetrabutylammonium perchlorate, with a linear range of 1-90 ng L(-1) for deposition times of 50s. LOD of 1.4 ng L(-1) and LOQ of 4.3 ng L(-1) were found. The method can be also applied to biological samples after a simple extraction with 1-chlorobutane. Copyright © 2014 Elsevier B.V. All rights reserved.

Electrochemical Deposition of Si-Ca/P on Nanotube Formed Beta Ti Alloy by Cyclic Voltammetry Method.

PubMed

Jeong, Yong-Hoon; Choe, Han-Cheol

2015-08-01

The purpose of this study was to investigate electrochemical deposition of Si-Ca/P on nanotube formed Ti-35Nb-10Zr alloy by cyclic voltammetry method. Electrochemical deposition of Si substituted Ca/P was performed by pulsing the applied potential on nanotube formed surface. The surface characteristics were observed by field-emission scanning electron microscopy, X-ray diffractometer, and potentiodynamic polarization test. The phase structure and surface morphologies of Si-Ca/P deposition were affected by deposition cycles. From the anodic polarization test, nanotube formed surface at 20 V showed the high corrosion resistance with lower value of Icorr, I300, and Ipass.

Non-platinum metal-organic framework based electro-catalyst for promoting oxygen reduction reaction

NASA Astrophysics Data System (ADS)

Das, Dipanwita; Raut, Vrushali; Kireeti, Kota V. M. K.; Jha, Neetu

2018-04-01

We developed two non-precious Metal Organic Framework (MOF) based electrocatalysts, MOF-5 and MOF-i using solvothermal and refluxing methods. The MOFs prepared has been characterized by powder X-ray diffractometer (XRD), Fourier Transform Infra-Red Spectroscopy (FTIR) and Scanning Electron Microscopy (SEM) for structural and morphological insights. SEM images reveal cubic shape for solvothermally synthesized MOF-5, whereas refluxing method leads to platelet morphology of MOF-i. The synthesized MOFs has been investigated for Oxygen Reduction Reaction (ORR) studies using Cyclic Voltammetry (CV) and Linear Sweep Voltammetry (LSV), with MOF modified Glassy Carbon (GC) as working electrode. The electrochemical data suggests higher activity of MOF-5 towards ORR compared to MOF-i.

Microbial Biofilm Voltammetry: Direct Electrochemical Characterization of Catalytic Electrode-Attached Biofilms▿ †

PubMed Central

Marsili, Enrico; Rollefson, Janet B.; Baron, Daniel B.; Hozalski, Raymond M.; Bond, Daniel R.

2008-01-01

While electrochemical characterization of enzymes immobilized on electrodes has become common, there is still a need for reliable quantitative methods for study of electron transfer between living cells and conductive surfaces. This work describes growth of thin (<20 μm) Geobacter sulfurreducens biofilms on polished glassy carbon electrodes, using stirred three-electrode anaerobic bioreactors controlled by potentiostats and nondestructive voltammetry techniques for characterization of viable biofilms. Routine in vivo analysis of electron transfer between bacterial cells and electrodes was performed, providing insight into the main redox-active species participating in electron transfer to electrodes. At low scan rates, cyclic voltammetry revealed catalytic electron transfer between cells and the electrode, similar to what has been observed for pure enzymes attached to electrodes under continuous turnover conditions. Differential pulse voltammetry and electrochemical impedance spectroscopy also revealed features that were consistent with electron transfer being mediated by an adsorbed catalyst. Multiple redox-active species were detected, revealing complexity at the outer surfaces of this bacterium. These techniques provide the basis for cataloging quantifiable, defined electron transfer phenotypes as a function of potential, electrode material, growth phase, and culture conditions and provide a framework for comparisons with other species or communities. PMID:18849456

Evaluation of homogeneous electrocatalysts by cyclic voltammetry.

PubMed

Rountree, Eric S; McCarthy, Brian D; Eisenhart, Thomas T; Dempsey, Jillian L

2014-10-06

The pursuit of solar fuels has motivated extensive research on molecular electrocatalysts capable of evolving hydrogen from protic solutions, reducing CO2, and oxidizing water. Determining accurate figures of merit for these catalysts requires the careful and appropriate application of electroanalytical techniques. This Viewpoint first briefly presents the fundamentals of cyclic voltammetry and highlights practical experimental considerations before focusing on the application of cyclic voltammetry for the characterization of electrocatalysts. Key metrics for comparing catalysts, including the overpotential (η), potential for catalysis (E(cat)), observed rate constant (k(obs)), and potential-dependent turnover frequency, are discussed. The cyclic voltammetric responses for a general electrocatalytic one-electron reduction of a substrate are presented along with methods to extract figures of merit from these data. The extension of this analysis to more complex electrocatalytic schemes, such as those responsible for H2 evolution and CO2 reduction, is then discussed.

Determination of band structure parameters and the quasi-particle gap of CdSe quantum dots by cyclic voltammetry.

PubMed

Inamdar, Shaukatali N; Ingole, Pravin P; Haram, Santosh K

2008-12-01

Band structure parameters such as the conduction band edge, the valence band edge and the quasi-particle gap of diffusing CdSe quantum dots (Q-dots) of various sizes were determined using cyclic voltammetry. These parameters are strongly dependent on the size of the Q-dots. The results obtained from voltammetric measurements are compared to spectroscopic and theoretical data. The fit obtained to the reported calculations based on the semi-empirical pseudopotential method (SEPM)-especially in the strong size-confinement region, is the best reported so far, according to our knowledge. For the smallest CdSe Q-dots, the difference between the quasi-particle gap and the optical band gap gives the electron-hole Coulombic interaction energy (J(e1,h1)). Interband states seen in the photoluminescence spectra were verified with cyclic voltammetry measurements.

Graphene decorated microelectrodes for simultaneous detection of ascorbic, dopamine, and folic acids by means of chemical vapor deposition

NASA Astrophysics Data System (ADS)

Namdar, N.; Hassanpour Amiri, M.; Dehghan Nayeri, F.; Gholizadeh, A.; Mohajerzadeh, S.

2015-09-01

In this paper, high quality and large area graphene layers were synthesized using thermal chemical vapour deposition on copper foil substrates. We use graphene incorporated electrodes to measure simultaneously ascorbic acid, dopamine and folic acid. Cyclic voltammetry and differential pulse voltammetry methods were used to evaluate electrochemical behaviour of the grown graphene layers. The graphene-modified electrode shows large electrochemical potential difference compared to bare gold electrodes with higher current responses. Also our fabricated electrodes configuration can be used easily for microfluidic analysis.

How many molecules are required to measure a cyclic voltammogram?

NASA Astrophysics Data System (ADS)

Cutress, Ian J.; Compton, Richard G.

2011-05-01

The stochastic limit at which fully-reversible cyclic voltammetry can accurately be measured is investigated. Specifically, Monte Carlo GPU simulation is used to study low concentration cyclic voltammetry at a microdisk electrode over a range of scan rates and concentrations, and the results compared to the statistical limit as predicted by finite difference simulation based on Fick's Laws of Diffusion. Both Butler-Volmer and Marcus-Hush electrode kinetics are considered, simulated via random-walk methods, and shown to give identical results in the fast kinetic limit.

Voltammetry at the Thin-Film Mercury Electrode (TFME).

ERIC Educational Resources Information Center

Pomeroy, R. S.; And Others

1989-01-01

Reviewed is the use of the Thin-Film Mercury Electrode for anodic stripping voltammetry, simple voltammetry of solution cations and cathodic stripping voltammetry for the determination of an environmentally important molecule, thiourea. The construction of a simple potentiostat and applications for student laboratory courses are included. (CW)

Enzymatic electrochemical detection coupled to multivariate calibration for the determination of phenolic compounds in environmental samples.

PubMed

Hernandez, Silvia R; Kergaravat, Silvina V; Pividori, Maria Isabel

2013-03-15

An approach based on the electrochemical detection of the horseradish peroxidase enzymatic reaction by means of square wave voltammetry was developed for the determination of phenolic compounds in environmental samples. First, a systematic optimization procedure of three factors involved in the enzymatic reaction was carried out using response surface methodology through a central composite design. Second, the enzymatic electrochemical detection coupled with a multivariate calibration method based in the partial least-squares technique was optimized for the determination of a mixture of five phenolic compounds, i.e. phenol, p-aminophenol, p-chlorophenol, hydroquinone and pyrocatechol. The calibration and validation sets were built and assessed. In the calibration model, the LODs for phenolic compounds oscillated from 0.6 to 1.4 × 10(-6) mol L(-1). Recoveries for prediction samples were higher than 85%. These compounds were analyzed simultaneously in spiked samples and in water samples collected close to tanneries and landfills. Published by Elsevier B.V.

Detection of mercury ions using L-cysteine modified electrodes by anodic stripping voltammetric method

NASA Astrophysics Data System (ADS)

Vanitha, M.; Balasubramanian, N.; Joni, I. Made; Panatarani, Camellia

2018-02-01

The detection of contaminants in wastewater is of massive importance in today's situation as they pose a serious threat to the environment as well as humans. One such vital contaminants is mercury and its compound, the reported mercury detectors grieve from low sensitivity, high cost and slow response. In the present work graphene based electrode material is developed for sensing mercury contaminants in wastewater using electrochemical technique. The synthesized material graphene oxide (GO) modified with L-Cysteine in presence of polyvinylpyrrolidone (PVP) as capping agent was characterized using SEM, TEM and Raman Spectroscopic analysis. It is ascertained from the morphological characterization that the nanocomposite exhibits a spherical morphology. The L-cysteine modified graphene oxide electrode is electrochemically characterized using redox couple [Fe(CN)63-/4-] and electrochemical impedance spectroscopic (EIS) analysis. Electrochemical sensing of Hg (II) ions in solution was done using Square wave anodic stripping voltammetry (SWASV). The incorporation of graphene significantly increases the sensitivity and selectivity towards mercury sensing.

Electrochemical Sensing toward Trace As(III) Based on Mesoporous MnFe₂O₄/Au Hybrid Nanospheres Modified Glass Carbon Electrode.

PubMed

Zhou, Shaofeng; Han, Xiaojuan; Fan, Honglei; Liu, Yaqing

2016-06-22

Au nanoparticles decorated mesoporous MnFe₂O₄ nanocrystal clusters (MnFe₂O₄/Au hybrid nanospheres) were used for the electrochemical sensing of As(III) by square wave anodic stripping voltammetry (SWASV). Modified on a cheap glass carbon electrode, these MnFe₂O₄/Au hybrid nanospheres show favorable sensitivity (0.315 μA/ppb) and limit of detection (LOD) (3.37 ppb) toward As(III) under the optimized conditions in 0.1 M NaAc-HAc (pH 5.0) by depositing for 150 s at the deposition potential of -0.9 V. No obvious interference from Cd(II) and Hg(II) was recognized during the detection of As(III). Additionally, the developed electrode displayed good reproducibility, stability, and repeatability, and offered potential practical applicability for electrochemical detection of As(III) in real water samples. The present work provides a potential method for the design of new and cheap sensors in the application of electrochemical determination toward trace As(III) and other toxic metal ions.

Stable platinum nanoclusters on genomic DNA–graphene oxide with a high oxygen reduction reaction activity

PubMed Central

Tiwari, Jitendra N.; Nath, Krishna; Kumar, Susheel; Tiwari, Rajanish N.; Kemp, K. Christian; Le, Nhien H.; Youn, Duck Hyun; Lee, Jae Sung; Kim, Kwang S.

2013-01-01

Nanosize platinum clusters with small diameters of 2–4 nm are known to be excellent catalysts for the oxygen reduction reaction. The inherent catalytic activity of smaller platinum clusters has not yet been reported due to a lack of preparation methods to control their size (<2 nm). Here we report the synthesis of platinum clusters (diameter ≤1.4 nm) deposited on genomic double-stranded DNA–graphene oxide composites, and their high-performance electrocatalysis of the oxygen reduction reaction. The electrochemical behaviour, characterized by oxygen reduction reaction onset potential, half-wave potential, specific activity, mass activity, accelerated durability test (10,000 cycles) and cyclic voltammetry stability (10,000 cycles) is attributed to the strong interaction between the nanosize platinum clusters and the DNA–graphene oxide composite, which induces modulation in the electronic structure of the platinum clusters. Furthermore, we show that the platinum cluster/DNA–graphene oxide composite possesses notable environmental durability and stability, vital for high-performance fuel cells and batteries. PMID:23900456

Sensitive Adsorptive Voltammetric Method for Determination of Bisphenol A by Gold Nanoparticle/Polyvinylpyrrolidone-Modified Pencil Graphite Electrode

PubMed Central

Yaman, Yesim Tugce; Abaci, Serdar

2016-01-01

A novel electrochemical sensor gold nanoparticle (AuNP)/polyvinylpyrrolidone (PVP) modified pencil graphite electrode (PGE) was developed for the ultrasensitive determination of Bisphenol A (BPA). The gold nanoparticles were electrodeposited by constant potential electrolysis and PVP was attached by passive adsorption onto the electrode surface. The electrode surfaces were characterized by electrochemical impedance spectroscopy (EIS) and scanning electron microscopy (SEM). The parameters that affected the experimental conditions were researched and optimized. The AuNP/PVP/PGE sensor provided high sensitivity and selectivity for BPA recognition by using square wave adsorptive stripping voltammetry (SWAdSV). Under optimized conditions, the detection limit was found to be 1.0 nM. This new sensor system offered the advantages of simple fabrication which aided the expeditious replication, low cost, fast response, high sensitivity and low background current for BPA. This new sensor system was successfully tested for the detection of the amount of BPA in bottled drinking water with high reliability. PMID:27231912

Pulse Voltammetry in Single Cells Using Platinum Microelectrodes

DTIC Science & Technology

1991-11-22

E. and the range for Ed in multiple pulse voltammetry can be chosen from examination of voltammograms obtained by cyclic voltammetry or lin-ir sweep ... voltametry [3,13]. As pointed out by Sinru et al. [14) the potential and time of each pulse has a direct effect on the nature of the voltammetry

Rapid fingerprinting of white wine oxidizable fraction and classification of white wines using disposable screen printed sensors and derivative voltammetry.

PubMed

Ugliano, Maurizio

2016-12-01

This work describes the application of disposable screen printed carbon paste sensors for the analysis of the main white wine oxidizable compounds as well as for the rapid fingerprinting and classification of white wines from different grape varieties. The response of individual white wine antioxidants such as flavanols, flavanol derivatives, phenolic acids, SO2 and ascorbic acid was first assessed in model wine. Analysis of commercial white wines gave voltammograms featuring two unresolved anodic waves corresponding to the oxidation of different compounds, mostly phenolic antioxidants. Calculation of the first order derivative of measured current vs. applied potential allowed resolving these two waves, highlighting the occurrence of several electrode processes corresponding to the oxidation of individual wine components. Through the application of Principal Component Analysis (PCA), derivative voltammograms were used to discriminate among wines of different varieties. Copyright © 2016 Elsevier Ltd. All rights reserved.

Memristive behavior of the SnO2/TiO2 interface deposited by sol-gel

NASA Astrophysics Data System (ADS)

Boratto, Miguel H.; Ramos, Roberto A.; Congiu, Mirko; Graeff, Carlos F. O.; Scalvi, Luis V. A.

2017-07-01

A novel and cheap Resistive Random Access Memory (RRAM) device is proposed within this work, based on the interface between antimony doped Tin Oxide (4%at Sb:SnO2) and Titanium Oxide (TiO2) thin films, entirely prepared through a low-temperature sol-gel process. The device was fabricated on glass slides using evaporated aluminum electrodes. Typical bipolar memristive behavior under cyclic voltage sweeping and square wave voltages, with well-defined high and low resistance states (HRS and LRS), and set and reset voltages are shown in our samples. The switching mechanism, explained by charges trapping/de-trapping by defects in the SnO2/TiO2 interface, is mainly driven by the external electric field. The calculated on/off ratio was about 8 × 102 in best conditions with good reproducibility over repeated measurement cycles under cyclic voltammetry and about 102 under applied square wave voltage.

Electrochemical studies and analysis of 1-10 wt% UCl3 concentrations in molten LiCl-KCl eutectic

NASA Astrophysics Data System (ADS)

Hoover, Robert O.; Shaltry, Michael R.; Martin, Sean; Sridharan, Kumar; Phongikaroon, Supathorn

2014-09-01

Three electrochemical methods - cyclic voltammetry (CV), chronopotentiometry (CP), and anodic stripping voltammetry (ASV) - were applied to solutions of up to 10 wt% UCl3 in the molten LiCl-KCl eutectic salt at 500 °C to determine electrochemical properties and behaviors and to help provide a scientific basis for the development of an in situ electrochemical probe for determining the concentration of uranium in a used nuclear fuel electrorefiner. Diffusion coefficients of UCl4 and UCl3 were calculated to be (6.72 ± 0.360) × 10-6 cm2/s and (1.04 ± 0.17) × 10-5 cm2/s, respectively. Apparent standard reduction potentials were determined to be (-0.381 ± 0.013) V and (-1.502 ± 0.076) V vs. 5 mol% Ag/AgCl or (-1.448 ± 0.013) V and (-2.568 ± 0.076) V vs. Cl2/Cl- for the U(IV)/U(III) and U(III)/U redox couples, respectively. In comparing this data with supercooled thermodynamic data to determine activity coefficients, the thermodynamic database used was important with resulting activity coefficients ranging from 2.34 × 10-3 to 1.08 × 10-2 for UCl4 and 4.94 × 10-5 to 4.50 × 10-4 for UCl3. Of anodic stripping voltammetry and cyclic voltammetry anodic or cathodic peaks, the CV cathodic peak height divided by square root of scan rate was shown to be the most reliable method of determining UCl3 concentration in the molten salt.

Variation sweep rate cyclic voltammetry on the capacitance electrode activated carbon/PVDF with polymer electrolyte

NASA Astrophysics Data System (ADS)

Rohmawati, L.; Setyarsih, W.; Nurjannah, T.

2018-03-01

Sweep rate of the process voltammetry cyclic characterization is very influential towards the electrode capacitance value, especially on activated carbon electrodes/PVDF. A simple method of this research by use a mixing for electrode activated carbon/10 wt. % PVDF and the separator is made of a polymer electrolyte (PVA/H3PO4) by a sol gel method. The prototype supercapacitor is made in the form of a sandwich with a separator placed between two electrodes. Electrodes and separators are arranged in layers at a pressure of 1500 psi, then heated at 50°C for 10 minutes. Next done cyclic voltammetry in a potential range of -1 V to 1 V with a sweep rate of 5 mV/s, 10 mV/s, 20 mV/s, 25 mV/s and 50 mV/s. This results of curves voltammogram is reversible, the most wide curve on the sweep rate of 5 mV/s and most narrow curve on a sweep rate of 50 mV/s. Supercapacitor capacitance values obtained by 86 F/g, 43 F/g, 21 F/g, 16 F/g, and 8 F/g.

A highly sensitive and selective sensor based on a graphene-coated carbon paste electrode modified with a computationally designed boron-embedded duplex molecularly imprinted hybrid membrane for the sensing of lamotrigine.

PubMed

Wang, Hongjuan; Qian, Duo; Xiao, Xilin; Gao, Shuqin; Cheng, Jianlin; He, Bo; Liao, Lifu; Deng, Jian

2017-08-15

An innovative electrochemical sensor, based on a carbon paste electrode (CPE) modified with graphene (GR) and a boron-embedded duplex molecularly imprinted hybrid membrane (B-DMIHM), was fabricated for the highly sensitive and selective determination of lamotrigine (LMT). Density functional theory (DFT) was employed to study the interactions between the template and monomers to screen appropriate functional monomers for rational design of the B-DMIHM. The distinct synergic effect of GR and B-DMIHM was evidenced by the positive shift of the reduction peak potential of LMT at B-DMIHM/GR modified CPE (B-DMIHM/GR/CPE) by about 300mV, and the 13-fold amplification of the peak current, compared to a bare carbon paste electrode (CPE). The electrochemical reduction mechanism of lamotrigine was investigated by different voltammetric techniques. It was illustrated that square wave voltammetry (SWV) was more sensitive than different pulse voltammetry (DPV) for the quantitative analysis of LMT. Thereafter, a highly sensitive electroanalytical method for LMT was established by SWV at B-DMIHM/GR/CPE with a good linear relationship from 5.0×10 -8 to 5.0×10 -5 and 5.0×10 -5 to 3.0×10 -4 molL -1 with a lower detection limit (1.52×10 -9 molL -1 ) based on the lower linear range(S/N=3). The practical application of the sensor was demonstrated by determining the concentration of LMT in pharmaceutical and biological samples with good precision (RSD 1.04-4.41%) and acceptable recoveries (92.40-107.0%). Copyright © 2017 Elsevier B.V. All rights reserved.

Evaluation of the degradation of acetaminophen by the filamentous fungus Scedosporium dehoogii using carbon-based modified electrodes.

PubMed

Mbokou, Serge Foukmeniok; Pontié, Maxime; Razafimandimby, Bienvenue; Bouchara, Jean-Philippe; Njanja, Evangéline; Tonle Kenfack, Ignas

2016-08-01

The nonpathogenic filamentous fungus Scedosporium dehoogii was used for the first time to study the electrochemical biodegradation of acetaminophen (APAP). A carbon fiber microelectrode (CFME) modified by nickel tetrasulfonated phthalocyanine (p-NiTSPc) and a carbon paste electrode (CPE) modified with coffee husks (CH) were prepared to follow the kinetics of APAP biodegradation. The electrochemical response of APAP at both electrodes was studied by cyclic voltammetry and square wave voltammetry. p-NiTSPc-CFME was suitable to measure high concentrations of APAP, whereas CH-CPE gave rise to high current densities but was subject to the passivation phenomenon. p-NiTSPc-CFME was then successfully applied as a sensor to describe the kinetics of APAP biodegradation: this was found to be of first order with a kinetics constant of 0.11 day(-1) (at 25 °C) and a half-life of 6.30 days. APAP biodegradation by the fungus did not lead to the formation of p-aminophenol (PAP) and hydroquinone (HQ) that are carcinogenic, mutagenic, and reprotoxic (CMR). Graphical Abstract The kinetics of APAP biodegradation, followed by a poly-nickel tetrasulfonated phtalocyanine modified carbon fiber microelectrode.

Binding mode and thermodynamic studies on the interaction of the anticancer drug dacarbazine and dacarbazine-Cu(II) complex with single and double stranded DNA.

PubMed

Temerk, Yassien; Ibrahim, Hossieny

2014-07-01

The binding mode and thermodynamic characteristics of the anticancer drug dacarbazine (Dac) with double and single stranded DNA were investigated in the absence and presence of Cu(II) using cyclic voltammetry, square wave voltammetry and fluorescence spectroscopy. The interaction of Dac and Dac-Cu(II) complex with dsDNA indicated their intercalation into the base stacking domain of dsDNA double helix and the strength of interaction is independent on the ionic strength. The interaction of Dac with dsDNA in the presence of Cu(II) leads to a much stronger intercalation. The interaction mode of Dac molecules with ssDNA is electrostatic attraction via negative phosphate on the exterior of the ssDNA with Dac. The binding constants, stoichiometric coefficients and thermodynamic parameters of Dac and Dac-Cu(II) complex with dsDNA and ssDNA were evaluated. Comparison of the mode interaction of Dac with dsDNA and ssDNA was discussed. The decrease of peak current of Dac was proportional to DNA concentration, which was applied for determination of dsDNA and ssDNA concentration. Copyright © 2014 Elsevier B.V. All rights reserved.

Electrochemical preparation of nickel and copper oxides-decorated graphene composite for simultaneous determination of dopamine, acetaminophen and tryptophan.

PubMed

Liu, Bingdi; Ouyang, Xiaoqian; Ding, Yaping; Luo, Liqing; Xu, Duo; Ning, Yanqun

2016-01-01

In the present work, transition metal oxides decorated graphene (GR) have been fabricated for simultaneous determination of dopamine (DA), acetaminophen (AC) and tryptophan (Trp) using square wave voltammetry. Electro-deposition is a facile preparation strategy for the synthesis of nickel oxide (NiO) and copper oxide (CuO) nanoparticles. GR can be modified by using citric acid to produce more functional groups, which is conducive to the deposition of dispersed metal particles. The morphologies and interface properties of the obtained NiO-CuO/GR nanocomposite were examined by scanning electron microscopy, energy dispersive X-ray spectroscopy and Raman spectroscopy. Moreover, the electrochemical performances of the composite film were investigated by cyclic voltammetry and electrochemical impedance spectroscopy. The modified electrode exhibited that the linear response ranges for detecting DA, AC and Trp were 0.5-20 μM, 4-400 μM and 0.3-40 μM, respectively, and the detection limits were 0.17 μM, 1.33 μM and 0.1 μM (S/N=3). Under optimal conditions, the sensor displayed high sensitivity, excellent stability and satisfactory results in real samples analysis. Copyright © 2015 Elsevier B.V. All rights reserved.

Bismuth-based electrochemical stripping analysis

DOEpatents

Wang, Joseph

2004-01-27

Method and apparatus for trace metal detection and analysis using bismuth-coated electrodes and electrochemical stripping analysis. Both anodic stripping voltammetry and adsorptive stripping analysis may be employed.

The redox status of experimental hemorrhagic shock as measured by cyclic voltammetry.

PubMed

Mittal, Anubhav; Göke, Friederike; Flint, Richard; Loveday, Benjamin P T; Thompson, Nichola; Delahunt, Brett; Kilmartin, Paul A; Cooper, Garth J S; MacDonald, Julia; Hickey, Anthony; Windsor, John A; Phillips, Anthony R J

2010-05-01

Hemorrhagic shock (HS) leads to reactive oxygen species production. However, clinicians do not have access to bedside measurements of the redox status during HS. Cyclic voltammetry (CyV) is a simple electrochemical method of measuring redox status. The aims of this study were to 1) report the first application of cyclic voltammetry to measure the acute changes in serum redox status after HS, 2) to contrast it with another severe systemic disease with a different redox pathology (acute pancreatitis [AP]), and 3) to describe the response of CyV over time in a resolving model of AP. In the acute study, 24 male Wistar rats were randomized into three groups: groups 1 (control), 2 (AP), and 3 (HS). In the time-course study, 28 rats were randomized to a sham-control as well as 6 and 24 h post-AP cohorts, respectively.Cyclic voltammetry was performed using a three-electrode system. In the acute study, the first and second voltammetric peaks increased significantly in HS. In contrast, within the AP group, only the first voltammetric peak showed a significant increase. The first voltammetric peak correlated with plasma protein carbonyls (PCs) and with thiobarbituric acid-reactive substances, whereas the second voltammetric peak correlated positively with plasma protein carbonyls. In the second study, the first voltammetric peak correlated with physiological improvements. Here, we showed that serum CyV could respond to the serum redox change in HS and AP. Cyclic voltammetry warrants evaluation as a potential real-time beside measure of a patient's redox status during shock.

Quantification of lead and cadmium in poultry and bird game meat by square-wave anodic-stripping voltammetry.

PubMed

Trevisani, M; Cecchini, M; Taffetani, L; Vercellotti, L; Rosmini, R

2011-02-01

A square-wave anodic-stripping voltammetric method for the analysis of lead and cadmium in chicken muscle and liver was developed and validated, and the results of a monitoring study relative to chicken and pigeon meat are reported. The voltammetric method allows the analysis of lead and cadmium at the same time in samples after acid digestion. The use of perchloric acid for digestion and of acetate buffer in the supporting electrolyte are suitable to reduce matrix interferences and obtain limits of quantification which were below 10 ng g⁻¹ for meat and liver samples. The regression between the analytical signal and the concentration of the target analytes in spiked samples and Certified Reference Materials proved to be linear within the 10-100 ng g⁻¹ range for meat and within the 50-500 ng g⁻¹ range for liver. The analytical method was verified using available Certified Reference Materials BCR-184 (cattle meat) and BCR-185R (cattle liver) as well as with spiked chicken samples. Precision (i.e. repeatability and intermediate precision) and accuracy (percentage recovery and bias) were of the order of 0.3-4.5% for both lead and cadmium The level of lead in muscle was in the range between 6.4 and 59.8 ng g⁻¹ in chickens and between 7.9 and 63.6 ng g⁻¹ in farmed pigeons, whereas it was between 8.0 and 84.4 ng g⁻¹ in chicken liver. The cadmium concentration was 0.4-10.4 ng g⁻¹ in chicken muscle, 10.4-90.6 ng g⁻¹ in chicken liver and 2.2-8.0 ng g⁻¹ in farmed pigeons.

Ascorbic Acid Determination in Commercial Fruit Juice Samples by Cyclic Voltammetry

PubMed Central

Pisoschi, Aurelia Magdalena; Danet, Andrei Florin; Kalinowski, Slawomir

2008-01-01

A method was developed for assessing ascorbic acid concentration in commercial fruit juice by cyclic voltammetry. The anodic oxidation peak for ascorbic acid occurs at about 490 mV on a Pt disc working electrode (versus SCE). The influence of the potential sweep speed on the peak height was studied. The obtained calibration graph shows a linear dependence between peak height and ascorbic acid concentration in the domain (0.1–10 mmol·L−1). The equation of the calibration graph was y = 6.391x + 0.1903 (where y represents the value of intensity measured for the anodic peak height, expressed as μA and x the analyte concentration, as mmol·L−1, r2 = 0.9995, r.s.d. = 1.14%, n = 10, Cascorbic acid = 2 mmol·L−1). The developed method was applied to ascorbic acid assessment in fruit juice. The ascorbic acid content determined ranged from 0.83 to 1.67 mmol·L−1 for orange juice, from 0.58 to 1.93 mmol·L−1 for lemon juice, and from 0.46 to 1.84 mmol·L−1 for grapefruit juice. Different ascorbic acid concentrations (from standard solutions) were added to the analysed samples, the degree of recovery being comprised between 94.35% and 104%. Ascorbic acid determination results obtained by cyclic voltammetry were compared with those obtained by the volumetric method with dichlorophenol indophenol. The results obtained by the two methods were in good agreement. PMID:19343183

Halloysite clay nanotubes and platinum nanoparticles dispersed in ionic liquid applied in the development of a catecholamine biosensor.

PubMed

Brondani, Daniela; Scheeren, Carla Weber; Dupont, Jairton; Vieira, Iolanda Cruz

2012-08-21

Halloysite clay nanotubes were used as a support for the immobilization of the enzyme peroxidase from clover sprouts (Trifolium), and employed together with platinum nanoparticles in 1-butyl-3-methylimidazolium hexafluorophosphate ionic liquid (Pt-BMI·PF(6)) in the development of a new biosensor for the determination of catecholamines by square-wave voltammetry. Under optimized conditions, the analytical curves showed detection limits of 0.05, 0.06, 0.07, 0.12 μM for dopamine, isoproterenol, dobutamine and epinephrine, respectively. The biosensor demonstrated high sensitivity, good repeatability and reproducibility, and long-term stability (18% decrease in response over 150 days). A recovery study of dopamine in pharmaceutical samples gave values from 97.5 to 101.4%. The proposed biosensor was successfully applied to the determination of dopamine in pharmaceutical samples, with a maximum relative error of ±1.0% in relation to the standard (spectrophotometric) method. The good analytical performance of the proposed method can be attributed to the efficient immobilization of the peroxidase in the nanoclay, and the facilitation of electron transfer between the protein and the electrode surface due to the presence of the Pt nanoparticles and ionic liquid.

Carbon paste electrode modified molecularly imprinted polymer as a sensor for creatinine analysis by stripping voltammetry

NASA Astrophysics Data System (ADS)

Khasanah, M.; Darmokoesoemo, H.; Rizki, D. A.

2017-09-01

Modification of carbon paste electrode with molecularly imprinted polymer (CP-MIP) as a voltammetric sensor for creatinine has been developed. MIP was synthesized by reacting melamine, chloranil and creatinine with a mole ratio of 1:1:0.1. Creatinine was extracted from polymer chain by using hot water to form a specific imprinted for creatinine molecule. Carbon paste-MIP electrode was prepared by mixing activated carbon, solid paraffin, and MIP in a 45:40:15(w/w %) ratio. The optimum conditions of creatinine analysis by differential pulse stripping voltammetry (DPSV) using the developed electrode were the accumulation potential -1000 mV during 90 s at pH 5. The precision of the method for 0.1-0.5 μlg/L creatinine was 88.7-96.3%, while the detection limit of this method was 0.0315 μlg/L. The accuracy compared by spectrophotometric method was 95.3-103.6%

Adsorptive Behavior and Voltammetric Determination of Hydralazine Hydrochloride at A Glassy Carbon Electrode Modified with Multiwalled Carbon Nanotubes

PubMed Central

Khodadadian, Mehdi; Jalili, Ronak; Bahrami, Mohammad Taher; Bahrami, Gholamreza

2017-01-01

An electroanalytical method has been introduced for highly sensitive determination of hydralazine hydrochloride (Hy-HCl) based on its oxidation at a glassy carbon electrode modified with multiwalled carbon nanotubes (MWCNT/GCE). Studies showed that the electrochemical oxidation of Hy-HCl was accompanied by adsorption and highly sensitive responses could be achieved by adsorptive stripping voltammetry. The electrooxidation of Hy-HCl at MWCNT/GCE occurred at ~32 mV which was lower than that observed at bare GCE (~52 mV). The optimum working conditions for determination of the drug using differential-pulse adsorptive stripping voltammetry (DPAdSV) were established. The method exhibited linear responses to Hy-HCl in the concentration range 10-220 nM with a detection limit of 2.7 nM. The proposed method was successfully applied to the determination of this compound in pharmaceutical dosage forms. PMID:29552043

Cyclic voltammetry as a sensitive method for in situ probing of chemical transformations in quantum dots.

PubMed

Osipovich, Nikolai P; Poznyak, Sergei K; Lesnyak, Vladimir; Gaponik, Nikolai

2016-04-21

The application of electrochemical methods for the characterization of colloidal quantum dots (QDs) attracts considerable attention as these methods may allow for monitoring of some crucial parameters, such as energetic levels of conduction and valence bands as well as surface traps and ligands under real conditions of colloidal solution. In the present work we extend the applications of cyclic voltammetry (CV) to in situ monitoring of degradation processes of water-soluble CdTe QDs. This degradation occurs under lowering of pH to the values around 5, i.e. under conditions relevant to bioimaging applications of these QDs, and is accompanied by pronounced changes of their photoluminescence. Observed correlations between characteristic features of CV diagrams and the fluorescence spectra allowed us to propose mechanisms responsible for evolution of the photoluminescence properties as well as degradation pathway of CdTe QDs at low pH.

Functionalization of reduced graphene oxide by electroactive polymer for biosensing applications

NASA Astrophysics Data System (ADS)

Nguyen, Le Huy; Dzung Nguyen, Tuan; Hoang Tran, Vinh; Thu Huyen Dang, Thi; Tran, Dai Lam

2014-09-01

A novel biosensing platform was designed by the functionalizing reduced graphene oxide sheets (rGO) with electroactive copolymer juglone. The composite film showed well-defined, stable electroactivity in a biocompatible buffer medium. Square wave voltammetry is used to record the redox signal for DNA hybridization. Current increase upon hybridization (signal-on) evidenced that short DNA target as well as polymerase chain reaction (PCR), so called ‘real sample’ products, related to different lineages of Mycobacterium tuberculosis strain. The signal-on reached ∼40% with 1 nM of short DNA (25 mer) target, while PCR product (Africanum, EAI and Beijing strains) produced a current change of ∼20%.

Investigation of antioxidant capacity of the extracts of bilberry (VACCINUM MYRTILLIS L.) by voltammetry

NASA Astrophysics Data System (ADS)

Vtorushina, A. N.; Nikonova, E. D.

2016-02-01

This paper deals with the urgent issue of the search of new drugs based on plant raw materials that have an influence on various stages of oxidation processes occurring in the human body. The aim of this paper is to determine the antioxidant activity of the bilberry extracts that are used in the medicine practice by a cathodic voltammetry method. We consider the influence of water and alcohol bilberry extracts on the process of oxygen electroreduction. From these extracts the most activity relation to the process of cathodic oxygen reduction showed alcohol (40%) bilberry extract. It was also stated that the alcohol extract of bilberry has a greater antioxidant activity than other known antioxidants such as ascorbic acid, glucose, dihydroquercetin. Thus, after consideration of a number of plant objects, we showed the possibility of applying the method of cathodic voltammetry for the determination of total antioxidant activity of plant material and identifying and highlighting the most perspective sources of biologically active substances (BAS), as well as the ability of identifying extractants that fully extract BAS from plant raw materials. The activity data of extracts of plant raw materials gives an opportunity of establishing an effective yield phytopreparation based on bilberry that has an antioxidant effect.

A Cuprous Oxide Thin Film Non-Enzymatic Glucose Sensor Using Differential Pulse Voltammetry and Other Voltammetry Methods and a Comparison to Different Thin Film Electrodes on the Detection of Glucose in an Alkaline Solution

PubMed Central

Molazemhosseini, Alireza; Liu, Chung Chiun

2018-01-01

A cuprous oxide (Cu2O) thin layer served as the base for a non-enzymatic glucose sensor in an alkaline medium, 0.1 NaOH solution, with a linear range of 50–200 mg/dL using differential pulse voltammetry (DPV) measurement. An X-ray photoelectron spectroscopy (XPS) study confirmed the formation of the cuprous oxide layer on the thin gold film sensor prototype. Quantitative detection of glucose in both phosphate-buffered saline (PBS) and undiluted human serum was carried out. Neither ascorbic acid nor uric acid, even at a relatively high concentration level (100 mg/dL in serum), interfered with the glucose detection, demonstrating the excellent selectivity of this non-enzymatic cuprous oxide thin layer-based glucose sensor. Chronoamperometry and single potential amperometric voltammetry were used to verify the measurements obtained by DPV, and the positive results validated that the detection of glucose in a 0.1 M NaOH alkaline medium by DPV measurement was effective. Nickel, platinum, and copper are commonly used metals for non-enzymatic glucose detection. The performance of these metal-based sensors for glucose detection using DPV were also evaluated. The cuprous oxide (Cu2O) thin layer-based sensor showed the best sensitivity for glucose detection among the sensors evaluated. PMID:29316652

Catalytic mechanism in cyclic voltammetry at disc electrodes: an analytical solution.

PubMed

Molina, Angela; González, Joaquín; Laborda, Eduardo; Wang, Yijun; Compton, Richard G

2011-08-28

The theory of cyclic voltammetry at disc electrodes and microelectrodes is developed for a system where the electroactive reactant is regenerated in solution using a catalyst. This catalytic process is of wide importance, not least in chemical sensing, and it can be characterized by the resulting peak current which is always larger than that of a simple electrochemical reaction; in contrast the reverse peak is always relatively diminished in size. From the theoretical point of view, the problem involves a complex physical situation with two-dimensional mass transport and non-uniform surface gradients. Because of this complexity, hitherto the treatment of this problem has been tackled mainly by means of numerical methods and so no analytical expression was available for the transient response of the catalytic mechanism in cyclic voltammetry when disc electrodes, the most popular practical geometry, are used. In this work, this gap is filled by presenting an analytical solution for the application of any sequence of potential pulses and, in particular, for cyclic voltammetry. The induction principle is applied to demonstrate mathematically that the superposition principle applies whatever the geometry of the electrode, which enabled us to obtain an analytical equation valid whatever the electrode size and the kinetics of the catalytic reaction. The theoretical results obtained are applied to the experimental study of the electrocatalytic Fenton reaction, determining the rate constant of the reduction of hydrogen peroxide by iron(II).

Synthesis and characterization of a new porphyrin-polyoxometalate hybrid material and investigation of its catalytic activity.

PubMed

Araghi, Mehdi; Mirkhani, Valiollah; Moghadam, Majid; Tangestaninejad, Shahram; Mohammdpoor-Baltork, Iraj

2012-03-14

In the present work, the preparation of a new organic-inorganic hybrid material in which tetrakis(p-aminophenylporphyrin) is covalently linked to a Lindqvist structure of polyoxometalate, is reported. This new porphyrin-polyoxometalate hybrid material was characterized by (1)H NMR, FT-IR and UV-Vis spectroscopic methods and cyclic voltammetry. These spectro- and electrochemical studies provided spectral data of the synthesis of this compound. Cyclic voltammetry showed the influence of the porphyrin on the redox process of the polyoxometalate. The catalytic activity of this hybrid material was investigated in the alkene epoxidation with NaIO(4).

Rapid Screening Method for Detecting Ethinyl Estradiol in Natural Water Employing Voltammetry

PubMed Central

2016-01-01

17α-Ethinyl estradiol (EE2), which is used worldwide in the treatment of some cancers and as a contraceptive, is often found in aquatic systems and is considered a pharmaceutically active compound (PhACs) in the environment. Current methods for the determination of this compound, such as chromatography, are expensive and lengthy and require large amounts of toxic organic solvents. In this work, a voltammetric procedure is developed and validated as a screening tool for detecting EE2 in water samples without prior extraction, clean-up, or derivatization steps. Application of the method we elaborate here to EE2 analysis is unprecedented. EE2 detection was carried out using differential pulse adsorptive cathodic stripping voltammetry (DP AdCSV) with a hanging mercury drop electrode (HMDE) in pH 7.0 Britton-Robinson buffer. The electrochemical process of EE2 reduction was investigated by cyclic voltammetry at different scan rates. Electroreduction of the hormone on a mercury electrode exhibited a peak at −1.16 ± 0.02 V versus Ag/AgCl. The experimental parameters were as follows: −0.7 V accumulation potential, 150 s accumulation time, and 60 mV s−1 scan rate. The limit of detection was 0.49 μg L−1 for a preconcentration time of 150 s. Relative standard deviations were less than 13%. The method was applied to the detection of EE2 in water samples with recoveries ranging from 93.7 to 102.5%. PMID:27738548

Affordable Cyclic Voltammetry

ERIC Educational Resources Information Center

Stewart, Greg; Kuntzleman, Thomas S.; Amend, John R.; Collins, Michael J.

2009-01-01

Cyclic voltammetry is an important component of the undergraduate chemical curriculum. Unfortunately, undergraduate students rarely have the opportunity to conduct experiments in cyclic voltammetry owing to the high cost of potentiostats, which are required to control these experiments. By using MicroLab data acquisition interfaces in conjunction…

A new molecularly imprinted polymer (MIP)-based electrochemical sensor for monitoring 2,4,6-trinitrotoluene (TNT) in natural waters and soil samples.

PubMed

Alizadeh, Taher; Zare, Mashaalah; Ganjali, Mohamad Reza; Norouzi, Parviz; Tavana, Babak

2010-01-15

A high selective voltammetric sensor for 2,4,6-trinitrotoluene (TNT) was introduced. TNT selective MIP and non-imprinted polymer (NIP) were synthesized and then used for carbon paste (CP) electrode preparation. The MIP, incorporated in the carbon paste electrode, functioned as selectively recognition element and pre-concentrator agent for TNT determination. The prepared electrode was used for TNT measurement by the three steps procedure, including analyte extraction in the electrode, electrode washing and electrochemical measurement of TNT. The MIP-CP electrode showed very high recognition ability in comparison to NIP-CP. It was shown that electrode washing after TNT extraction led to enhanced selectivity. The response of square wave voltammetry for TNT determination by proposed electrode was higher than that of differential pulse voltammetry. Some parameters affecting sensor response were optimized and then a calibration curve plotted. A dynamic linear range of 5x10(-9) to 1x10(-6) mol l(-1) was obtained. The detection limit of the sensor was calculated equal to 1.5x10(-9) mol l(-1). This sensor was used successfully for TNT determination in different water and soil samples. Copyright 2009 Elsevier B.V. All rights reserved.

AuNPs/CNOs/SWCNTs/chitosan-nanocomposite modified electrochemical sensor for the label-free detection of carcinoembryonic antigen.

PubMed

Rizwan, Mohammad; Elma, Syazwani; Lim, Syazana Abdullah; Ahmed, Minhaz Uddin

2018-06-01

In this work, a nanocomposite of gold nanoparticles (AuNPs), carbon nano-onions (CNOs), single-walled carbon nanotubes (SWCNTs) and chitosan (CS) (AuNPs/CNOs/SWCNTs/CS) was prepared for the development of highly sensitive electrochemical immunosensor for the detection of carcinoembryonic antigen (CEA), clinical tumor marker. Firstly, layer-by-layer fabrication of the CEA-immunosensors was studied using cyclic voltammetry (CV) and square wave voltammetry (SWV). By combining the advantages of large surface area and electronic properties of AuNPs, CNOs, SWCNTs, and film forming properties of CS, AuNPs/CNOs/SWCNTs/CS-nanocomposite-modified glassy carbon electrode showed a 200% increase in effective surface area and electronic conductivity. The calibration plot gave a negative linear relationship between log[concentration] of CEA and electrical current with a correlation coefficient of 0.9875. The CEA-immunosensor demonstrated a wide linear detection range of 100 fg mL -1 to 400 ng mL -1 with a low detection limit of 100 fg mL -1 . In addition to high sensitivity, reproducibility and large stability, CEA-immunosensor provided an excellent selectivity and resistant-to-interference in the presence of other antigens in serum and hence a potential to be used with real samples. Copyright © 2018 Elsevier B.V. All rights reserved.

Electrosynthesis and binding properties of molecularly imprinted poly-o-phenylenediamine for selective recognition and direct electrochemical detection of myoglobin.

PubMed

Shumyantseva, Victoria V; Bulko, Tatiana V; Sigolaeva, Larisa V; Kuzikov, Alexey V; Archakov, Alexander I

2016-12-15

Electrosynthesis of molecularly imprinted polymer (MIP) templated with myoglobin (Mb) and the reference non-imprinted polymer (NIP) was examined with o-phenylenediamine (o-PD) as a monomer. Mass-sensitive quartz crystal microbalance with dissipation monitoring supplied by an electrochemical module (EQCM-D) was applied to characterize and optimize MIP/NIP electrosynthesis. Mb rebinding was detected by direct electrocatalytic reduction of Mb by square wave voltammetry (SWV) or differential pulse voltammetry (DPV). The results obtained showed high specificity of polymeric antibodies to template Mb, with an imprinting factor determined as a ratio Imax(MIP)/Imax(NIP) of 2-4. The prepared MIP sensor is characterized by an apparent dissociation constant of (3.3±0.5)×10(-9)M and has a broad range of working concentrations of 1nM-1μМ, with the detection limit of 0.5nM (9ng/ml). Mb rebinding was examined in Mb-free diluted human serum spiked with Mb as well as in plasma samples of patients with acute myocardial infarction (AMI) and in control plasma of healthy donors in order to demonstrate the potential medical application of developed MIP sensors. Copyright © 2016 Elsevier B.V. All rights reserved.

Cathodic stripping voltammetry of nickel: sonoelectrochemical exploitation of the Ni(III)/Ni(II) couple.

PubMed

Davis, James; Vaughan, D Huw; Stirling, David; Nei, Lembit; Compton, Richard G

2002-07-19

The exploitation of the Ni(III)/Ni(II) transition as a means of quantifying the concentration of nickel within industrial samples was assessed. The methodology relies upon the reagentless electrodeposition of Ni onto a glassy carbon electrode and the subsequent oxidative conversion of the metallic layer to Ni(III). The analytical signal is derived from a cathodic stripping protocol in which the reduction of the Ni(III) layer to Ni(II) is monitored through the use of square wave voltammetry. The procedure was refined through the introduction of an ultrasonic source which served to both enhance the deposition of nickel and to remove the nickel hydroxide layer that results from the measurement process. A well-defined stripping peak was observed at +0.7 V (vs. Agmid R:AgCl) with the response found to be linear over the range 50 nM to 1 muM (based on a 30 s deposition time). Other metal ions such as Cu(II), Mn(II), Cr(III), Pb(II), Cd(II), Zn(II), Fe(III) and Co(II) did not interfere with the response when present in hundred fold excess. The viability of the technique was evaluated through the determination of nickel within a commercial copper nickel alloy and validated through an independent comparison with a standard ICP-AES protocol.

Electrochemical Measurement of Activities for NiO, Ru2O3, and ZnO in a Lunar Volcanic Glass Analog

NASA Technical Reports Server (NTRS)

Colson, R. O.; Hendrickson, T. R.; Malum, K. M.; Floden, A. M.

2000-01-01

Differential Pulse Voltammetry is a fast in situ method for measuring component activities in silicate melts. We report methods for confirming equilibrium conditions and activities for oxide components in an Apollo 15 green glass analog composition.

ON-SITE MERCURY ANALYSIS OF SOIL AT HAZARDOUS WASTE SITES BY IMMUNOASSAY AND ASV

EPA Science Inventory

Two field methods for Hg, immunoassay and anodic stripping voltammetry (ASV), that can provide onsite results for quick decisions at hazardous waste sites were evaluated. Each method was applied to samples from two Superfund sites that contain high levels of Hg; Sulphur Bank Me...

Electrochemical Behavior of Quinoxalin-2-one Derivatives at Mercury Electrodes and Its Analytical Use

PubMed Central

Zimpl, Milan; Skopalova, Jana; Jirovsky, David; Bartak, Petr; Navratil, Tomas; Sedonikova, Jana; Kotoucek, Milan

2012-01-01

Derivatives of quinoxalin-2-one are interesting compounds with potential pharmacological activity. From this point of view, understanding of their electrochemical behavior is of great importance. In the present paper, a mechanism of electrochemical reduction of quinoxalin-2-one derivatives at mercury dropping electrode was proposed. Pyrazine ring was found to be the main electroactive center undergoing a pH-dependent two-electron reduction process. The molecule protonization of nitrogen in the position 4 precedes the electron acceptance forming a semiquinone radical intermediate which is relatively stable in acidic solutions. Its further reduction is manifested by separated current signal. A positive mesomeric effect of the nonprotonized amino group in the position 7 of the derivative III accelerates the semiquinone reduction yielding a single current wave. The suggested reaction mechanism was verified by means of direct current polarography, differential pulse, cyclic and elimination voltammetry, and coulometry with subsequent GC/MS analysis. The understanding of the mechanism was applied in developing of analytical method for the determination of the studied compounds. PMID:22666117

Effect of tunable redox behavior of bis chelate substituted 1,10-phenantroline Cu(II) complexes on its reaction with superoxide anion in DMSO. Toward a simple criterion to identify a SOD-like mechanism.

PubMed

Manzanera-Estrada, Mayra E; Cruz-Ramírez, Marisela; Flores-Alamo, Marcos; Gracia Y Jiménez, José Miguel; Galindo-Murillo, Rodrigo; García-Ramos, Juan Carlos; Ruiz-Azuara, Lena; Ortiz-Frade, Luis

2017-10-01

In this work we report a series of Cu(II) complexes [Cu(N-N) 2 (X)] + , (N-N=substituted 1,10-phenanthroline derivatives and X=Cl - or NO 3 - ), with tunable E 1/2 for electrochemical reduction [Cu II (N-N) 2 (X)] + +1e - ⇌[Cu I (N-N) 2 ]+X - . The disproportion of O 2 •- was explored in presence of the electro-generated species [Cu I (N-N) 2 ] + using cyclic voltammetry in a non-aqueous media, arising a new simple method to propose a SOD-like mechanism, which can be used as a quick guide test for a compound, before being proven in biological assays. It was found that complexes with high negative half wave potential values (E 1/2 ) for Cu(II)/Cu(I) couple shown a current increment for oxygen reduction, related to the capability of the disproportion of this reactive oxygen species. Copyright © 2017 Elsevier Inc. All rights reserved.

Direct electrochemical stripping detection of cystic-fibrosis-related DNA linked through cadmium sulfide quantum dots

NASA Astrophysics Data System (ADS)

Marin, Sergio; Merkoçi, Arben

2009-02-01

Electrochemical detection of a cadmium sulfide quantum dots (CdS QDs)-DNA complex connected to paramagnetic microbeads (MB) was performed without the need for chemical dissolving. The method is based on dropping 20 µl of CdS QD-DNA-MB suspension on the surface of a screen-printed electrode. It is followed by magnetic collection on the surface of the working electrode and electrochemical detection using square-wave voltammetry (SWV), giving a well-shaped and sensitive analytical signal. A cystic-fibrosis-related DNA sequence was sandwiched between the two DNA probes. One DNA probe is linked via biotin-streptavidin bonding with MB and the other one via thiol groups with the CdS QD used as tags. Nonspecific signals of DNA were minimized using a blocking agent and the results obtained were successfully employed in a model DNA sensor with an interest in future applications in the clinical field. The developed nanoparticle biosensing system may offer numerous opportunities in other fields where fast, low cost and efficient detection of small volume samples is required.

[Na5(THF)10Ce(mnt)4]infinity: a honeycomb network polymer that yields homoleptic cerium(III) tetrakis(dithiolene) complexes in donor solvents.

PubMed

Weis, Eric M; Barnes, Charles L; Duval, Paul B

2006-12-11

The first example of a lanthanide tetrakis(dithiolene) complex, [Na5(THF)10Ce(mnt)4] (1) (mnt = 1,2-maleonitrile-1,2-dithiolate), has been synthesized and characterized by X-ray crystallography and spectroscopic methods. In the solid state, 1 exists as a 2-D corrugated honeycomb network polymer in which the monomeric units comprising the trigonal nodes are knitted together by interlocking dative Na-N bonds extended from nitrile groups of bifunctional mnt ligands coordinated through the sulfur atoms to adjacent cerium centers. Individual honeycomb sheets are separated by 14.8 A. Compound 1 dissolves in donor solvents such as THF and acetonitrile to give soluble [Ce(mnt)4]5- units that exhibit spectroscopic features (i.e., NMR, luminescence, UV-vis) that are consistent with the 4f1 Ce(III) ion. In the first examination of the redox chemistry of a lanthanide dithiolene complex, cyclic voltammetry measurements conducted on 1 reveal a single irreversible oxidation wave that is likely attributable to ligand-centered oxidation.

Simultaneous determination of hydroquinone and catechol at gold nanoparticles mesoporous silica modified carbon paste electrode.

PubMed

Tashkhourian, J; Daneshi, M; Nami-Ana, F; Behbahani, M; Bagheri, A

2016-11-15

A new electrochemical sensor based on gold nanoparticles mesoporous silica modified carbon paste electrode (AuNPs-MPS) was developed for simultaneous determination of hydroquinone and catechol. Morphology and structure of the AuNPs-MPS were characterized by transmission electron microscopy, X-ray diffraction and Fourier transform infrared spectroscopy. The electrochemical behavior of hydroquinone and catechol were investigated using square wave voltammetry and the results indicate that the electrochemical responses are improved significantly at the modified electrode. The observed oxidative peaks separation of about 120mV made possible the simultaneous determination of hydroquinone and catechol in their binary-mixture. Under the optimized condition, a linear dynamic range of 10.0μM-1.0mM range for hydroquinone with the detection limit of 1.2μM and from 30.0μM-1.0mM for catechol with the detection limit of 1.1μM were obtained. The applicability of the method was demonstrated by the recovery studies of hydroquinone and catechol in spiked tap water samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Polyaniline-graphene oxide nanocomposite sensor for quantification of calcium channel blocker levamlodipine.

PubMed

Jain, Rajeev; Sinha, Ankita; Khan, Ab Lateef

2016-08-01

A novel polyaniline-graphene oxide nanocomposite (PANI/GO/GCE) sensor has been fabricated for quantification of a calcium channel blocker drug levamlodipine (LAMP). Fabricated sensor has been characterized by electrochemical impedance spectroscopy, square wave and cyclic voltammetry, Raman spectroscopy and Fourier transform infrared (FTIR) spectroscopy. The developed PANI/GO/GCE sensor has excellent analytical performance towards electrocatalytic oxidation as compared to PANI/GCE, GO/GCE and bare GCE. Under optimized experimental conditions, the fabricated sensor exhibits a linear response for LAMP for its oxidation over a concentration range from 1.25μgmL(-1) to 13.25μgmL(-1) with correlation coefficient of 0.9950 (r(2)), detection limit of 1.07ngmL(-1) and quantification limit of 3.57ngmL(-1). The sensor shows an excellent performance for detecting LAMP with reproducibility of 2.78% relative standard deviation (RSD). The proposed method has been successfully applied for LAMP determination in pharmaceutical formulation with a recovery from 99.88% to 101.75%. Copyright © 2015 Elsevier B.V. All rights reserved.

Hydrothermal synthesis and processing of hydrogen titanate nanotubes for nicotine electrochemical sensing

NASA Astrophysics Data System (ADS)

Mersal, Gaber A. M.; Mostafa, Nasser Y.; Omar, Abd-Elkader H.

2017-08-01

Hydrogen titanate nanotubes (HTNT) were prepared via acid washing of hydrothermally synthesized sodium titantate nanotube. HTNTs with diameters in the range 7-9 nm and length of several hundred nanometers were annealed at different temperatures and used to modify carbon paste electrode (CPE). Cyclic and square wave voltammetric techniques were used to investigate the behavior of nicotine at HTNT modified carbon paste electrode (HTNTCPE). The nicotine-oxidation reaction over HTNTCPE was irreversible and adsorption process is the rate determining step. HTNTs annealed at 500 °C showed the best response to nicotine. The nicotine concentration was determined at the ideal conditions by square wave voltammetry (SWV). The calibration was linear from 0.1 to 500.0 µmol l-1 with a correlation coefficient of 0.995. The detection limits were found to be 0.005 µmol l-1. The present HTNTCPE was used to the determination of nicotine in two cigarette brands and it showed outstanding performance with respect to detection limit and sensitivity.

Combined characterization of bovine polyhemoglobin microcapsules by UV-Vis absorption spectroscopy and cyclic voltammetry.

PubMed

Knirsch, Marcos Camargo; Dell'Anno, Filippo; Salerno, Marco; Larosa, Claudio; Polakiewicz, Bronislaw; Eggenhöffner, Roberto; Converti, Attilio

2017-03-01

Polyhemoglobin produced from pure bovine hemoglobin by reaction with PEG bis(N-succynimidil succinate) as a cross-linking agent was encapsulated in gelatin and dehydrated by freeze-drying. Free carboxyhemoglobin and polyhemoglobin microcapsules were characterized by UV-Vis spectroscopy in the absorption range 450-650 nm and cyclic voltammetry in the voltage range from -0.8 to 0.6 mV to evaluate the ability to break the bond with carbon monoxide and to study the carrier's affinity for oxygen, respectively. SEM used to observe the shape of cross-linked gelatin-polyhemoglobin microparticles showed a regular distribution of globular shapes, with mean size of ~750 nm, which was ascribed to gelatin. Atomic absorption spectroscopy was also performed to detect iron presence in microparticles. Cyclic voltammetry using an Ag-AgCl electrode highlighted characteristic peaks at around -0.6 mV that were attributed to reversible oxygen bonding with iron in oxy-polyhemoglobin structure. These results suggest this technique as a powerful, direct and alternative method to evaluate the extent of hemoglobin oxygenation.

Electrochemical and spectroscopic study on the interaction between isoprenaline and DNA using multivariate curve resolution-alternating least squares.

PubMed

Ni, Yongnian; Wei, Min; Kokot, Serge

2011-11-01

Interaction of isoprenaline (ISO) with calf-thymus DNA was studied by spectroscopic and electrochemical methods. The behavior of ISO was investigated at a glassy carbon electrode (GCE) by cyclic voltammetry (CV) and differential pulse stripping voltammetry (DPSV); ISO was oxidized and an irreversible oxidation peak was observed. The binding constant K and the stoichiometric coefficient m of ISO with DNA were evaluated. Also, with the addition of DNA, hyperchromicity of the UV-vis absorption spectra of ISO was noted, while the fluorescence intensity decreased significantly. Multivariate curve resolution-alternating least squares (MCR-ALS) chemometrics method was applied to resolve the combined spectroscopic data matrix, which was obtained by the UV-vis and fluorescence methods. Pure spectra of ISO, DNA and ISO-DNA complex, and their concentration profiles were then successfully obtained. The results indicated that the ISO molecule intercalated into the base-pairs of DNA, and the complex of ISO-DNA was formed. Copyright © 2011 Elsevier B.V. All rights reserved.

Ultramicroelectrode voltammetry and scanning electrochemical microscopy in room-temperature ionic liquid electrolytes.

PubMed

Walsh, Darren A; Lovelock, Kevin R J; Licence, Peter

2010-11-01

The high viscosity and unusual properties of room temperature ionic liquids (RTILs) present a number of challenges when performing steady-state voltammetry and scanning electrochemical microscopy in RTILs. These include difficulties in recording steady-state currents at ultramicroelectrode surfaces due to low diffusion coefficients of redox species and problems associated with unequal diffusion coefficients of oxidised and reduced species in RTILs. In this tutorial review, we highlight the recent progress in the use of RTILs as electrolytes for ultramicroelectrode voltammetry and SECM. We describe the basic principles of ultramicroelectrode voltammetry and SECM and, using examples from the recent literature, we discuss the conditions that must be met to perform steady-state voltammetry and SECM measurements in RTILs. Finally, we briefly discuss the electrochemical insights that can be obtained from such measurements.

Recent Advances in Voltammetry

PubMed Central

Batchelor-McAuley, Christopher; Kätelhön, Enno; Barnes, Edward O; Compton, Richard G; Laborda, Eduardo; Molina, Angela

2015-01-01

Recent progress in the theory and practice of voltammetry is surveyed and evaluated. The transformation over the last decade of the level of modelling and simulation of experiments has realised major advances such that electrochemical techniques can be fully developed and applied to real chemical problems of distinct complexity. This review focuses on the topic areas of: multistep electrochemical processes, voltammetry in ionic liquids, the development and interpretation of theories of electron transfer (Butler–Volmer and Marcus–Hush), advances in voltammetric pulse techniques, stochastic random walk models of diffusion, the influence of migration under conditions of low support, voltammetry at rough and porous electrodes, and nanoparticle electrochemistry. The review of the latter field encompasses both the study of nanoparticle-modified electrodes, including stripping voltammetry and the new technique of ‘nano-impacts’. PMID:26246984

Metal molybdate nanorods as non-precious electrocatalysts for the oxygen reduction

NASA Astrophysics Data System (ADS)

Wu, Tian; Zhang, Lieyu

2015-12-01

Development of non-precious electrocatalysts with applicable electrocatalytic activity towards the oxygen reduction reaction (ORR) is important to fulfill broad-based and large-scale applications of metal/air batteries and fuel cells. Herein, nickel and cobalt molybdates with uniform nanorod morphology are synthesized using a facile one-pot hydrothermal method. The ORR activity of the prepared metal molybdate nanorods in alkaline media are investigated by using cyclic voltammetry (CV), linear sweep voltammetry (LSV) and chronoamperomety in rotating disk electrode (RDE) techniques. The present study suggests that the prepared metal molybdate nanorods exhibit applicable electrocatalytic activities towards the ORR in alkaline media, promising the applications as non-precious cathode in fuel cells and metal-air batteries.

Effect of Alternating Current on the Cathodic Protection and Interface Structure of X80 Steel.

PubMed

Wang, Huiru; Du, Cuiwei; Liu, Zhiyong; Wang, Luntao; Ding, De

2017-07-25

This study employs potential-monitoring techniques, cyclic voltammetry tests, alternating current (AC) voltammetry methods, and surface characterization to investigate the AC corrosion of cathodically protected X80 pipeline steel. In a non-passive neutral solution at pH 7.2, a sufficiently negative potential completely protects steel at an AC current density of 100 A/m². In an alkaline solution at pH 9.6, more serious AC corrosion occurs at more negative cathodic protection (CP) potential, whereas without CP the steel suffers negligible corrosion. In addition, the interface capacitance increases with AC amplitude. Based on these results, the AC corrosion mechanisms that function under various conditions are analyzed and described.

An approximate theoretical treatment of ion transfer processes at asymmetric microscopic and nanoscopic liquid-liquid interfaces: Single and double potential pulse techniques

NASA Astrophysics Data System (ADS)

Molina, A.; Laborda, E.; Compton, R. G.

2014-03-01

Simple theory for the electrochemical study of reversible ion transfer processes at micro- and nano-liquid|liquid interfaces supported on a capillary is presented. Closed-form expressions are obtained for the response in normal pulse and differential double pulse voltammetries, which describe adequately the particular behaviour of these systems due to the ‘asymmetric’ ion diffusion inside and outside the capillary. The use of different potential pulse techniques for the determination of the formal potential and diffusion coefficients of the ion is examined. For this, very simple analytical expressions are presented for the half-wave potential in NPV and the peak potential in DDPV.

Simultaneous determination of three herbicides by differential pulse voltammetry and chemometrics.

PubMed

Ni, Yongnian; Wang, Lin; Kokot, Serge

2011-01-01

A novel differential pulse voltammetry method (DPV) was researched and developed for the simultaneous determination of Pendimethalin, Dinoseb and sodium 5-nitroguaiacolate (5NG) with the aid of chemometrics. The voltammograms of these three compounds overlapped significantly, and to facilitate the simultaneous determination of the three analytes, chemometrics methods were applied. These included classical least squares (CLS), principal component regression (PCR), partial least squares (PLS) and radial basis function-artificial neural networks (RBF-ANN). A separately prepared verification data set was used to confirm the calibrations, which were built from the original and first derivative data matrices of the voltammograms. On the basis relative prediction errors and recoveries of the analytes, the RBF-ANN and the DPLS (D - first derivative spectra) models performed best and are particularly recommended for application. The DPLS calibration model was applied satisfactorily for the prediction of the three analytes from market vegetables and lake water samples.

Nanoalloy electrocatalysis: simulating cyclic voltammetry from configurational thermodynamics with adsorbates.

PubMed

Wang, Lin-Lin; Tan, Teck L; Johnson, Duane D

2015-11-14

We simulate the adsorption isotherms for alloyed nanoparticles (nanoalloys) with adsorbates to determine cyclic voltammetry (CV) during electrocatalysis. The effect of alloying on nanoparticle adsorption isotherms is provided by a hybrid-ensemble Monte Carlo simulation that uses the cluster expansion method extended to non-exchangeable coupled lattices for nanoalloys with adsorbates. Exemplified here for the hydrogen evolution reaction, a 2-dimensional CV is mapped for Pd-Pt nanoalloys as a function of both electrochemical potential and the global Pt composition, and shows a highly non-linear alloying effect on CV. Detailed features in CV arise from the interplay among the H-adsorption in multiple sites that is closely correlated with alloy configurations, which are in turn affected by the H-coverage. The origins of specific features in CV curves are assigned. The method provides a more complete means to design nanoalloys for electrocatalysis.

Nanoalloy electrocatalysis: Simulating cyclic voltammetry from configurational thermodynamics with adsorbates

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, Lin -Lin; Tan, Teck L.; Johnson, Duane D.

2015-02-27

We simulate the adsorption isotherms for alloyed nanoparticles (nanoalloys) with adsorbates to determine cyclic voltammetry (CV) during electrocatalysis. The effect of alloying on nanoparticle adsorption isotherms is provided by a hybrid-ensemble Monte Carlo simulation that uses the cluster expansion method extended to non-exchangeable coupled lattices for nanoalloys with adsorbates. Exemplified here for the hydrogen evolution reaction, a 2-dimensional CV is mapped for Pd–Pt nanoalloys as a function of both electrochemical potential and the global Pt composition, and shows a highly non-linear alloying effect on CV. Detailed features in CV arise from the interplay among the H-adsorption in multiple sites thatmore » is closely correlated with alloy configurations, which are in turn affected by the H-coverage. The origins of specific features in CV curves are assigned. As a result, the method provides a more complete means to design nanoalloys for electrocatalysis.« less

Synthesis and immobilization of Ag(0) nanoparticles on diazonium modified electrodes: SECM and cyclic voltammetry studies of the modified interfaces.

PubMed

Noël, Jean-Marc; Zigah, Dodzi; Simonet, Jacques; Hapiot, Philippe

2010-05-18

A versatile method was used to prepare modified surfaces on which metallic silver nanoparticles are immobilized on an organic layer. The preparation method takes advantage, on one hand, of the activated reactivity of some alkyl halides with Ag-Pd alloys to produce metallic silver nanoparticles and, on the other hand, of the facile production of an anchoring polyphenyl acetate layer by the electrografting of substituted diazonium salts on carbon surfaces. Transport properties inside such modified layers were investigated by cyclic voltammetry, scanning electrochemical microscopy (SECM) in feedback mode, and conducting AFM imaging for characterizing the presence and nature of the conducting pathways. The modification of the blocking properties of the surface (or its conductivity) was found to vary to a large extent on the solvents used for surface examination (H(2)O, CH(2)Cl(2), and DMF).

The use of cyclic voltammetry to study the oxidation of l-5-methyltetrahydrofolate and its preservation by ascorbic acid.

PubMed

Rozoy, Elodie; Simard, Stephan; Liu, Yazheng; Kitts, David; Lessard, Jean; Bazinet, Laurent

2012-06-01

A cyclic voltammetry study of 1mM l-5-methyltetrahydrofolate (l-5-MTHF) was performed in pH 5.5 Britton-Robinson buffer at room temperature to study the stability of l-5-MTHF alone and in combination with ascorbic acid (AA). The degradation of l-5-MTHF and AA over a period of 12h both followed first order reaction kinetics. Using this technique, oxidation peaks of l-5-MTHF were identified at +0.17 and +1.18V, and another oxidation peak appeared after 4h under air at +0.89V. Cyclic voltammetry and HPLC quantification enable us to confirm that l-5-MTHF can be highly preserved by the addition of an equimolar concentration of AA. This treatment was equivalent to a purge of nitrogen used to remove oxygen and thus minimise oxidation of l-5-MTHF when present in aqueous solutions. HPLC confirmed the fact that a full regeneration of oxidised l-5-MTHF occurred with the addition of sodium ascorbate, thus denoting that the redox character of l-5-MTHF can be controlled by the presence of reducing agents. Cyclic voltammetry proved to be a sensitive and accurate method for characterising l-5-MTHF oxidation and potential preservation with ascorbic acid. To our knowledge, this is the first study that has demonstrated the number of oxidation sites on l-5-MTHF. Copyright © 2011 Elsevier Ltd. All rights reserved.

A Practical Beginner's Guide to Cyclic Voltammetry

ERIC Educational Resources Information Center

Elgrishi, Noémie; Rountree, Kelley J.; McCarthy, Brian D.; Rountree, Eric S.; Eisenhart, Thomas T.; Dempsey, Jillian L.

2018-01-01

Despite the growing popularity of cyclic voltammetry, many students do not receive formalized training in this technique as part of their coursework. Confronted with self-instruction, students can be left wondering where to start. Here, a short introduction to cyclic voltammetry is provided to help the reader with data acquisition and…

Analytical methods for determination of free metal ion concentration, labile species fraction and metal complexation capacity of environmental waters: a review.

PubMed

Pesavento, Maria; Alberti, Giancarla; Biesuz, Raffaela

2009-01-12

Different experimental approaches have been suggested in the last few decades to determine metal species in complex matrices of unknown composition as environmental waters. The methods are mainly focused on the determination of single species or groups of species. The more recent developments in trace elements speciation are reviewed focusing on methods for labile and free metal determination. Electrochemical procedures with low detection limit as anodic stripping voltammetry (ASV) and the competing ligand exchange with adsorption cathodic stripping voltammetry (CLE-AdCSV) have been widely employed in metal distribution studies in natural waters. Other electrochemical methods such as stripping chronopotentiometry and AGNES seem to be promising to evaluate the free metal concentration at the low levels of environmental samples. Separation techniques based on ion exchange (IE) and complexing resins (CR), and micro separation methods as the Donnan membrane technique (DMT), diffusive gradients in thin-film gels (DGT) and the permeation liquid membrane (PLM), are among the non-electrochemical methods largely used in this field and reviewed in the text. Under appropriate conditions such techniques make possible the evaluation of free metal ion concentration.

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

PubMed

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

2013-03-15

This paper describes the use of 4-carboxyphenyl-grafted screen-printed carbon electrodes (4-CP-SPEs) for trace lead analysis. These novel and simple use of electrodes were easily prepared by the electrochemical reduction of the corresponding diazonium salt. Pb detection was then performed by a three-steps method in order to avoid oxygen interference: (i) immersion of the grafted screen-printed electrode (SPE) in the sample and adsorption of Pb(II), (ii) reduction of adsorbed Pb(II) by chronoamperometry (CA), and (iii) oxidation of Pb by Anodic Square Wave Voltammetry (SWV). The reoxidation response was exploited for lead detection and quantification. In order to optimize the analytical responses, the influence of the adsorption medium pH and the adsorption time were investigated. Moreover, an interference study was carried out with Cu(II), Hg(II), Al(III), Mn(II), Zn(II), Cd(II) and no major interference can be expected to quantify Pb(II). The described method provided a limit of detection and a limit of quantification of 1.2 × 10(-9)M and 4.1 × 10(-9)M, respectively. These performances indicate that the 4-CP-SPE could be considered as an efficient tool for environmental analysis. Copyright © 2013 Elsevier B.V. All rights reserved.

Examining the Complex Regulation and Drug-Induced Plasticity of Dopamine Release and Uptake Using Voltammetry in Brain Slices

PubMed Central

2013-01-01

Fast scan cyclic voltammetry in brain slices (slice voltammetry) has been used over the last several decades to increase substantially our understanding of the complex local regulation of dopamine release and uptake in the striatum. This technique is routinely used for the study of changes that occur in the dopamine system associated with various disease states and pharmacological treatments, and to study mechanisms of local circuitry regulation of dopamine terminal function. In the context of this Review, we compare the relative advantages of voltammetry using striatal slice preparations versus in vivo preparations, and highlight recent advances in our understanding of dopamine release and uptake in the striatum specifically from studies that use slice voltammetry in drug-naïve animals and animals with a history of psychostimulant self-administration. PMID:23581570

Adsorptive Stripping Voltammetric Determination of Amaranth and Tartrazine in Drinks and Gelatins Using a Screen-Printed Carbon Electrode

PubMed Central

Perdomo, Yeny; Arancibia, Verónica; Nagles, Edgar

2017-01-01

A fast, sensitive, and selective method for the simultaneous determination of one pair of synthetic colorants commonly found mixed in food products, Amaranth (AM) and Tartrazine (TZ), based on their adsorption and oxidation on a screen-printed electrode (SPE) is presented. The variation of peak current with pH, supporting electrolyte, adsorption time, and adsorption potential were optimized using square wave adsorptive voltammetry. The optimal conditions were found to be: pH 3.2 (PBS), Eads 0.00 V, and tads 30 s. Under these conditions, the AM and TZ signals were observed at 0.56 and 0.74 V, respectively. A linear response were found over the 0.15 to 1.20 µmol L−1 and 0.15 to 0.80 µmol L−1 concentrations, with detection limits (3σ/slope) of 26 and 70 nmol L−1 for AM and TZ, respectively. Reproducibility for 17.7 µmol L–1 AM and TZ solutions were 2.5 and 3.0% (n = 7), respectively, using three different electrodes. The method was validated by determining AM and TZ in spiked tap water and unflavored gelatin spiked with AM and TZ. Because a beverage containing both AM and TZ was not found, the method was applied to the determination of AM in a kola soft drink and TZ in an orange jelly and a soft drink powder. PMID:29156561

Cloud Point Extraction for Electroanalysis: Anodic Stripping Voltammetry of Cadmium

PubMed Central

Rusinek, Cory A.; Bange, Adam; Papautsky, Ian; Heineman, William R.

2016-01-01

Cloud point extraction (CPE) is a well-established technique for the pre-concentration of hydrophobic species from water without the use of organic solvents. Subsequent analysis is then typically performed via atomic absorption spectroscopy (AAS), UV-Vis spectroscopy, or high performance liquid chromatography (HPLC). However, the suitability of CPE for electroanalytical methods such as stripping voltammetry has not been reported. We demonstrate the use of CPE for electroanalysis using the determination of cadmium (Cd2+) by anodic stripping voltammetry (ASV) as a representative example. Rather than using the chelating agents which are commonly used in CPE to form a hydrophobic, extractable metal complex, we used iodide and sulfuric acid to neutralize the charge on Cd2+ to form an extractable ion pair. Triton X-114 was chosen as the surfactant for the extraction because its cloud point temperature is near room temperature (22–25° C). Bare glassy carbon (GC), bismuth-coated glassy carbon (Bi-GC), and mercury-coated glassy carbon (Hg-GC) electrodes were compared for the CPE-ASV. A detection limit for Cd2+ of 1.7 nM (0.2 ppb) was obtained with the Hg-GC electrode. Comparison of ASV analysis without CPE was also investigated and a 20x decrease (4.0 ppb) in the detection limit was observed. The suitability of this procedure for the analysis of tap and river water samples was also demonstrated. This simple, versatile, environmentally friendly and cost-effective extraction method is potentially applicable to a wide variety of transition metals and organic compounds that are amenable to detection by electroanalytical methods. PMID:25996561

Voltammetric behaviour of free DNA bases, methylcytosine and oligonucleotides at disposable screen printed graphite electrode platforms.

PubMed

Brotons, Ariadna; Mas, Luis Alcaraz; Metters, Jonathan P; Banks, Craig E; Iniesta, Jesús

2013-09-21

Improvements in analytical methods for the determination and quantification of methylcytosine in DNA are vital since it has the potential to be used as a biomarker to detect different diseases in the first stage such as in the case of carcinomas and sterility. In this work we utilized screen printed graphite electrodes (SPGE) for studying the electrochemical response of all free DNA bases, methylcytosine and short oligonucleotides by cyclic voltammetry (CV) and square wave voltammetry (SWV). CV and SWV responses of free DNA bases and methylcytosine have been investigated by using SPGE platforms and the feasibility of detecting and quantifying cytosine and methylcytosine as free DNA moieties has been evaluated as a function of pH, concentration and the presence of the other free DNA bases in solution simultaneously. Repeatability of using SWV has been performed for the electrochemical behavior of both 250 μM cytosine and 250 μM methylcytosine in the presence of 25 μM guanine, with coefficient of variations of 6.9% and 2.6% respectively based upon peak current (N = 5). Six-mer oligonucleotides with a sequence 5'-XXXCGC-3', where the XXX motif corresponds to TTT, TTA, TAA and AAA have been performed using SWV in 0.1 M acetate buffer pH 5.0 to explore how the DNA base position effects the electrooxidation of guanine and cytosine into the oligonucleotide. Furthermore SWV comparisons of the electrooxidation of the oligonucleotides 5'-CGCGCG-3' and its methylated 5'-mCGmCGmCG-3' have been performed with concentrations in acetate buffer solutions, and the interaction of both oligonucleotides with the graphitic surface of the SPGE has been demonstrated by fitting well-known adsorption models such as Freundlich and Langmuir kinetics according to the SWV current response of guanine, cytosine and methylcytosine into the oligonucleotide.

Preparation of magnetic TNT-imprinted polymer nanoparticles and their accumulation onto magnetic carbon paste electrode for TNT determination.

PubMed

Alizadeh, Taher

2014-11-15

In this study, the TNT-imprinted polymer shell was created on nano-sized Fe3O4 cores in order to construct the nano-sized magnetic molecularly imprinted polymer (nano-MMIP). For this purpose, the surface of the synthesized magnetic nanoparticles was modified with methacrylic acid. The modified particles were then utilized as the core on which the TNT-imprinted polymeric shell was synthesized. The synthesized materials were then characterized by scanning electron microscopy, FT-IR and thermal gravimetric analysis (TGA). The resulting nano-MMIP particles were suspended in TNT solution and then collected on the surface of a carbon paste electrode via a permanent magnet, situated within the CP electrode. The extracted TNT was analyzed on the CP electrode by applying square wave voltammetry (SWV). It was found that the oxidative signal of TNT is much favorable for TNT detection on the resulting magnetic carbon paste electrode. The electrode with nano-MMIP showed distinctly higher signal to TNT, compared to that containing magnetic non-imprinted polymer (MNIP) nanoparticles. All parameters influencing the method performance including extraction pH, extraction time and sorbent amount were evaluated and optimized. The developed method showed a dynamic linear concentration range of 1.0-130.0 nM for TNT measurement. The detection limit of the method was calculated to be 0.5 nM. The method showed appropriate capability for TNT analysis in real water samples. Copyright © 2014. Published by Elsevier B.V.

Use B-spline interpolation fitting baseline for low concentration 2, 6-di-tertbutyl p-cresol determination in jet fuels by differential pulse voltammetry

NASA Astrophysics Data System (ADS)

Wen, D. S.; Wen, H.; Shi, Y. G.; Su, B.; Li, Z. C.; Fan, G. Z.

2018-01-01

The B-spline interpolation fitting baseline in electrochemical analysis by differential pulse voltammetry was established for determining the lower concentration 2,6-di-tert-butyl p-cresol(BHT) in Jet Fuel that was less than 5.0 mg/L in the condition of the presence of the 6-tert-butyl-2,4-xylenol.The experimental results has shown that the relative errors are less than 2.22%, the sum of standard deviations less than 0.134mg/L, the correlation coefficient more than 0.9851. If the 2,6-ditert-butyl p-cresol concentration is higher than 5.0mg/L, linear fitting baseline method would be more applicable and simpler.

Effect of Alternating Current on the Cathodic Protection and Interface Structure of X80 Steel

PubMed Central

Wang, Huiru; Du, Cuiwei; Liu, Zhiyong; Wang, Luntao; Ding, De

2017-01-01

This study employs potential-monitoring techniques, cyclic voltammetry tests, alternating current (AC) voltammetry methods, and surface characterization to investigate the AC corrosion of cathodically protected X80 pipeline steel. In a non-passive neutral solution at pH 7.2, a sufficiently negative potential completely protects steel at an AC current density of 100 A/m2. In an alkaline solution at pH 9.6, more serious AC corrosion occurs at more negative cathodic protection (CP) potential, whereas without CP the steel suffers negligible corrosion. In addition, the interface capacitance increases with AC amplitude. Based on these results, the AC corrosion mechanisms that function under various conditions are analyzed and described. PMID:28773211

Studying Current-Potential Curves Using a Bipotentiometric Lodometric Back-Titration for the Determination of Ascorbic Acid in Fruits and Vegetables

ERIC Educational Resources Information Center

Verdini, Roxana A.; Lagier, Claudia M.

2004-01-01

Voltammetry principles are introduced to students by means of a bipotentiometric method to determine vitamin C in fruits and vegetables. The aim is to draw attention to voltammetric methods, particular to the study of current-potential curves, stressing the potential applicability in areas of food quality control.

Investigating Arsenic Contents in Surface and Drinking Water by Voltammetry and the Method of Standard Additions

ERIC Educational Resources Information Center

Cheng, Anran; Tyne, Rebecca; Kwok, Yu Ting; Rees, Louis; Craig, Lorraine; Lapinee, Chaipat; D'Arcy, Mitch; Weiss, Dominik J.; Salau¨n, Pascal

2016-01-01

Testing water samples for arsenic contamination has become an important water quality issue worldwide. Arsenic usually occurs in very small concentrations, and a sensitive analytical method is needed. We present here a 1-day laboratory module developed to introduce Earth Sciences and/or Chemistry student undergraduates to key aspects of this…

Detailed electrochemical studies of the tetraruthenium polyoxometalate water oxidation catalyst in acidic media: identification of an extended oxidation series using Fourier transformed alternating current voltammetry.

PubMed

Lee, Chong-Yong; Guo, Si-Xuan; Murphy, Aidan F; McCormac, Timothy; Zhang, Jie; Bond, Alan M; Zhu, Guibo; Hill, Craig L; Geletii, Yurii V

2012-11-05

The electrochemistry of the water oxidation catalyst, Rb(8)K(2)[{Ru(4)O(4)(OH)(2)(H(2)O)(4)}(γ-SiW(10)O(36))(2)] (Rb(8)K(2)-1(0)) has been studied in the presence and absence of potassium cations in both hydrochloric and sulfuric acid solutions by transient direct current (dc) cyclic voltammetry, a steady state dc method in the rotating disk configuration and the kinetically sensitive technique of Fourier transformed large-amplitude alternating current (ac) voltammetry. In acidic media, the presence of potassium ions affects the kinetics (apparent rate of electron transfer) and thermodynamics (reversible potentials) of the eight processes (A'/A to H/H') that are readily detected under dc voltammetric conditions. The six most positive processes (A'/A to F/F'), each involve a one electron ruthenium based charge transfer step (A'/A, B'/B are Ru(IV/V) oxidation and C/C' to F/F' are Ru(IV/III) reduction). The apparent rate of electron transfer of the ruthenium centers in sulfuric acid is higher than in hydrochloric acid. The addition of potassium cations increases the apparent rates and gives rise to a small shift of reversible potential. Simulations of the Fourier transformed ac voltammetry method show that the B'/B, E/E', and F/F' processes are quasi-reversible, while the others are close to reversible. A third Ru(IV/V) oxidation process is observed just prior to the positive potential limit via dc methods. Importantly, the ability of the higher harmonic components of the ac method to discriminate against the irreversible background solvent process allows this (process I) as well as an additional fourth reversible ruthenium based process (J) to be readily identified. The steady-state rotating disk electrode (RDE) method confirmed that all four Ru-centers in Rb(8)K(2)-1(0) are in oxidation state IV. The dc and ac data indicate that reversible potentials of the four ruthenium centers are evenly spaced, which may be relevant to understanding of the water oxidation electrocatalysis. A profound effect of the potassium cation is observed for the one-electron transfer process (G/G') assigned to Ru(III/II) reduction and the multiple electron transfer reduction process (H/H') that arise from the tungstate polyoxometalate framework. A significant shift of E°' to a more positive potential value for process H/H' was observed on removal of K(+) (~100 mV in H(2)SO(4) and ~50 mV in HCl).

Amperometric detection of catechol using tyrosinase modified electrodes enhanced by the layer-by-layer assembly of gold nanocubes and polyelectrolytes.

PubMed

Karim, Md Nurul; Lee, Ji Eun; Lee, Hye Jin

2014-11-15

A novel amperometric biosensor for catechol was developed using the layer-by-layer (LbL) self-assembly of positively charged hexadecyltrimethylammonium stabilized gold nanocubes (AuNCs), negatively charged poly(sodium 4-styrenesulfonate) and tyrosinase on a screen printed carbon electrode (SPCE). A carboxylic acid terminated alkanethiol assembled on electrochemically deposited Au nanoparticles on a SPCE was used as a platform for LbL assembly. Each SPCE sensor surface was terminated with tyrosinase and the electrocatalytic response due to the tyrosinase reaction with catechol was measured using cyclic voltammetry and square wave voltammetry (SWV). The effect of introducing AuNCs into the LbL assembly to further enhance the catechol detection performance was then investigated by comparing the SWV results to those from biosensors created using both the tyrosinase modified LbL assembly in the absence of NCs and the covalent attachment of tyrosinase. A wide dynamic range from 10nM to 80 µM of catechol with an excellent sensitivity of 13.72 A/M and a detection limit of 0.4 nM were both achieved alongside a good selectivity and reproducibility for the AuNC-modified electrodes. As a demonstration, the optimized biosensor design was applied to determine catechol concentrations in tea samples. Copyright © 2014 Elsevier B.V. All rights reserved.

Theoretical Treatment of Ion Transfers in Two Polarizable Interface Systems When the Analyte Has Access to Both Interfaces.

PubMed

Olmos, José Manuel; Molina, Ángela; Laborda, Eduardo; Millán-Barrios, Enrique; Ortuño, Joaquín Ángel

2018-02-06

A new theory is presented to tackle the study of transfer processes of hydrophilic ions in two polarizable interface systems when the analyte is initially present in both aqueous phases. The treatment is applied to macrointerfaces (linear diffusion) and microholes (highly convergent diffusion), obtaining analytical equations for the current response in any voltammetric technique. The novel equations predict two signals in the current-potential curves that are symmetric when the compositions of the aqueous phases are identical while asymmetries appear otherwise. The theoretical results show good agreement with the experimental behavior of the "double transfer voltammograms" reported by Dryfe et al. in cyclic voltammetry (CV) ( Anal. Chem. 2014 , 86 , 435 - 442 ) as well as with cyclic square wave voltammetry (cSWV) experiments performed in the current work. The theoretical treatment is also extended to the situation where the target ion is lipophilic and initially present in the organic phase. The theory predicts an opposite effect of the lipophilicity of the ion on the shape of the voltammograms, which is validated experimentally via both CV and cSWV. For the above two cases, simple and manageable expressions and diagnosis criteria are derived for the qualitative and quantitative study of ion lipophilicity. The ion-transfer potentials can be easily quantified from the separation between the two signals making use of explicit analytical equations.

Synthesis and (spectro)electrochemistry of mixed-valent diferrocenyl-dihydrothiopyran derivatives.

PubMed

Kowalski, Konrad; Karpowicz, Rafał; Mlostoń, Grzegorz; Miesel, Dominique; Hildebrandt, Alexander; Lang, Heinrich; Czerwieniec, Rafał; Therrien, Bruno

2015-04-07

Three novel diferrocenyl complexes were prepared and characterised. 2,2-Diferrocenyl-4,5-dimethyl-3,6-dihydro-2H-thiopyran (1, sulphide) was accessible by the hetero-Diels-Alder reaction of diferrocenyl thioketone with 2,3-dimethyl-1,3-butadiene. Stepwise oxidation of 1 gave the respective oxides 2,2-diferrocenyl-4,5-dimethyl-3,6-dihydro-2H-thiopyran-1-oxide (2, sulfoxide) and 2,2-diferrocenyl-4,5-dimethyl-3,6-dihydro-2H-thiopyran-1,1-dioxide (3, sulfone), respectively. The molecular structures of 1 and 3 in the solid state were determined by single crystal X-ray crystallography. The oxidation of sulphide 1 to sulfone 3, plays only a minor role on the overall structure of the two compounds. Electrochemical (cyclic voltammetry (= CV), square wave voltammetry (= SWV)) and spectroelectrochemical (in situ UV-Vis/NIR spectroscopy) studies were carried out. The CV and SWV measurements showed that an increase of the sulphur atom oxidation from -2 in 1 to +2 in 3 causes an anodic shift of the ferrocenyl-based oxidation potentials of about 100 mV. The electrochemical oxidation of 1-3 generates mixed-valent cations 1(+)-3(+). These monooxidised species display low-energy electronic absorption bands between 1000 and 3000 nm assigned to IVCT (= Inter-Valence Charge Transfer) electronic transitions. Accordingly, the mixed-valent cations 1(+)-3(+) are classified as weakly coupled class II systems according to Robin and Day.

In vitro chloramphenicol detection in a Haemophilus influenza model using an aptamer-polymer based electrochemical biosensor.

PubMed

Yadav, Saurabh K; Agrawal, Bharati; Chandra, Pranjal; Goyal, Rajendra N

2014-05-15

A sensitive and selective electrochemical biosensor is developed for the determination of chloramphenicol (CAP) exploring its direct electron transfer processes in in-vitro model and pharmaceutical samples. This biosensor exploits a selective binding of CAP with aptamer, immobilized onto the poly-(4-amino-3-hydroxynapthalene sulfonic acid) (p-AHNSA) modified edge plane pyrolytic graphite. The electrochemical reduction of CAP was observed in a well-defined peak. A quartz crystal microbalance (QCM) study is performed to confirm the interaction between the polymer film and the aptamer. Cyclic voltammetry (CV) and square wave voltammetry (SWV) were used to detect CAP. The in-vitro CAP detection is performed using the bacterial strain of Haemophilus influenza. A significant accumulation of CAP by the drug sensitive H. influenza strain is observed for the first time in this study using a biosensor. Various parameters affecting the CAP detection in standard solution and in in vitro detection are optimized. The detection of CAP is linear in the range of 0.1-2500 nM with the detection limit and sensitivity of 0.02 nM and 0.102 µA/nM, respectively. CAP is also detected in the presence of other common antibiotics and proteins present in the real sample matrix, and negligible interference is observed. Copyright © 2013 Elsevier B.V. All rights reserved.

Electrochemical determination of paraquat in citric fruit based on electrodeposition of silver particles onto carbon paste electrode.

PubMed

Farahi, Abdelfettah; Achak, Mounia; El Gaini, Laila; El Mhammedi, Moulay Abderrahim; Bakasse, Mina

2015-09-01

Carbon paste electrodes (CPEs) modified with silver particles present an interesting tool in the determination of paraquat (PQ) using square wave voltammetry. Metallic silver particle deposits have been obtained via electrochemical deposition in acidic media using cyclic voltammetry. Scanning electron microscopy and X-ray diffraction measurements show that the silver particles are deposited onto carbon surfaces in aggregate form. The response of PQ with modified electrode (Ag-CPE) related to Ag/CP loading, preconcentration time, and measuring solution pH was investigated. The result shows that the increase in the two cathodic peak currents (Peak 1 and Peak 2), under optimized conditions, was linear with the increase in PQ concentration in the range 1.0 × 10 -7  mol/L to 1.0 × 10 -3  mol/L. The detection limit and quantification limit were 2.01 × 10 -8  mol/L and 6.073 × 10 -8  mol/L, respectively for Peak 1. The precision expressed as relative standard deviation for the concentration level 1.0 × 10 -5  mol/L (n = 8) was found to be 1.45%. The methodology was satisfactorily applied for the determination of PQ in citric fruit cultures. Copyright © 2015. Published by Elsevier B.V.

Dopamine and uric acid electrochemical sensor based on a glassy carbon electrode modified with cubic Pd and reduced graphene oxide nanocomposite.

PubMed

Wang, Jin; Yang, Beibei; Zhong, Jiatai; Yan, Bo; Zhang, Ke; Zhai, Chunyang; Shiraishi, Yukihide; Du, Yukou; Yang, Ping

2017-07-01

A cubic Pd and reduced graphene oxide modified glassy carbon electrode (Pd/RGO/GCE) was fabricated to simultaneously detect dopamine (DA) and uric acid (UA) by cyclic voltammetry (CV) and different pulse voltammetry (DPV) methods. Compared with Pd/GCE and RGO/GCE, the Pd/RGO/GCE exhibited excellent electrochemical activity in electrocatalytic behaviors. Performing the Pd/RGO/GCE in CV measurement, the well-defined oxidation peak potentials separation between DA and UA reached to 145mV. By using the differential pulse voltammetry (DPV) technique, the calibration curves for DA and UA were found linear with the concentration range of 0.45-421μM and 6-469.5μM and the detection limit (S/N =3) were calculated to be 0.18μM and 1.6μM, respectively. Furthermore, the Pd/RGO/GCE displayed high selectivity when it was applied into the determination of DA and UA even though in presence of high concentration of interferents. Additionally, the prepared electrochemical sensor of Pd/RGO/GCE demonstrated a practical feasibility in rat urine and serum samples determination. Copyright © 2017 Elsevier Inc. All rights reserved.

Assessing Principal Component Regression Prediction of Neurochemicals Detected with Fast-Scan Cyclic Voltammetry

PubMed Central

2011-01-01

Principal component regression is a multivariate data analysis approach routinely used to predict neurochemical concentrations from in vivo fast-scan cyclic voltammetry measurements. This mathematical procedure can rapidly be employed with present day computer programming languages. Here, we evaluate several methods that can be used to evaluate and improve multivariate concentration determination. The cyclic voltammetric representation of the calculated regression vector is shown to be a valuable tool in determining whether the calculated multivariate model is chemically appropriate. The use of Cook’s distance successfully identified outliers contained within in vivo fast-scan cyclic voltammetry training sets. This work also presents the first direct interpretation of a residual color plot and demonstrated the effect of peak shifts on predicted dopamine concentrations. Finally, separate analyses of smaller increments of a single continuous measurement could not be concatenated without substantial error in the predicted neurochemical concentrations due to electrode drift. Taken together, these tools allow for the construction of more robust multivariate calibration models and provide the first approach to assess the predictive ability of a procedure that is inherently impossible to validate because of the lack of in vivo standards. PMID:21966586

Assessing principal component regression prediction of neurochemicals detected with fast-scan cyclic voltammetry.

PubMed

Keithley, Richard B; Wightman, R Mark

2011-06-07

Principal component regression is a multivariate data analysis approach routinely used to predict neurochemical concentrations from in vivo fast-scan cyclic voltammetry measurements. This mathematical procedure can rapidly be employed with present day computer programming languages. Here, we evaluate several methods that can be used to evaluate and improve multivariate concentration determination. The cyclic voltammetric representation of the calculated regression vector is shown to be a valuable tool in determining whether the calculated multivariate model is chemically appropriate. The use of Cook's distance successfully identified outliers contained within in vivo fast-scan cyclic voltammetry training sets. This work also presents the first direct interpretation of a residual color plot and demonstrated the effect of peak shifts on predicted dopamine concentrations. Finally, separate analyses of smaller increments of a single continuous measurement could not be concatenated without substantial error in the predicted neurochemical concentrations due to electrode drift. Taken together, these tools allow for the construction of more robust multivariate calibration models and provide the first approach to assess the predictive ability of a procedure that is inherently impossible to validate because of the lack of in vivo standards.

Micropatterned ferrocenyl monolayers covalently bound to hydrogen-terminated silicon surfaces: effects of pattern size on the cyclic voltammetry and capacitance characteristics.

PubMed

Fabre, Bruno; Pujari, Sidharam P; Scheres, Luc; Zuilhof, Han

2014-06-24

The effect of the size of patterns of micropatterned ferrocene (Fc)-functionalized, oxide-free n-type Si(111) surfaces was systematically investigated by electrochemical methods. Microcontact printing with amine-functionalized Fc derivatives was performed on a homogeneous acid fluoride-terminated alkenyl monolayer covalently bound to n-type H-terminated Si surfaces to give Fc patterns of different sizes (5 × 5, 10 × 10, and 20 × 20 μm(2)), followed by backfilling with n-butylamine. These Fc-micropatterned surfaces were characterized by static water contact angle measurements, ellipsometry, X-ray photoelectron spectroscopy (XPS), infrared reflection-absorption spectroscopy (IRRAS), atomic force microscopy (AFM), and scanning electron microscopy (SEM). The charge-transfer process between the Fc-micropatterned and underlying Si interface was subsequently studied by cyclic voltammetry and capacitance. By electrochemical studies, it is evident that the smallest electroactive ferrocenyl patterns (i.e., 5 × 5 μm(2) squares) show ideal surface electrochemistry, which is characterized by narrow, perfectly symmetric, and intense cyclic voltammetry and capacitance peaks. In this respect, strategies are briefly discussed to further improve the development of photoswitchable charge storage microcells using the produced redox-active monolayers.

Nucleic acid sensor for insecticide detection.

PubMed

Solanki, Pratima R; Prabhakar, Nirmal; Pandey, M K; Malhotra, B D

2008-01-01

Nucleic acid sensor based on polyaniline (PANI) has been fabricated by covalently immobilizing double stranded calf thymus (dsCT) DNA onto perchlorate (ClO(-) (4))-doped PANI film deposited onto indium-tin-oxide (ITO) glass plate using 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (EDC)/N-hydroxysuccinimide (NHS) chemistry. These dsCT-DNA-PANI-ClO(4)/ITO and PANI-ClO(4)/ITO electrodes have been characterized using square wave voltammetry, electrochemical impedance, scanning electron microscopy (SEM) and Fourier-transform-infrared (FTIR) measurements. This disposable dsCT-DNA-PANI-ClO(4)/ITO bioelectrode, stable for about 4 months, can be used to detect cypermethrin (0.005 ppm) and trichlorfon (0.01 ppm) in 30 and 60 s, respectively. John Wiley & Sons, Ltd

Pd0@Polyoxometalate Nanostructures as Green Electrocatalysts: Illustrative Example of Hydrogen Production

PubMed Central

Biboum, Rosa N.; Keita, Bineta; Franger, Sylvain; Njiki, Charles P. Nanseu; Zhang, Guangjin; Zhang, Jie; Liu, Tianbo; Mbomekalle, Israel-Martyr; Nadjo, Louis

2010-01-01

Green-chemistry type procedures were used to synthesize Pd0 nanostructures encapsulated by a vanadium-substituted Wells-Dawson-type polyoxometalate (Pd0@POM). The cyclic voltammogram run with the Pd0@POM-modified glassy carbon electrode shows well-defined waves, associated with Pd0 nanostructures and the VV/VIV redox couple. The Pd0@POM-modified electrode displayed remarkably reproducible cyclic voltammetry patterns. The hydrogen evolution reaction (HER) was selected as an illustrative example to test the electrocatalytic behavior of the electrode. The kinetic parameters of the HER show the high efficiency of the Pd0@POM-modified electrode. This is the first example of electrochemical characterization of a modified electrode based on a vanado-tungstic POM and Pd0 nanostructures.

A new synthetic route to the preparation of a series of strong photoreducing agents: fac Tris-ortho-metalated complexes of iridium(III) with substituted 2-phenylpyridines

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhang, Y.; Baer, C.D.; Camaioni-Neto, C.

1991-04-17

A new procedure is reported for the high-yield synthesis of fac-tris-ortho-metalated complexes of Ir(III) with 2-phenylpyridine (Hppy) and with substituted 2-phenylpyridine (R-Hppy) ligands. The reported procedure uses the Ir(III) starting material Ir(acac){sub 3} (acac = 2,4-pentanedionate) and typically produces the fac-tris-ortho-metalated complexes in yields of 40-75%. Each of the complexes formed with substituted phenylpyridines exhibited a luminescence lifetime of approximately 2-5 microseconds in nitrogen-saturated acetonitrile at room temperature, and each complex is characterized by a reversible oxidative wave in cyclic voltammetry in acetonitrile. 42 refs., 1 fig., 1 tab.

Anodic Stripping Voltammetry with Pencil Graphite Electrode for Determination of Chromium (III)

NASA Astrophysics Data System (ADS)

Wyantuti, S.; Hafidza, R. A.; Ishmayana, S.; Hartati, Y. W.

2017-02-01

Chromium is required as micronutrient that has roles in insulin metabolism and blood glucose level regulation. Chromium (III) deficiency can cause hyperglycemia and glycosuria. However, a high amount of chromium in body can cause allergic reaction, organ damage, and even death because of its toxicity. Chromium is commonly used in steel industries. Simultaneously with the development of industry, the waste disposal that can endanger environment also increased. Therefore, a sensitive and specific analysis method for chromium detection is required. Stripping voltammetry is one of the voltammetric methods that is commonly used for heavy metal analysis due to the very low limit of detection (sub ppb). The present study was conducted to develop an analysis method for chromium (III) determination using pencil graphite electrode. Quantitative determination was performed for chromium (III) which measured at -0.8 to +1.0 V with deposition time for 60 s and 50 mV/s scan rate. Stripping voltammetric analysis of chromium (III) using pencil graphite electrode gave linear range at 12.5 to 75 ppm with limit of detection of 0.31 ppm.

Electrochemical Behavior and Determination of Chlorogenic Acid Based on Multi-Walled Carbon Nanotubes Modified Screen-Printed Electrode

PubMed Central

Ma, Xiaoyan; Yang, Hongqiao; Xiong, Huabin; Li, Xiaofen; Gao, Jinting; Gao, Yuntao

2016-01-01

In this paper, the multi-walled carbon nanotubes modified screen-printed electrode (MWCNTs/SPE) was prepared and the MWCNTs/SPE was employed for the electrochemical determination of the antioxidant substance chlorogenic acids (CGAs). A pair of well-defined redox peaks of CGA was observed at the MWCNTs/SPE in 0.10 mol/L acetic acid-sodium acetate buffer (pH 6.2) and the electrode process was adsorption-controlled. Cyclic voltammetry (CV) and differential pulse voltammetry (DPV) methods for the determination of CGA were proposed based on the MWCNTs/SPE. Under the optimal conditions, the proposed method exhibited linear ranges from 0.17 to 15.8 µg/mL, and the linear regression equation was Ipa (µA) = 4.1993 C (×10−5 mol/L) + 1.1039 (r = 0.9976) and the detection limit for CGA could reach 0.12 µg/mL. The recovery of matrine was 94.74%–106.65% (RSD = 2.92%) in coffee beans. The proposed method is quick, sensitive, reliable, and can be used for the determination of CGA. PMID:27801797

Cloud Point Extraction for Electroanalysis: Anodic Stripping Voltammetry of Cadmium.

PubMed

Rusinek, Cory A; Bange, Adam; Papautsky, Ian; Heineman, William R

2015-06-16

Cloud point extraction (CPE) is a well-established technique for the preconcentration of hydrophobic species from water without the use of organic solvents. Subsequent analysis is then typically performed via atomic absorption spectroscopy (AAS), UV-vis spectroscopy, or high performance liquid chromatography (HPLC). However, the suitability of CPE for electroanalytical methods such as stripping voltammetry has not been reported. We demonstrate the use of CPE for electroanalysis using the determination of cadmium (Cd(2+)) by anodic stripping voltammetry (ASV). Rather than using the chelating agents which are commonly used in CPE to form a hydrophobic, extractable metal complex, we used iodide and sulfuric acid to neutralize the charge on Cd(2+) to form an extractable ion pair. This offers good selectivity for Cd(2+) as no interferences were observed from other heavy metal ions. Triton X-114 was chosen as the surfactant for the extraction because its cloud point temperature is near room temperature (22-25 °C). Bare glassy carbon (GC), bismuth-coated glassy carbon (Bi-GC), and mercury-coated glassy carbon (Hg-GC) electrodes were compared for the CPE-ASV. A detection limit for Cd(2+) of 1.7 nM (0.2 ppb) was obtained with the Hg-GC electrode. ASV with CPE gave a 20x decrease (4.0 ppb) in the detection limit compared to ASV without CPE. The suitability of this procedure for the analysis of tap and river water samples was demonstrated. This simple, versatile, environmentally friendly, and cost-effective extraction method is potentially applicable to a wide variety of transition metals and organic compounds that are amenable to detection by electroanalytical methods.

ESR, electrochemical and cyclodextrin-inclusion studies of triazolopyridyl pyridyl ketones and dipyridyl ketones derivatives

NASA Astrophysics Data System (ADS)

Olea-Azar, C.; Abarca, B.; Norambuena, E.; Opazo, L.; Jullian, C.; Valencia, S.; Ballesteros, R.; Chadlaoui, M.

2008-11-01

The electron spin resonance (ESR) spectra of free radicals obtained by electrolytic reduction of triazolopyridyl pyridyl ketones and dipyridyl ketones derivatives were measured in dimethylsulfoxide (DMSO). The hyperfine patterns indicate that the spin density delocalization is dependent of the rings presented in the molecule. The electrochemistry of these compounds was characterized using cyclic voltammetry, in DMSO as solvent. When one carbonyl is present in the molecule one step in the reduction mechanism was observed while two carbonyl are present two steps were detected. The first wave was assigned to the generation of the correspondent free radical species, and the second wave was assigned to the dianion derivatives. The phase-solubility measurements indicated an interaction between molecules selected and cyclodextrins in water. These inclusion complexes are 1:1 with βCD, and HP-βCD. The values of Ks showed a different kind of complexes depending on which rings are included. AM1 and DFT calculations were performed to obtain the optimized geometries, theoretical hyperfine constants, and spin distributions, respectively. The theoretical results are in complete agreement with the experimental ones.

Electrochemistry of redox-active self-assembled monolayers

PubMed Central

Eckermann, Amanda L.; Feld, Daniel J.; Shaw, Justine A.; Meade, Thomas J.

2010-01-01

Redox-active self-assembled monolayers (SAMs) provide an excellent platform for investigating electron transfer kinetics. Using a well-defined bridge, a redox center can be positioned at a fixed distance from the electrode and electron transfer kinetics probed using a variety of electrochemical techniques. Cyclic voltammetry, AC voltammetry, electrochemical impedance spectroscopy, and chronoamperometry are most commonly used to determine the rate of electron transfer of redox-activated SAMs. A variety of redox species have been attached to SAMs, and include transition metal complexes (e.g., ferrocene, ruthenium pentaammine, osmium bisbipyridine, metal clusters) and organic molecules (e.g., galvinol, C60). SAMs offer an ideal environment to study the outer-sphere interactions of redox species. The composition and integrity of the monolayer and the electrode material influence the electron transfer kinetics and can be investigated using electrochemical methods. Theoretical models have been developed for investigating SAM structure. This review discusses methods and monolayer compositions for electrochemical measurements of redox-active SAMs. PMID:20563297

Low-cost and reagent-free paper-based device to detect chloride ions in serum and sweat.

PubMed

Cinti, Stefano; Fiore, Luca; Massoud, Renato; Cortese, Claudio; Moscone, Danila; Palleschi, Giuseppe; Arduini, Fabiana

2018-03-01

The recent goal of sustainability in analytical chemistry has boosted the development of eco-designed analytical tools to deliver fast and cost-effective analysis with low economic and environmental impact. Due to the recent focus in sustainability, we report the use of low-cost filter paper as a sustainable material to print silver electrodes and to load reagents for a reagent-free electrochemical detection of chloride in biological samples, namely serum and sweat. The electrochemical detection of chloride ions was carried out by exploiting the reaction of the analyte (i.e. chloride) with the silver working electrode. During the oxidation wave in cyclic voltammetry the silver ions are produced, thus they react with chloride ions to form AgCl, while in the reduction wave, the following reaction occurs: AgCl + e - -->Ag + Cl - . These reactions at the electrode surface resulted in anodic/cathodic peaks directly proportional to the chloride ions in solution. Chloride ions were detected with the addition of only 10μL of the sample on the paper-based electrochemical cell, obtaining linearity up to 200mM with a detection limit equal to 1mM and relative standard deviation lower than 10%. The accuracy of the sensor was evaluated in serum and sweat samples, with percentage recoveries between 93 ± 10 and 108 ± 8%. Moreover, the results achieved with the paper-based device were positively compared with those obtained by using the gold standard method (Ion Selective Electrode) adopted in routine clinical analyses. Copyright © 2017 Elsevier B.V. All rights reserved.

Architecture-dependent surface chemistry for Pt monolayers on carbon-supported Au.

PubMed

Cheng, Shuang; Rettew, Robert E; Sauerbrey, Marc; Alamgir, Faisal M

2011-10-01

Pt monolayers were grown by surface-limited redox replacement (SLRR) on two types of Au nanostructures. The Au nanostructures were fabricated electrochemically on carbon fiber paper (CFP) by either potentiostatic deposition (PSD) or potential square wave deposition (PSWD). The morphology of the Au/CFP heterostructures, examined using scanning electron microscopy (SEM), was found to depend on the type of Au growth method employed. The properties of the Pt deposit, as studied using X-ray photoelectron spectroscopy (XPS), X-ray absorption spectroscopy (XAS), and cyclic voltammetry (CV), were found to depend strongly on the morphology of the support. Specifically, it was found that smaller Au morphologies led to a higher degree of cationicity in the resulting Pt deposit, with Pt(4+) and Pt(2+) species being identified using XPS and XAS. For fuel-cell catalysts, the resistance of ultrathin catalyst deposits to surface area loss through dissolution, poisoning, and agglomeration is critical. This study shows that an equivalent of two monolayers (ML) is the low-loading limit of Pt on Au. At 1 ML or below, the Pt film decreases in activity and durability very rapidly due to presence of cationic Pt. © 2011 American Chemical Society

A novel conducting poly(p-aminobenzene sulphonic acid)-based electrochemical sensor for sensitive determination of Sudan I and its application for detection in food stuffs.

PubMed

Li, Bang Lin; Luo, Jun Hua; Luo, Hong Qun; Li, Nian Bing

2015-04-15

In the present work, a new method for the determination of Sudan I has been developed based on a conducting poly(p-aminobenzene sulphonic acid) (poly(p-ABSA)) film modified electrode. The new electrochemical sensor showed strong accumulation ability and excellent electrocatalytic activity for Sudan I. Electrochemical oxidation signal of Sudan I at the poly(p-ABSA) modified glassy carbon electrode (poly(p-ABSA)/GCE) was significantly increased when compared to that at the bare GCE. The experimental conditions such as amount of alcohol, pH of buffer solution, accumulation time, and instrumental parameters for square wave anodic stripping voltammetry were optimised for the determination of Sudan I. Under optimum conditions, the linear regression equation of Sudan I was ip=1.868+0.1213c (ip: μA, c: μgL(-1), R=0.9981) from 1 to 500 μg L(-1) with a detection limit of 0.3 μg L(-1). Finally, this sensor was successfully employed to detect Sudan I in some hot chili and ketchup samples. Copyright © 2014 Elsevier Ltd. All rights reserved.

One pot synthesis of dandelion-like polyaniline coated gold nanoparticles composites for electrochemical sensing applications.

PubMed

Lu, Zhiwei; Dai, Wanlin; Liu, Baichen; Mo, Guangquan; Zhang, Junjun; Ye, Jiaping; Ye, Jianshan

2018-04-18

In this work, we report a facile and green strategy for one pot and in-situ synthesis of a dandelion-like conductive polyaniline coated gold nanoparticle nanocomposites (Au@PANI). The Au@PANI was characterized by SEM, TEM, XRD, TGA, FTIR, UV-vis and conductivity measurement, respectively. Newly-designed Au@PANI materials possessed a significantly high conductivity and strong adsorption capability. Thus, the Au@PANI modified glassy carbon electrode (GCE) was utilized for construct a novel electrochemical sensor for the simultaneous assay of Pb 2+ and Cu 2+ using square wave anodic stripping voltammetry (SWASV). Under the optimized conditions, an excellent electrochemical response in the simultaneous of Pb 2+ and Cu 2+ with detection limit of 0.003 and 0.008 μM (S/N = 3), respectively. Moreover, the prepared sensors realized an excellent reproducibility, repeatability and long term stability, as well as reliable practical assays in real water samples. Besides, the possible formation mechanism and sensing mechanism of Au@PANI nanocomposites have been discussed in detail. We believe this study provides a novel method of fabrication of noble metal nanoparticles decorated conducting polymer materials for the electrochemical sensing applications. Copyright © 2018 Elsevier Inc. All rights reserved.

Electrochemical detection of nitromethane vapors combined with a solubilization device.

PubMed

Delile, Sébastien; Aussage, Adeline; Maillou, Thierry; Palmas, Pascal; Lair, Virginie; Cassir, Michel

2015-01-01

During the past decade, the number of terrorism acts has increased and the need for efficient explosive detectors has become an urgent worldwide necessity. A prototype, Nebulex™, was recently developed in our laboratory. Basically, it couples the solubilization of an analyte from the atmosphere by a nebulization process and in-situ detection. This article presents the development and integration of an electrochemical sensor for the detection of nitromethane, a common chemical product that can be used to make an improvised explosive device. A gold screen-printed electrode was used in a flow-cell and a detection limit of 4.5 µM was achieved by square wave voltammetry. The detection method was also determined to be selective toward nitromethane over a large panel of interfering compounds. Detection tests with the Nebulex™ were thus carried out using a custom-made calibrated nitromethane vapor generator. Detection times of less than one minute were obtained for nitromethane contents of 8 and 90 ppmv. Further measurements were performed in a room-measurement configuration leading to detection times in the range of 1-2 min, clearly demonstrating the system's efficiency under quasi-real conditions. Copyright © 2014 Elsevier B.V. All rights reserved.

Flexible nanopillar-based electrochemical sensors for genetic detection of foodborne pathogens

NASA Astrophysics Data System (ADS)

Park, Yoo Min; Lim, Sun Young; Jeong, Soon Woo; Song, Younseong; Bae, Nam Ho; Hong, Seok Bok; Choi, Bong Gill; Lee, Seok Jae; Lee, Kyoung G.

2018-06-01

Flexible and highly ordered nanopillar arrayed electrodes have brought great interest for many electrochemical applications, especially to the biosensors, because of its unique mechanical and topological properties. Herein, we report an advanced method to fabricate highly ordered nanopillar electrodes produced by soft-/photo-lithography and metal evaporation. The highly ordered nanopillar array exhibited the superior electrochemical and mechanical properties in regard with the wide space to response with electrolytes, enabling the sensitive analysis. As-prepared gold and silver electrodes on nanopillar arrays exhibit great and stable electrochemical performance to detect the amplified gene from foodborne pathogen of Escherichia coli O157:H7. Additionally, lightweight, flexible, and USB-connectable nanopillar-based electrochemical sensor platform improves the connectivity, portability, and sensitivity. Moreover, we successfully confirm the performance of genetic analysis using real food, specially designed intercalator, and amplified gene from foodborne pathogens with high reproducibility (6% standard deviation) and sensitivity (10 × 1.01 CFU) within 25 s based on the square wave voltammetry principle. This study confirmed excellent mechanical and chemical characteristics of nanopillar electrodes have a great and considerable electrochemical activity to apply as genetic biosensor platform in the fields of point-of-care testing (POCT).

Construction of novel sensitive electrochemical sensor for electro-oxidation and determination of citalopram based on zinc oxide nanoparticles and multi-walled carbon nanotubes.

PubMed

Ghaedi, Hamed; Afkhami, Abbas; Madrakian, Tayyebeh; Soltani-Felehgari, Farzaneh

2016-02-01

A new chemically modified carbon paste electrode (CMCPE) was applied to the simple, rapid, highly selective and sensitive determination of citalopram in human serum and pharmaceutical preparations using adsorptive square wave voltammetry (ASWV). The ZnO nanoparticles and multi-walled carbon nanotubes modified CPE (ZnO-MWCNT/CPE) electrode was prepared by incorporation of the ZnO nanoparticles and multi-walled carbon nanotubes (MWCNT) in carbon paste electrode. The limit of detection and the linear range were found to be 0.005 and 0.012 to 1.54μmolL(-1) of citalopram, respectively. The effects of potentially interfering substances on the determination of this compound were investigated and found that the electrode is highly selective. The proposed CMCPE was used to the determination of citalopram in human serum, urine and pharmaceutical samples. This reveals that ZnO-MWCNT/CPE shows excellent analytical performance for the determination of citalopram in terms of very low detection limit, high sensitivity, very good repeatability and reproducibility over other methods reported in the literature. Copyright © 2015. Published by Elsevier B.V.

New porphyrin-polyoxometalate hybrid materials: synthesis, characterization and investigation of catalytic activity in acetylation reactions.

PubMed

Araghi, Mehdi; Mirkhani, Valiollah; Moghadam, Majid; Tangestaninejad, Shahram; Mohammdpoor-Baltork, Iraj

2012-10-14

New hybrid complexes based on covalent interaction between 5,10,15,20-tetrakis(4-aminophenyl)porphyrinatozinc(II) and 5,10,15,20-tetrakis(4-aminophenyl)porphyrinatotin(IV) chloride, and a Lindqvist-type polyoxometalate, Mo(6)O(19)(2-), were prepared. These new porphyrin-polyoxometalate hybrid materials were characterized by (1)H NMR, FT IR and UV-Vis spectroscopic methods and cyclic voltammetry. These spectro- and electrochemical studies provided several spectral data for synthesis of these compounds. Cyclic voltammetry showed the influence of the polyoxometalate on the redox process of the porphyrin ring. The catalytic activity of tin(IV)porphyrin-hexamolybdate hybrid material was investigated in the acetylation of alcohols and phenols with acetic anhydride. The reusability of this catalyst was also investigated.

Approach for discrimination and quantification of electroactive species: kinetics difference revealed by higher harmonics of Fourier transformed sinusoidal voltammetry.

PubMed

Fang, Yishan; Huang, Xinjian; Wang, Lishi

2015-01-06

Discrimination and quantification of electroactive species are traditionally realized by a potential difference which is mainly determined by thermodynamics. However, the resolution of this approach is limited to tens of millivolts. In this paper, we described an application of Fourier transformed sinusoidal voltammetry (FT-SV) that provides a new approach for discrimination and quantitative evaluation of electroactive species, especially thermodynamic similar ones. Numerical simulation indicates that electron transfer kinetics difference between electroactive species can be revealed by the phase angle of higher order harmonics of FT-SV, and the difference can be amplified order by order. Thus, even a very subtle kinetics difference can be amplified to be distinguishable at a certain order of harmonics. This method was verified with structurally similar ferrocene derivatives which were chosen as the model systems. Although these molecules have very close redox potential (<10 mV), discrimination and selective detection were achieved by as high as the thirteenth harmonics. The results demonstrated the feasibility and reliability of the method. It was also implied that the combination of the traditional thermodynamic method and this kinetics method can form a two-dimension resolved detection method, and it has the potential to extend the resolution of voltammetric techniques to a new level.

The theory of cyclic voltammetry of electrochemically heterogeneous surfaces: comparison of different models for surface geometry and applications to highly ordered pyrolytic graphite.

PubMed

Ward, Kristopher R; Lawrence, Nathan S; Hartshorne, R Seth; Compton, Richard G

2012-05-28

The cyclic voltammetry at electrodes composed of multiple electroactive materials, where zones of one highly active material are distributed over a substrate of a second, less active material, is investigated by simulation. The two materials are assumed to differ in terms of their electrochemical rate constants towards any given redox couple. For a one-electron oxidation or reduction, the effect on voltammetry of the size and relative surface coverages of the zones as well as the rate constant of the slower zone are considered for systems where it is much slower than the rate constant of the faster zones. The occurrence of split peak cyclic voltammetry where two peaks are observed in the forward sweep, is studied in terms of the diffusional effects present in the system. A number of surface geometries are compared: specifically the more active zones are modelled as long, thin bands, as steps in the surface, as discs, and as rings (similar to a partially blocked electrode). Similar voltammetry for the band, step and ring models is seen but the disc geometry shows significant differences. Finally, the simulation technique is applied to the modelling of highly-ordered pyrolytic graphite (HOPG) surface and experimental conditions under which it may be possible to observe split peak voltammetry are predicted.

Nanoparticle-based immunosensor with apoferritin templated metallic phosphate label for quantification of phosphorylated acetylcholinesterase

DOE Office of Scientific and Technical Information (OSTI.GOV)

Du, Dan; Chen, Aiqiong; Xie, Yunying

2011-05-15

A new sandwich-like electrochemical immunosensor has been developed for quantification of organophosphorylated acetylcholinesterase (OP-AChE), an exposure biomarker of organophosphate pesticides and nerve agents. Zirconia nanoparticles (ZrO2 NPs) were anchored on a screen printed electrode (SPE) to preferably capture OP-AChE adducts by metal chelation with phospho-moieties, which was selectively recognized by lead phosphate-apoferritin labeled anti-AChE antibody (LPA-anti-AChE). The sandwich-like immunoreactions were performed among ZrO2 NPs, OP-AChE and LPA-anti-AChE to form ZrO2/OP-AChE/LPA-anti-AChE complex and the released lead ions were detected on a disposable SPE. The binding affinity was investigated by both square wave voltammetry (SWV) and quartz crystal microbalance (QCM) measurements. Themore » proposed immunosensor yielded a linear response current over a broad OP-AChE concentrations range from 0.05 nM to 10 nM, with detection limit of 0.02 nM, which has enough sensitivity for monitoring of low-dose exposure to OPs. This method avoids the drawback of unavailability of commercial OP-specific antibody as well as amplifies detection signal by using apoferritin encoded metallic phosphate nanoparticle tags. This nanoparticle-based immunosensor offers a new method for rapid, sensitive, selective and inexpensive quantification of phosphorylated adducts for monitoring of OP pesticides and nerve agents exposures.« less

Designing of fluorescent and magnetic imprinted polymer for rapid, selective and sensitive detection of imidacloprid via activators regenerated by the electron transfer-atom transfer radical polymerization (ARGET-ATRP) technique

NASA Astrophysics Data System (ADS)

Kumar, Sunil; Karfa, Paramita; Madhuri, Rashmi; Sharma, Prashant K.

2018-05-01

In this work, we report on a dual-behavior electrochemical/optical sensor for sensitive determination of Imidacloprid by fluorescent dye (fluorescein, FL) and imprinted polymer modified europium doped superparamagnetic iron oxide nanoparticles (FL@SPIONs@MIP). The imidacloprid (IMD)-imprinted polymer was directly synthesized on the Eu-SPIONs surface via Activators regenerated by the electron transfer-atom transfer radical polymerization (ARGET-ATRP) technique. Preparation, characterization and application of the prepared FL@SPIONs@MIP were systematically investigated using scanning electron microscopy (SEM), X-ray diffraction (XRD), vibrating sample magnetometer (VSM), fluorescence spectroscopy and electrochemical techniques. The electrochemical experiments exhibited a remarkable selectivity of the prepared sensor towards IMD. Determination of IMD by the square wave stripping voltammetry method represented a wide linear range of 0.059-0.791 μg L-1 with a detection limit of 0.0125 μg L-1. In addition, the fluorescence method shows a linear range of 0.039-0.942 μg L-1 and LOD of 0.0108 μg L-1. The fluorescence property of prepared FL@SPIONs@MIP was used for rapid, on-spot but selective detection of IMD in real samples. The proposed electrode displayed excellent repeatability and long-term stability and was successfully applied for quantitative and trace level determination of IMD in several real samples.

Demon voltammetry and analysis software: Analysis of cocaine-induced alterations in dopamine signaling using multiple kinetic measures

PubMed Central

Yorgason, Jordan T.; España, Rodrigo A.; Jones, Sara R.

2011-01-01

The fast sampling rates of fast scan cyclic voltammetry make it a favorable method for measuring changes in brain monoamine release and uptake kinetics in slice, anesthetized, and freely moving preparations. The most common analysis technique for evaluating changes in dopamine signaling uses well-established Michaelis-Menten kinetic methods that can accurately model dopamine release and uptake parameters across multiple experimental conditions. Nevertheless, over the years, many researchers have turned to other measures to estimate changes in dopamine release and uptake, yet to our knowledge no systematic comparison amongst these measures has been conducted. To address this lack of uniformity in kinetic analyses, we have created the Demon Voltammetry and Analysis software suite, which is freely available to academic and non-profit institutions. Here we present an explanation of the Demon Acquisition and Analysis features, and demonstrate its utility for acquiring voltammetric data under in vitro, in vivo anesthetized, and freely moving conditions. Additionally, the software was used to compare the sensitivity of multiple kinetic measures of release and uptake to cocaine-induced changes in electrically evoked dopamine efflux in nucleus accumbens core slices. Specifically, we examined and compared tau, full width at half height, half-life, T20, T80, slope, peak height, calibrated peak dopamine concentration, and area under the curve to the well-characterized Michaelis-Menten parameters, dopamine per pulse, maximal uptake rate, and apparent affinity. Based on observed results we recommend tau for measuring dopamine uptake and calibrated peak dopamine concentration for measuring dopamine release. PMID:21392532

E-tongue 2 REDOX response to heavy metals

NASA Technical Reports Server (NTRS)

Buehler, M. G.; Kuhlman, G. M.; Kounaves, S. P.

2002-01-01

E-Tongue 2 an array of electrochemical sensors including REDOX electrodes for Cylic Voltammetry and Anodic Stripping Voltammetry measurements, Galvanic cells for corrosion measurements, and Ion Selective Electrodes.

Ultrasonic enhancement of battery diffusion.

PubMed

Hilton, R; Dornbusch, D; Branson, K; Tekeei, A; Suppes, G J

2014-03-01

It has been demonstrated that sonic energy can be harnessed to enhance convection in Galvanic cells during cyclic voltammetry; however, the practical value of this approach is limited due to the lack of open volumes for convection patterns to develop in most batteries. This study evaluates the ability of ultrasonic waves to enhance diffusion in membrane separators commonly used in sandwich-architecture batteries. Studies include the measuring of open-circuit performance curves to interpret performances in terms of reductions in concentration overpotentials. The use of a 40 kHz sonicator bath can consistently increase the voltage of the battery and reduce overpotential losses up to 30%. This work demonstrates and quantifies battery enhancement due to enhanced diffusion made possible with ultrasonic energy. Copyright © 2013 Elsevier B.V. All rights reserved.

Electrochemistry of uranium in molten LiF-CaF2

NASA Astrophysics Data System (ADS)

Nourry, C.; Souček, P.; Massot, L.; Malmbeck, R.; Chamelot, P.; Glatz, J.-P.

2012-11-01

This article is focused on the electrochemical behaviour of U ions in molten LiF-CaF2 (79-21 wt.%) eutectic. On a W electrode, U(III) is reduced in one step to U metal and U(III) can be also oxidised to U(IV). Both systems were studied by cyclic and square wave voltammetry. Reversibility of both systems for both techniques was verified and number of exchanged electrons was determined, as well as diffusion coefficients for U(III) and U(IV). The results are in a good agreement with previous studies. On a Ni electrode, the depolarisation effect due to intermetallic compounds formation was observed. Electrorefining of U metal in a melt containing U and Gd ions was carried out using a reactive Ni electrode with promising results.

NiCo2O4/N-doped graphene as an advanced electrocatalyst for oxygen reduction reaction

NASA Astrophysics Data System (ADS)

Zhang, Hui; Li, Huiyong; Wang, Haiyan; He, Kejian; Wang, Shuangyin; Tang, Yougen; Chen, Jiajie

2015-04-01

Developing low-cost catalyst for high-performance oxygen reduction reaction (ORR) is highly desirable. Herein, NiCo2O4/N-doped reduced graphene oxide (NiCo2O4/N-rGO) hybrid is proposed as a high-performance catalyst for ORR for the first time. The well-formed NiCo2O4/N-rGO hybrid is studied by cyclic voltammetry (CV) curves and linear-sweep voltammetry (LSV) performed on the rotating-ring-disk-electrode (RDE) in comparison with N-rGO-free NiCo2O4 and the bare N-rGO. Due to the synergistic effect, the NiCo2O4/N-rGO hybrid exhibits significant improvement of catalytic performance with an onset potential of -0.12 V, which mainly favors a direct four electron pathway in ORR process, close to the behavior of commercial carbon-supported Pt. Also, the benefits of N-incorporation are investigated by comparing NiCo2O4/N-rGO with NiCo2O4/rGO, where higher cathodic currents, much more positive half-wave potential and more electron transfer numbers are observed for the N-doping one, which should be ascribed to the new highly efficient active sites created by N incorporation into graphene. The NiCo2O4/N-rGO hybrid could be used as a promising catalyst for high power metal/air battery.

Finite-element simulations of the influence of pore wall adsorption on cyclic voltammetry of ion transfer across a liquid-liquid interface formed at a micropore.

PubMed

Ellis, Jonathan S; Strutwolf, Jörg; Arrigan, Damien W M

2012-02-21

Adsorption onto the walls of micropores was explored by computational simulations involving cyclic voltammetry of ion transfer across an interface between aqueous and organic phases located at the micropore. Micro-interfaces between two immiscible electrolyte solutions (micro-ITIES) have been of particular research interest in recent years and show promise for biosensor and biomedical applications. The simulation model combines diffusion to and within the micropore, Butler-Volmer kinetics for ion transfer at the liquid-liquid interface, and Langmuir-style adsorption on the pore wall. Effects due to pore radius, adsorption and desorption rates, surface adsorption site density, and scan rates were examined. It was found that the magnitude of the reverse peak current decreased due to adsorption of the transferring ion on the pore wall; this decrease was more marked as the scan rate was increased. There was also a shift in the half-wave potential to lower values following adsorption, consistent with a wall adsorption process which provides a further driving force to transfer ions across the ITIES. Of particular interest was the disappearance of the reverse peak from the cyclic voltammogram at higher scan rates, compared to the increase in the reverse peak size in the absence of wall adsorption. This occurred for scan rates of 50 mV s(-1) and above and may be useful in biosensor applications using micropore-based ITIES.

Influence of electron delocalization in heterocyclic core systems on the electrochemical communication in 2,5-di- and 2,3,4,5-tetraferrocenyl thiophenes, furans, and pyrroles.

PubMed

Hildebrandt, Alexander; Schaarschmidt, Dieter; Claus, Ron; Lang, Heinrich

2011-11-07

A series of 2,5-di- and 2,3,4,5-tetraferrocenyl-substituted thiophenes, furans, and pyrroles were synthesized using the Negishi C,C cross-coupling protocol. The electronic and electrochemical properties of these compounds were investigated by cyclic voltammetry (CV), square wave voltammetry (SWV), and in situ UV-vis/NIR spectroscopy. The molecular structures of 2,5-diferrocenyl furan and 2,3,4,5-tetraferrocenyl-1-methyl-1H-pyrrole in the solid state are discussed. The ferrocenyls could sequentially be oxidized giving two or four reversible responses for the appropriate di- or tetraferrocenyl-substituted heterocyclic molecules. The observed ΔE°' values range between 186 and 450 mV. The NIR measurements confirm electronic communication as intervalence charge transfer (IVCT) absorptions were found in the corresponding mono- and in case of the tetraferrocenyl compounds also in the dicationic species. All compounds, except tetraferrocenyl thiophene (a class I system), were classified as class II systems according to Robin and Day. They show a linear relationship between ΔE°' and the IVCT oscillator strength f which could be shown for the first time in organometallic chemistry. This was possible because the series of molecules exhibit analogous geometries and hence, similar electrostatic properties. This correlation was confirmed by electro- and spectro-electrochemical measurements. Within these studies a new approach for the estimation of the effective electron transfer distances r(ab) is discussed. © 2011 American Chemical Society

Determination of carmine food dye (E120) in foodstuffs by stripping voltammetry.

PubMed

Alghamdi, Ahmad H; Alshammery, Hamed M; Abdalla, Mohamed A; Alghamdi, Ali F

2009-01-01

The behavior of the food colorant agent carmine (E120) was studied by square-wave adsorptive stripping voltammetry (SW-AdSV) at the hanging mercury drop electrode. It was observed that carmine gave a sensitive stripping voltammetric peak at -350 mV in pH 3 acetate buffer. The cyclic voltammetric technique was also used to characterize the electrochemical reduction process of carmine. The adsorptive voltammetric signal was evaluated with respect to various experimental conditions, and the optimized values were supporting electrolyte, acetate buffer; buffer acidity, pH 3; dye concentration, 3 x 10(-7) M; accumulation time, 150 s; accumulation potential, -0.2 V; scan rate, 300 mV/s; pulse amplitude, 185 mV; SW frequency, 20 Hz; working electrode area, 0.6 mm2; and convection rate, 2600 rpm. The SW-AdSV peak currents depended linearly on the concentration of carmine from 5 x 10(-8) to 1.25 x 10(-7) mol/L (r = 0.99). A detection limit of 1.43 x 10(-9) mol/L with an RSD of 2.2% and a mean recovery of 97.9% were obtained. Possible interferences by several substances usually present in food products such as food additive dyes (E102, E100, E123, E127, and E129), artificial sweeteners, preservatives, and antioxidants were also evaluated. The proposed electrochemical procedure was successfully applied to the determination of carmine food dye in spiked commercially available ice cream and soft drinks.

Gold leaf counter electrodes for dye-sensitized solar cells

NASA Astrophysics Data System (ADS)

Shimada, Kazuhiro; Toyoda, Takeshi

2018-03-01

In this study, a gold leaf 100 nm thin film is used as the counter electrode in dye-sensitized solar cells. The traditional method of hammering gold foil to obtain a thin gold leaf, which requires only small amounts of gold, was employed. The gold leaf was then attached to the substrate using an adhesive to produce the gold electrode. The proposed approach for fabricating counter electrodes is demonstrated to be facile and cost-effective, as opposed to existing techniques. Compared with electrodes prepared with gold foil and sputtered gold, the gold leaf counter electrode demonstrates higher catalytic activity with a cobalt-complex electrolyte and higher cell efficiency. The origin of the improved performance was investigated by surface morphology examination (scanning electron microscopy), various electrochemical analyses (cyclic voltammetry, linear sweep voltammetry, and electrochemical impedance spectroscopy), and crystalline analysis (X-ray diffractometry).

Application of graphene-ionic liquid-chitosan composite-modified carbon molecular wire electrode for the sensitive determination of adenosine-5'-monophosphate.

PubMed

Shi, Fan; Gong, Shixing; Xu, Li; Zhu, Huanhuan; Sun, Zhenfan; Sun, Wei

2013-12-01

In this paper, a graphene (GR) ionic liquid (IL) 1-octyl-3-methylimidazolium hexafluorophosphate and chitosan composite-modified carbon molecular wire electrode (CMWE) was fabricated by a drop-casting method and further applied to the sensitive electrochemical detection of adenosine-5'-monophosphate (AMP). CMWE was prepared with diphenylacetylene (DPA) as the modifier and the binder. The properties of modified electrode were examined by scanning electron microscopy, cyclic voltammetry and electrochemical impedance spectroscopy. Electrochemical behaviors of AMP was carefully investigated with enhanced responses appeared, which was due to the presence of GR-IL composite on the electrode surface with excellent electrocatalytic ability. A well-defined oxidation peak of AMP appeared at 1.314 V and the electrochemical parameters were calculated by electrochemical methods. Under the selected conditions, the oxidation peak current of AMP was proportional to its concentration in the range from 0.01 μM to 80.0 μM with the detection limit as 3.42 nM (3σ) by differential pulse voltammetry. The proposed method exhibited good selectivity and was applied to the detection of vidarabine monophosphate injection samples with satisfactory results. © 2013.

Conductive polymer/reduced graphene oxide/Au nano particles as efficient composite materials in electrochemical supercapacitors

NASA Astrophysics Data System (ADS)

Shabani Shayeh, J.; Ehsani, A.; Ganjali, M. R.; Norouzi, P.; Jaleh, B.

2015-10-01

Polyaniline/reduced graphene oxide/Au nano particles (PANI/rGO/AuNPs) as a hybrid supercapacitor were deposited on a glassy carbon electrode (GCE) by cyclic voltammetry (CV) method as ternary composites and their electrochemical performance was evaluated in acidic medium. Scanning electron micrographs clearly revealed the formation of nanocomposites on the surface of the working electrode. Scanning electron micrographs (SEM) clearly revealed the formation of nanocomposites on the surface of working electrode. Different electrochemical methods including galvanostatic charge-discharge (CD) experiments, cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) were carried out in order to investigate the applicability of the system as a supercapacitor. Based on the cyclic voltammogram results obtained, PANI/rGO/AuNPs gave higher specific capacitance, power and energy values than PANI at a current density of 1 mA cm-2. Specific capacitance (SC) of PANI and PANI/rGO/AuNPs electrodes calculated using CV method are 190 and 303 F g-1, respectively. The present study introduces new nanocomposite materials for electrochemical redox capacitors with advantages including long life cycle and stability due to synergistic effects of each component.

Highly sensitive determination of sunset yellow FCF (E110) in food products based on Chitosan/Nanoparticles/MWCNTs with modified gold electrode

NASA Astrophysics Data System (ADS)

Rovina, K.; Siddiquee, S.; Shaarani, S. M.

2016-06-01

Sunset Yellow belongs to the family of azo dyes, commonly used in food industry. High consumption of Sunset Yellow can cause health problem to human. Due to arising of the health issues, there are several analytical methods available for determination of Sunset Yellow. However, these methods are required skilled manpower, complicated procedures, time consuming and high cost. Herein, an electrochemical sensor was developed based on the combination of chitosan (CHIT), calcium oxide nanoparticles (CaONPs) and multiwall carbon nanotubes (MWCNTs) sensing film for detection of Sunset Yellow in food products. Electrochemical behavior of the modified gold electrode in the presence of Sunset Yellow was studied by using cyclic voltammetry (CV) and differential pulse voltammetry (DPV). The morphological characteristics of CHIT/CaONPs/MWCNTs were observed under scanning electron microscope and transmission electron microscope. Under optimal conditions, the DPV was detected with different concentrations of Sunset Yellow in the range of 0.9 to 10 ppm, with detection limit of 0.8 ppm. The developed method has successfully applied for monitoring the presence of Sunset Yellow with different food products including candy, royal jelly, ice cream and soft drink with satisfactory results.

Development of electrochemical folic acid sensor based on hydroxyapatite nanoparticles

NASA Astrophysics Data System (ADS)

Kanchana, P.; Sekar, C.

2015-02-01

We report the synthesis of hydroxyapatite (HA) nanoparticles (NPs) by a simple microwave irradiation method and its application as sensing element for the precise determination of folic acid (FA) by electrochemical method. The structure and composition of the HA NPs characterized using XRD, FTIR, Raman and XPS. SEM and EDX studies confirmed the formation of elongated spherical shaped HA NPs with an average particle size of about 34 nm. The HA NPs thin film on glassy carbon electrode (GCE) were deposited by drop casting method. Electrocatalytic behavior of FA in the physiological pH 7.0 was investigated by cyclic voltammetry (CV), linear sweep voltammetry (LSV) and chronoamperometry. The fabricated HA/GCE exhibited a linear calibration plot over a wide FA concentration ranging from 1.0 × 10-7 to 3.5 × 10-4 M with the detection limit of 75 nM. In addition, the HA NPs modified GCE showed good selectivity toward the determination of FA even in the presence of a 100-fold excess of ascorbic acid (AA) and 1000-fold excess of other common interferents. The fabricated biosensor exhibits good sensitivity and stability, and was successfully applied for the determination of FA in pharmaceutical samples.

One-Step Fabrication of a Multifunctional Magnetic Nickel Ferrite/Multi-walled Carbon Nanotubes Nanohybrid-Modified Electrode for the Determination of Benomyl in Food.

PubMed

Wang, Qiong; Yang, Jichun; Dong, Yuanyuan; Zhang, Lei

2015-05-20

Benomyl, as one kind of agricultural pesticide, has adverse impact on human health and the environment. It is urgent to develop effective and rapid methods for quantitative determination of benomyl. A simple and sensitive electroanalytical method for determination of benomyl using a magnetic nickel ferrite (NiFe2O4)/multi-walled carbon nanotubes (MWCNTs) nanohybrid-modified glassy carbon electrode (GCE) was presented. The electrocatalytic properties and electroanalysis of benomyl on the modified electrode were investigated by cyclic voltammetry (CV) and differential pulse voltammetry (DPV). In the phosphate-buffered saline (PBS) of pH 6.0, this constructed biosensor exhibited two linear relationships with the benomyl concentration range from 1.00 × 10(-7) to 5.00 × 10(-7) mol/L and from 5.00 × 10(-7) to 1.00 × 10(-5) mol/L, respectively. The detection limit was 2.51 × 10(-8) mol/L (S/N = 3). Moreover, the proposed method was successfully applied to determine benomyl in real samples with satisfactory results. The NiFe2O4/MWCNTs/GCE showed good reproducibility and stability, excellent catalytic activity, and anti-interference.

Continuous fast Fourier transforms cyclic voltammetry as a new approach for investigation of skim milk k-casein proteolysis, a comparative study.

PubMed

Shayeh, Javad Shabani; Sefidbakht, Yahya; Siadat, Seyed Omid Ranaei; Niknam, Kaveh

2017-10-01

Cheese production is relied upon the action of Rennet on the casein micelles of milk. Chymosin assay methods are usually time consuming and offline. Herein, we report a new electrochemical technique for studying the proteolysis of K-casein. The interaction of rennet and its substrate was studied by fast Fourier transform continuous cyclic voltammetry (FFTCCV) based on a determination of k-casein in aqueous solution. FFTCCV technique is a very useful method for studying the enzymatic procedures. Fast response, no need of modified electrodes or complex equipment is some of FFTCCV advantages. Various concentrations of enzyme and substrate were selected and the increase in the appearance of charged species in solution as a result of the addition of rennet was studied. Data obtained using FFTCCV technique were also confirmed by turbidity analysis. The results show that rennet proteolysis activity occurs in much shorter time scales compare with its aggregation. Hence, following the appearance of charged segments as a result of proteolysis could be under consideration as a rapid and online method. Copyright © 2017 Elsevier B.V. All rights reserved.

Differential thermal voltammetry for tracking of degradation in lithium-ion batteries

NASA Astrophysics Data System (ADS)

Wu, Billy; Yufit, Vladimir; Merla, Yu; Martinez-Botas, Ricardo F.; Brandon, Nigel P.; Offer, Gregory J.

2015-01-01

Monitoring of lithium-ion batteries is of critical importance in electric vehicle applications in order to manage the operational condition of the cells. Measurements on a vehicle often involve current, voltage and temperature which enable in-situ diagnostic techniques. This paper presents a novel diagnostic technique, termed differential thermal voltammetry, which is capable of monitoring the state of the battery using voltage and temperature measurements in galvanostatic operating modes. This tracks battery degradation through phase transitions, and the resulting entropic heat, occurring in the electrodes. Experiments to monitor battery degradation using the new technique are compared with a pseudo-2D cell model. Results show that the differential thermal voltammetry technique provides information comparable to that of slow rate cyclic voltammetry at shorter timescale and with load conditions easier to replicate in a vehicle.

A Simple and Low-Cost Ultramicroelectrode Fabrication and Characterization Method for Undergraduate Students

ERIC Educational Resources Information Center

Sur, Ujjal Kumar; Dhason, A.; Lakshminarayanan, V.

2012-01-01

A laboratory experiment is described in which students fabricate disk-shaped gold and platinum microelectrodes with diameters of 10-50 [mu]m by sealing sodalime glass with metal microwires. The electrodes are characterized by performing cyclic voltammetry in aqueous and acetonitrile solution. Commercial microelectrodes are expensive (cost depends…

Double-Polymer-Modified Pencil Lead for Stripping Voltammetry of Perchlorate in Drinking Water

ERIC Educational Resources Information Center

Izadyar, Anahita; Kim, Yushin; Ward, Michelle M.; Amemiya, Shigeru

2012-01-01

The inexpensive and disposable electrode based on a double-polymer-modified pencil lead is proposed for upper-division undergraduate instrumental laboratories to enable the highly sensitive detection of perchlorate. Students fabricate and utilize their own electrodes in the 3-4 h laboratory session to learn important concepts and methods of…

Glassy carbon electrode modified with carbon black for sensitive estradiol determination by means of voltammetry and flow injection analysis with amperometric detection.

PubMed

Smajdor, Joanna; Piech, Robert; Ławrywianiec, Martyna; Paczosa-Bator, Beata

2018-03-01

A voltammetric method for fast and sensitive estradiol determination using carbon black modified glassy carbon electrode (CBGC) is proposed. The use of carbon black as a modifying layer led to obtain low detection limit (9.2·10 -8  mol L -1 for a preconcentration time of 60 s) and stability of registered signals (measured as RSD is 1.3%, n = 7, estradiol concentration 0.5·10 -6  mol L -1 ). Cyclic voltammetry study revealed that in phosphate media estradiol suffers irreversible one-proton and one-electron oxidation process. Under the optimum conditions, estradiol calibration curve was linear in the concentration range from 0.15·10 -6 to 3.5·10 -6  mol L -1 . The proposed method enable to determine estradiol content in different pharmaceutical formulation with good recovery. Amperometric measurements of estradiol were performed as well to indicate the possibility of its fast and accurate determination under the flow conditions. Copyright © 2017 Elsevier Inc. All rights reserved.

Cyclic Voltammetry Experiment.

ERIC Educational Resources Information Center

Van Benschoten, James J.; And Others

1983-01-01

Describes a three-part experiment designed to introduce cyclic voltammetry to graduate/undergraduate students. Part 1 demonstrates formal reduction potential, redox electron transfer, diffusion coefficient, and electrochemical reversibility. Part 2 investigates electrochemical behavior of acetaminophen. Part 3 examines such experimental variables…

Metal–organic complexation in the marine environment

PubMed Central

Luther, George W; Rozan, Timothy F; Witter, Amy; Lewis, Brent

2001-01-01

We discuss the voltammetric methods that are used to assess metal–organic complexation in seawater. These consist of titration methods using anodic stripping voltammetry (ASV) and cathodic stripping voltammetry competitive ligand experiments (CSV-CLE). These approaches and a kinetic approach using CSV-CLE give similar information on the amount of excess ligand to metal in a sample and the conditional metal ligand stability constant for the excess ligand bound to the metal. CSV-CLE data using different ligands to measure Fe(III) organic complexes are similar. All these methods give conditional stability constants for which the side reaction coefficient for the metal can be corrected but not that for the ligand. Another approach, pseudovoltammetry, provides information on the actual metal–ligand complex(es) in a sample by doing ASV experiments where the deposition potential is varied more negatively in order to destroy the metal–ligand complex. This latter approach gives concentration information on each actual ligand bound to the metal as well as the thermodynamic stability constant of each complex in solution when compared to known metal–ligand complexes. In this case the side reaction coefficients for the metal and ligand are corrected. Thus, this method may not give identical information to the titration methods because the excess ligand in the sample may not be identical to some of the actual ligands binding the metal in the sample. PMID:16759421

A simple ultrasensitive electrochemical sensor for simultaneous determination of gallic acid and uric acid in human urine and fruit juices based on zirconia-choline chloride-gold nanoparticles-modified carbon paste electrode.

PubMed

Shahamirifard, Seyed Alireza; Ghaedi, Mehrorang; Razmi, Zahra; Hajati, Shaaker

2018-08-30

The determination of gallic acid (GA) and uric acid (UA) is essential due to their biological properties. Numerous methods have been reported for the analysis of GA and UA in various real samples. However, the development of a simple, rapid and practical sensor still remains a great challenge. Here, a carbon paste electrode (CPE) was modified by nanocomposite containing zirconia nanoparticles (ZrO 2 NPs), Choline chloride (ChCl) and gold nanoparticles (AuNPs) to construct ZrO 2 -ChCl-AuNPs/CPE as electrochemical sensor for the simultaneous electro-oxidation of GA and UA. Characterization was performed by Fourier transform infrared spectroscopy, X-ray diffraction, field emission scanning electron microscopy and energy dispersive X-ray spectroscopy. The modified electrode was investigated by different methods including electrochemical impedance spectroscopy and cyclic voltammetry. Kinetic parameters such as charge transfer coefficient, standard heterogeneous electron transfer rate constant and other parameters were calculated via voltammetry techniques. Differential pulse voltammetry was used for simultaneous determination of GA and UA applying the ZrO 2 -ChCl-AuNPs/CPE electrode. At the optimum conditions, this sensor showed a linear response in the ranges 0.22- 55 and 0.12-55 µM for GA and UA, respectively. In addition, low detection limits of 25 and 15 nM were obtained for GA and UA, respectively. Furthermore, ZrO 2 -ChCl-AuNPs/CPE was successfully applied for the independent determination of GA in green tea and fruit juice as well as the simultaneous determination of GA and UA in human urine samples. Copyright © 2018 Elsevier B.V. All rights reserved.

Detection of cephradine through the electrochemical study of the degradation product of cephradine

NASA Astrophysics Data System (ADS)

Jiang, Qingfeng; Ying, Yibin; Wang, Jianping; Ye, Zunzhong; Li, Yanbin

2005-11-01

The degradation product of cephradine(CEP), a broad spectrum antibiotic, with NaOH was studied in solution by Cyclic Voltammetry and Differential Pulse Voltammetry at a three electrode system (Gold working electrode, Hg/HgCl reference electrode and Platinum counter electrode). Our experiment was based on that the R-SH in degradation product could cause a deoxidization peak at gold working electrode. The response was optimized with respect to accumulation time, ionic strength, drug concentration, reproducibility and other variables. We found that the degradation product of CEP in Na2HPO4-NaH2PO4 buffer could cause a sensitive deoxidization peak at -0.68V. A linear dependence of peak currents on the concentration was observed in the range of 10-7 - 10-6 mol/L, with a detection limit of 0.5*10-7mol/L. This method can achieve satisfactory results in the application of detecting human-made CEP.

Graphene-multiwall carbon nanotube-gold nanocluster composites modified electrode for the simultaneous determination of ascorbic acid, dopamine, and uric acid.

PubMed

Liu, Xiaofang; Wei, Shaping; Chen, Shihong; Yuan, Dehua; Zhang, Wen

2014-08-01

In this paper, graphene-multiwall carbon nanotube-gold nanocluster (GP-MWCNT-AuNC) composites were synthesized and used as modifier to fabricate a sensor for simultaneous detection of ascorbic acid (AA), dopamine (DA), and uric acid (UA). The electrochemical behavior of the sensor was investigated by electrochemical impedance spectroscopy (EIS), cyclic voltammetry (CV) and differential pulse voltammetry (DPV) techniques. The combination of GP, MWCNTs, and AuNCs endowed the electrode with a large surface area, good catalytic activity, and high selectivity and sensitivity. The linear response range for simultaneous detection of AA, DA, and UA at the sensor were 120-1,701, 2-213, and 0.7-88.3 μM, correspondingly, and the detection limits were 40, 0.67, and 0.23 μM (S/N=3), respectively. The proposed method offers a promise for simple, rapid, selective, and cost-effective analysis of small biomolecules.

Detection of platinum species in plant material.

PubMed

Messerschmidt, J; Alt, F; Tölg, G

1995-05-01

Model experiments for the detection of platinum species in extracts from native and platinum-treated grass cultivations are described. The procedural steps are cultivation of the grass samples, extraction and concentration of the platinum species by ultrafiltration and freeze-drying, preparative separation of the species by gel chromatography followed by isotachophoresis, and sequential analytical detection of the separated platinum species by adsorptive voltammetry. After isotachophoresis, sharp peaks of platinum species could be detected. In the native grass extract only one platinum species (160-200 kDa) was found. In the platinum-treated grass extracts several platinum species were observed in the molecular mass range from 1 to > 1000 kDa. By an extremely sensitive platinum determination method (adsorptive voltammetry; detection limit, 2 pg Pt abs.) it was possible to detect platinum even in stained protein bands from horizontal gel electrophoresis of platinum containing fractions obtained after isotachophoresis.

Kinetic determinations of accurate relative oxidation potentials of amines with reactive radical cations.

PubMed

Gould, Ian R; Wosinska, Zofia M; Farid, Samir

2006-01-01

Accurate oxidation potentials for organic compounds are critical for the evaluation of thermodynamic and kinetic properties of their radical cations. Except when using a specialized apparatus, electrochemical oxidation of molecules with reactive radical cations is usually an irreversible process, providing peak potentials, E(p), rather than thermodynamically meaningful oxidation potentials, E(ox). In a previous study on amines with radical cations that underwent rapid decarboxylation, we estimated E(ox) by correcting the E(p) from cyclic voltammetry with rate constants for decarboxylation obtained using laser flash photolysis. Here we use redox equilibration experiments to determine accurate relative oxidation potentials for the same amines. We also describe an extension of these experiments to show how relative oxidation potentials can be obtained in the absence of equilibrium, from a complete kinetic analysis of the reversible redox kinetics. The results provide support for the previous cyclic voltammetry/laser flash photolysis method for determining oxidation potentials.

The Study on the Performance of Carbon Supported PtSnM (M = W, Pd, and Ni) Ternary Electro-Catalysts for Ethanol Electro-Oxidation Reaction.

PubMed

Noh, Chang Soo; Heo, Dong Hyun; Lee, Ki Rak; Jeon, Min Ku; Sohn, Jung Min

2016-05-01

PtSn/C and Pt5Sn4M/C (M = W, Pd, Ni) electrocatalysts were prepared by impregnation method using NaBH4 as a reducing agent. Chemical composition, crystalline size, and alloy formation were determined by EDX, XRD and TEM. The average particle sizes of the synthesized catalysts were approximately 3.64-4.95 nm. The electro-chemical properties were measured by CO stripping, cyclic voltammetry, linear sweep voltammetry, and chronoamperometry. The maximum specific activity of the electro-catalysts for ethanol electro-oxidation was 406.08 mA m(-2) in Pt5Sn4Pd/C. The poisoning rate of the Pt5Sn4Pd/C (0.0017% s(-1)) was 4.5 times lower than that of the PtSn/C (0.0076% s(-1)).

Application of catalytic adsorptive stripping voltammetry of the cobalt-alpha-benzil dioxime complex to analysis of cobalt traces in metallic zinc.

PubMed

Bobrowski, A

1994-05-01

The catalytic adsorptive stripping voltammetric method with alpha-benzil dioxime and nitrite affords numerous advantages in cobalt determination. The detailed conditions of the determination of the cobalt traces in metallic zinc by catalytic adsorptive stripping voltammetry have been investigated. Both the linear sweep and the differential pulse stripping modes can be used with similar sensitivity. Possible interferences by Mn, Pb, Cu, Ni and Fe are evaluated. In the presence of 5 x 10(5) fold excess of Zn the linear dependence of the cobalt CASV peak current on concentration ranged from 0.05 mug/l to 3 mug/l. Optimal conditions include the accumulation potential of -0.65 V and the accumulation time of 10 sec. The results of the determination of 10(-5)% level of Co in the metallic zinc showed good reproducibility (relative standard deviation, RSD = 0.07) and reliability.

The (2 × 2) tunnels structured manganese dioxide nanorods with α phase for lithium air batteries

NASA Astrophysics Data System (ADS)

Ghouri, Zafar Khan; Zahoor, Awan; Barakat, Nasser A. M.; Alsoufi, Mohammad S.; Bawazeer, Tahani M.; Mohamed, Ahmed F.; Kim, Hak Yong

2016-02-01

The (2 × 2) tunnels structured manganese dioxide nanorods with α phase (α-MnO2) are synthesized via simplistic hydrothermal method at low temperature. The obtained tunnels structured α-MnO2 nanorods are characterized by, Transmission electron microscopy, Scanning electron microscopy, and X-ray diffraction techniques. The oxygen reduction reaction (ORR) activity was studied by cyclic voltammetry and rotating ring-disc electrode voltammetry techniques in alkaline media. Moreover; the highly electrocatalytic tunnels structured α-MnO2 nanorods were then also applied as cathode in rechargeable Li-O2 cells. The Li-O2 cells exhibited initial discharge capacity as high as ∼4000 mAh/g with the tunnels structured α-MnO2 nanorods which was double the original capacity of the cells without any catalyst. Also we obtained 100% round trip efficiency upon cycling with limited capacity for more than 50 cycles.

Mechanism-Based Condition Screening for Sustainable Catalysis in Single-Electron Steps by Cyclic Voltammetry.

PubMed

Liedtke, Theresa; Spannring, Peter; Riccardi, Ludovico; Gansäuer, Andreas

2018-04-23

A cyclic-voltammetry-based screening method for Cp 2 TiX-catalyzed reactions is introduced. Our mechanism-based approach enables the study of the influence of various additives on the electrochemically generated active catalyst Cp 2 TiX, which is in equilibrium with catalytically inactive [Cp 2 TiX 2 ] - . Thioureas and ureas are most efficient in the generation of Cp 2 TiX in THF. Knowing the precise position of the equilibrium between Cp 2 TiX and [Cp 2 TiX 2 ] - allowed us to identify reaction conditions for the bulk electrolysis of Cp 2 TiX 2 complexes and for Cp 2 TiX-catayzed radical arylations without having to carry out the reactions. Our time- and resource-efficient approach is of general interest for the design of catalytic reactions that proceed in single-electron steps. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Chemometric study of Maya Blue from the voltammetry of microparticles approach.

PubMed

Doménech, Antonio; Doménech-Carbó, María Teresa; de Agredos Pascual, María Luisa Vazquez

2007-04-01

The use of the voltammetry of microparticles at paraffin-impregnated graphite electrodes allows for the characterization of different types of Maya Blue (MB) used in wall paintings from different archaeological sites of Campeche and YucatAn (Mexico). Using voltammetric signals for electron-transfer processes involving palygorskite-associated indigo and quinone functionalities generated by scratching the graphite surface, voltammograms provide information on the composition and texture of MB samples. Application of hierarchical cluster analysis and other chemometric methods allows us to characterize samples from different archaeological sites and to distinguish between samples proceeding from different chronological periods. Comparison between microscopic, spectroscopic, and electrochemical examination of genuine MB samples and synthetic specimens indicated that the preparation procedure of the pigment evolved in time via successive steps anticipating modern synthetic procedures, namely, hybrid organic-inorganic synthesis, temperature control of chemical reactivity, and template-like synthesis.

Study binding of Al-curcumin complex to ds-DNA, monitoring by multispectroscopic and voltammetric techniques

NASA Astrophysics Data System (ADS)

Ahmadi, F.; Alizadeh, A. A.; Shahabadi, N.; Rahimi-Nasrabadi, M.

2011-09-01

In this work a complex of Al 3+ with curcumin ([Al(curcumin) (EtOH) 2](NO 3) 2) was synthesized and characterized by UV-vis, FT-IR, elemental analysis and spectrophotometric titration techniques. The mole ratio plot revealed a 1:1 complex between Al 3+ and curcumin in solution. For binding studies of this complex to calf thymus-DNA various methods such as: UV-vis, fluorescence, circular dichroism (CD), FT-IR spectroscopy and cyclic voltammetry were used. The intrinsic binding constant of ACC with DNA at 25 °C was calculated by UV-vis and cyclic voltammetry as 2.1 × 10 4 and 2.6 × 10 4, respectively. The thermodynamic studies showed that the reaction is enthalpy and entropy favored. The CD results showed that only the Δ-ACC interacts with DNA and the Δ-ACC form has not any tendency to interact with DNA, also the pure curcumin has not any stereoselective interaction with CT-DNA. Fluorimetric studies showed that fluorescence enhancement was initiated by a static process in the ground state. The cyclic voltammetry showed that ACC interact with DNA with a binding site size of 2. From the FT-IR we concluded that the Δ-ACC interacts with DNA via partial electrostatic and minor groove binding. In comparison with previous works it was concluded that curcumin significantly reduced the affinity of Al 3+ to the DNA.

Enzyme-modified carbon-fiber microelectrode for the quantification of dynamic fluctuations of nonelectroactive analytes using fast-scan cyclic voltammetry.

PubMed

Lugo-Morales, Leyda Z; Loziuk, Philip L; Corder, Amanda K; Toups, J Vincent; Roberts, James G; McCaffrey, Katherine A; Sombers, Leslie A

2013-09-17

Neurotransmission occurs on a millisecond time scale, but conventional methods for monitoring nonelectroactive neurochemicals are limited by slow sampling rates. Despite a significant global market, a sensor capable of measuring the dynamics of rapidly fluctuating, nonelectroactive molecules at a single recording site with high sensitivity, electrochemical selectivity, and a subsecond response time is still lacking. To address this need, we have enabled the real-time detection of dynamic glucose fluctuations in live brain tissue using background-subtracted, fast-scan cyclic voltammetry. The novel microbiosensor consists of a simple carbon fiber surface modified with an electrodeposited chitosan hydrogel encapsulating glucose oxidase. The selectivity afforded by voltammetry enables quantitative and qualitative measurements of enzymatically generated H2O2 without the need for additional strategies to eliminate interfering agents. The microbiosensors possess a sensitivity and limit of detection for glucose of 19.4 ± 0.2 nA mM(-1) and 13.1 ± 0.7 μM, respectively. They are stable, even under deviations from physiological normoxic conditions, and show minimal interference from endogenous electroactive substances. Using this approach, we have quantitatively and selectively monitored pharmacologically evoked glucose fluctuations with unprecedented chemical and spatial resolution. Furthermore, this novel biosensing strategy is widely applicable to the immobilization of any H2O2 producing enzyme, enabling rapid monitoring of many nonelectroactive enzyme substrates.

An analytical model of memristors in plants

PubMed Central

Markin, Vladislav S; Volkov, Alexander G; Chua, Leon

2014-01-01

The memristor, a resistor with memory, was postulated by Chua in 1971 and the first solid-state memristor was built in 2008. Recently, we found memristors in vivo in plants. Here we propose a simple analytical model of 2 types of memristors that can be found within plants. The electrostimulation of plants by bipolar periodic waves induces electrical responses in the Aloe vera and Mimosa pudica with fingerprints of memristors. Memristive properties of the Aloe vera and Mimosa pudica are linked to the properties of voltage gated K+ ion channels. The potassium channel blocker TEACl transform plant memristors to conventional resistors. The analytical model of a memristor with a capacitor connected in parallel exhibits different characteristic behavior at low and high frequency of applied voltage, which is the same as experimental data obtained by cyclic voltammetry in vivo. PMID:25482769

Non-aggregated axially disubstituted silicon phthalocyanines bearing electropolymerizable ligands and their aggregation, electropolymerizaton and thermal properties.

PubMed

Biyiklioglu, Zekeriya; Bas, Huseyin; Alp, Hakan

2015-08-21

A novel series of axially disubstituted silicon(iv) phthalocyanines bearing electropolymerizable ligands were designed and synthesized for the first time. The silicon(iv) phthalocyanines were characterized by various spectroscopic techniques as well as elemental analysis. The aggregation behavior of the SiPcs were examined in different solvents and at different concentrations in chloroform. In all the studied solvents and concentrations, the SiPcs were non-aggregated. The thermal behavior of the silicon(iv) phthalocyanines was also studied. The electropolymerization properties of the silicon(iv) phthalocyanines were investigated by cyclic and square wave voltammetry. This study is the first example of the electropolymerization of axially disubstituted silicon phthalocyanines. The type of axial ligand on the phthalocyanine ring did not show any effect on the absorption and thermal properties but influenced the electropolymerization of the phthalocyanines.

A Cyclic Voltammetry Experiment for the Instrumental Analysis Laboratory.

ERIC Educational Resources Information Center

Baldwin, Richard P.; And Others

1984-01-01

Background information and procedures are provided for experiments that illustrate the nature of cyclic voltammetry and its application in the characterization of organic electrode processes. The experiments also demonstrate the concepts of electrochemical reversibility and diffusion-controlled mass transfer. (JN)

Stripping voltammetry in environmental and food analysis.

PubMed

Brainina, K Z; Malakhova, N A; Stojko, N Y

2000-10-01

The review covers over 230 papers published mostly in the last 5 years. The goal of the review is to attract the attention of researchers and users to stripping voltammetry in particular, its application in environmental monitoring and analysis of foodstuffs. The sensors employed are impregnated graphite, carbon paste, thick film carbon/graphite and thin film metallic electrodes modified in-situ or beforehand. Hanging mercury drop electrodes and mercury coated glassy carbon electrodes are also mentioned. Strip and long-lived sensors for portable instruments and flow through systems are discussed as devices for future development and application of stripping voltammetry.

Electrochemical Sensor for Organophosphate Pesticides and Nerve Agents Using Zirconia Nanoparticles as Selective Sorbents

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liu, Guodong; Lin, Yuehe

2005-09-15

Electrochemical sensor for detection of organophosphate (OP) pesticides and nerve agents using zirconia (ZrO₂) nanoparticles as selective sorbents is presented. Zirconia nanoparticles were electrodynamically deposited onto the polycrystalline gold electrode by cyclic voltammetry. Because of a strong affinity of zirconia to the phosphoric group, nitroaromatic OPs strongly bind to the ZrO₂ nanoparticle surface. The electrochemical characterization and anodic stripping voltammetric performance of bound OPs were evaluated using cyclic voltammetric and square-wave voltammetric (SWV) analysis. SWV was used to monitor the amount of bound OPs and provide simple, fast, and facile quantitative methods for nitroaromatic OP compounds. The sensor surface canmore » be regenerated by successively running SWV scanning. Operational parameters, including the amount of nanoparticles, adsorption time, and the pH of the reaction medium have been optimized. The stripping voltammetric response is highly linear over the 5–200 ng/mL (ppb) methyl parathion range examined (2-min adsorption), with a detection limit of 1 ng/mL (10 min accumulation), and good precision (RSD=5.3 %, n = 10). The promising stripping voltammetric performances open new opportunities for fast, simple, and sensitive analyzing of OPs in environmental and biological samples. These findings can lead to a widespread use of electrochemical sensors to detect OP contaminates.« less

Versatile Redox Chemistry Complicates Antioxidant Capacity Assessment: Flavonoids as Milieu-Dependent Antiand Pro-Oxidants

PubMed Central

Chobot, Vladimir; Kubicova, Lenka; Bachmann, Gert; Hadacek, Franz

2013-01-01

Some antioxidants have been shown to possess additional pro-oxidant effects. Diverse methodologies exist for studying redox properties of synthetic and natural chemicals. The latter are substantial components of our diet. Exploration of their contribution to life-extending or -compromising effects is mandatory. Among reactive oxygen species (ROS), hydroxyl radical (•OH) is the most damaging species. Due to its short half-life, the assay has to contain a specific generation system. Plants synthesize flavonoids, phenolic compounds recognized as counter-agents to coronary heart disease. Their antioxidant activities are affected by their hydroxylation patterns. Moreover, in the plant, they mainly occur as glycosides. We chose three derivatives, quercetin, luteolin, and rutin, in attempts to explore their redox chemistry in contrasting hydrogen peroxide environments. Initial addition of hydrogen peroxide in high concentration or gradual development constituted a main factor affecting their redox chemical properties, especially in case of quercetin. Our study exemplifies that a combination of a chemical assay (deoxyribose degradation) with an electrochemical method (square-wave voltammetry) provides insightful data. The ambiguity of the tested flavonoids to act either as anti- or pro-oxidant may complicate categorization, but probably contributed to their evolution as components of a successful metabolic system that benefits both producer and consumer. PMID:23736691

Electron flow in large metallomacromolecules and electronic switch of nanoparticle stabilization: new click ferrocenyl dentromers that reduce Au(III) to Au nanoparticles.

PubMed

Astruc, Didier; Wang, Qi; Fu, Fangyu; Martinez-Villacorta, Angel M; Moya, Sergio; Salmon, Lionel; Ruiz, Jaime; Hunel, Julien; Vax, Amélie

2018-06-04

Click ferrocenyl-terminal dentromers, a family of arene-cored dendrimers with triple branching (9-Fc, 27-Fc, 81-Fc and 243-Fc) reduce Au(III) to ferricinium dentromer-stabilized Au nanoparticles (AuNPs). Cyclic voltammetry studies in CH2Cl2 show reversible CV waves with some adsorption for the 243-Fc dentromer and a number of redox groups found, 255 ± 25, using the Bard-Anson method, close to the theoretical number of 243. The dentromers reduce aqueous HAuCl4 to water-soluble ferricinium chloride dentromer-stabilized gold nanoparticles (AuNPs) with core sizes between 30 and 47 nm. These triazolylferricinium dentromer-stabilized AuNPs are reduced by cobaltocene to cobalticinium chloride and ferrocene dentromer-weakly stabilized AuNPs together with red shift of the AuNP plasmon. The weakness of the AuNP stabilization is characterized by dentromer extraction with CH2Cl2 along with irreversible AuNP agglomeration for the 9, 27 and 81-ferrocenyl dentromer, only the 243-ferrocenyl dentromer-AuNP withstanding this process. Altogether this demonstrates the electronic switch of the dentromer-mediated AuNP stabilization. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Ultrasensitive electrochemical detection of nucleic acids by template enhanced hybridization followed with rolling circle amplification.

PubMed

Ji, Hanxu; Yan, Feng; Lei, Jianping; Ju, Huangxian

2012-08-21

An ultrasensitive protocol for electrochemical detection of DNA is designed with quantum dots (QDs) as a signal tag by combining the template enhanced hybridization process (TEHP) and rolling circle amplification (RCA). Upon the recognition of the molecular beacon (MB) to target DNA, the MB hybridizes with assistants and target DNA to form a ternary ''Y-junction''. The target DNA can be dissociated from the structure under the reaction of nicking endonuclease to initiate the next hybridization process. The template enhanced MB fragments further act as the primers of the RCA reaction to produce thousands of repeated oligonucleotide sequences, which can bind with oligonucleotide functionalized QDs. The attached signal tags can be easily read out by square-wave voltammetry after dissolving with acid. Because of the cascade signal amplification and the specific TEHP and RCA reaction, this newly designed protocol provides an ultrasensitive electrochemical detection of DNA down to the attomolar level (11 aM) with a linear range of 6 orders of magnitude (from 1 × 10(-17) to 1 × 10(-11) M) and can discriminate mismatched DNA from perfect matched target DNA with high selectivity. The high sensitivity and specificity make this method a great potential for early diagnosis in gene-related diseases.

Highly sensitive dual mode electrochemical platform for microRNA detection

NASA Astrophysics Data System (ADS)

Jolly, Pawan; Batistuti, Marina R.; Miodek, Anna; Zhurauski, Pavel; Mulato, Marcelo; Lindsay, Mark A.; Estrela, Pedro

2016-11-01

MicroRNAs (miRNAs) play crucial regulatory roles in various human diseases including cancer, making them promising biomarkers. However, given the low levels of miRNAs present in blood, their use as cancer biomarkers requires the development of simple and effective analytical methods. Herein, we report the development of a highly sensitive dual mode electrochemical platform for the detection of microRNAs. The platform was developed using peptide nucleic acids as probes on gold electrode surfaces to capture target miRNAs. A simple amplification strategy using gold nanoparticles has been employed exploiting the inherent charges of the nucleic acids. Electrochemical impedance spectroscopy was used to monitor the changes in capacitance upon any binding event, without the need for any redox markers. By using thiolated ferrocene, a complementary detection mode on the same sensor was developed where the increasing peaks of ferrocene were recorded using square wave voltammetry with increasing miRNA concentration. This dual-mode approach allows detection of miRNA with a limit of detection of 0.37 fM and a wide dynamic range from 1 fM to 100 nM along with clear distinction from mismatched target miRNA sequences. The electrochemical platform developed can be easily expanded to other miRNA/DNA detection along with the development of microarray platforms.

Application of differential pulse voltammetry to determine the efficiency of stripping tocopherols from commercial fish oil

USDA-ARS?s Scientific Manuscript database

There has been an increase in the use of electrochemical methods for monitoring antioxidant levels in a variety of disciplines due to the sensitivity, low detection limits, ease of use, low cost and rapid analysis time offered by these techniques. One technique that has received specific attention i...

An Environmentally Friendly, Cost-Effective Determination of Lead in Environmental Samples Using Anodic Stripping Voltammetry

ERIC Educational Resources Information Center

Goldcamp, Michael J.; Underwood, Melinda N.; Cloud, Joshua L.; Harshman, Sean

2008-01-01

Contamination of the environment with heavy metals such as lead presents many health risks. Simple, effective, and field-portable methods for the measurement of toxic metals in environmental samples are vital tools for evaluating the risks that these contaminants pose. This article describes the use of new developments in anodic stripping…

An enzyme free electrochemical biosensor for sensitive detection of miRNA with a high discrimination factor by coupling the strand displacement reaction and catalytic hairpin assembly recycling.

PubMed

Yao, Juan; Zhang, Zhang; Deng, Zhenghua; Wang, Youqiang; Guo, Yongcan

2017-10-23

An isothermal, enzyme free, ultra-specific and ultra-sensitive protocol for electrochemical detection of miRNAs is proposed based on the toehold-mediated strand displacement reaction (SDR) and non-enzymatic catalytic hairpin reaction (CHA) recycling. The SDR was first triggered only in the presence of target miRNA and this process also affects other miRNA interferences having similar target sequences, thus guaranteeing a high discrimination factor and could be used in rare content miRNA detection with various amounts of interferences having similar target sequences. The output protector strand then triggered enzyme free CHA amplification and generates plenty of hairpin self-assembly products. This process in turn influences SDR equilibrium to move to the right and generates large amounts of protector output to ensure analysis sensitivity. Compared with traditional CHA, our proposed method greatly improved the signal to noise ratio and shows excellent performance in rare miRNA detection with miRNA analogue interference. Under the optimal experimental conditions and using square wave voltammetry, the established biosensor could detect target miRNA-21 down to 30 fM (S/N = 3) with a dynamic range from 100 fM to 2 nM, and discriminate rare target miRNA-21 from mismatched miRNA with high selectivity. This method holds great promise in miRNA detection from human cancer cell lines and would be a versatile and powerful tool for clinical molecular diagnostics.

Simultaneous detection of morphine and codeine in urine samples of heroin addicts using multi-walled carbon nanotubes modified SnO2-Zn2SnO4 nanocomposites paste electrode

NASA Astrophysics Data System (ADS)

Taei, M.; Hasanpour, F.; Hajhashemi, V.; Movahedi, M.; Baghlani, H.

2016-02-01

The SnO2-Zn2SnO4 nanocomposite was successfully prepared via a simple solid state method. Then, a chemically modified electrode based on incorporating SnO2-Zn2SnO4 into multi-walled carbon nanotube paste matrix (MWCNTs/SnO2-Zn2SnO4/CPE) was prepared for the simultaneous determination of morphine(MO) and codeine (CO). The measurements were carried out by application of differential pulse voltammetry (DPV), cyclic voltammetry, and chronoamperometry. The MWCNTs/SnO2-Zn2SnO4/CPE showed an efficient electrocatalytic activity for the oxidation of MO and CO. The separation of the oxidation peak potential for MO-CO was about 550 mV. The calibration curves obtained for MO and CO were in the ranges of 0.1-310 μmol L-1 and 0.1-600.0 μmol L-1, respectively. The detection limits (S/N = 3) were 0.009 μmol L-1 for both drugs. The method also successfully employed as a selective, simple, and precise method for the determination of MO and CO in pharmaceutical and biological samples.

2,3-diaminopyridine functionalized reduced graphene oxide-supported palladium nanoparticles with high activity for electrocatalytic oxygen reduction reaction

NASA Astrophysics Data System (ADS)

Yasmin, Sabina; Joo, Yuri; Jeon, Seungwon

2017-06-01

The electrochemical deposition of Pd nanoparticles (Pd NPs) on 2,3 diamino pyridine functionalized reduced graphene oxide (2,3 DAP-rGO/Pd) has been investigated for the oxygen reduction reaction (ORR) in alkaline media. First, 2,3 diaminopyridine functionalized graphene oxide (2,3 DAP-rGO) has been synthesized via simple hydrothermal method. Then, palladium is directly incorporated into the 2,3 DAP-rGO by electrochemical deposition method to generate 2,3 DAP-rGO/Pd composites. The as-prepared material 2,3 DAP-rGO/Pd has been characterized by various instrumental methods. The morphological analysis shows the cluster-like Pd nanoparticles are dispersed onto the 2,3 diamino pyridine functionalized reduced graphene oxide (2,3 DAP-rGO). The electrocatalytic activities have been verified using cyclic voltammetry (CV) and hydrodynamic voltammetry and chronoamperometry techniques in 0.1 M KOH electrolyte. The as-synthesized 2,3 DAP-rGO/Pd shows higher catalytic activity toward ORR with more positive onset potential and cathodic current density, superior methanol/ethanol tolerance and excellent stability in alkaline medium. It is also noteworthy that the 2,3 DAP-rGO/Pd exhibits a four-electron transfer pathway for ORR with lower H2O2 yield.

Development of electrochemical folic acid sensor based on hydroxyapatite nanoparticles.

PubMed

Kanchana, P; Sekar, C

2015-02-25

We report the synthesis of hydroxyapatite (HA) nanoparticles (NPs) by a simple microwave irradiation method and its application as sensing element for the precise determination of folic acid (FA) by electrochemical method. The structure and composition of the HA NPs characterized using XRD, FTIR, Raman and XPS. SEM and EDX studies confirmed the formation of elongated spherical shaped HA NPs with an average particle size of about 34 nm. The HA NPs thin film on glassy carbon electrode (GCE) were deposited by drop casting method. Electrocatalytic behavior of FA in the physiological pH 7.0 was investigated by cyclic voltammetry (CV), linear sweep voltammetry (LSV) and chronoamperometry. The fabricated HA/GCE exhibited a linear calibration plot over a wide FA concentration ranging from 1.0×10(-7) to 3.5×10(-4) M with the detection limit of 75 nM. In addition, the HA NPs modified GCE showed good selectivity toward the determination of FA even in the presence of a 100-fold excess of ascorbic acid (AA) and 1000-fold excess of other common interferents. The fabricated biosensor exhibits good sensitivity and stability, and was successfully applied for the determination of FA in pharmaceutical samples. Copyright © 2014 Elsevier B.V. All rights reserved.

Simultaneous determination of hydroquinone, catechol and resorcinol by voltammetry using graphene screen-printed electrodes and partial least squares calibration.

PubMed

Aragó, Miriam; Ariño, Cristina; Dago, Àngela; Díaz-Cruz, José Manuel; Esteban, Miquel

2016-11-01

Catechol (CC), resorcinol (RC) and hydroquinone (HQ) are dihydroxybenzene isomers that usually coexist in different samples and can be determined using voltammetric techniques taking profit of their fast response, high sensitivity and selectivity, cheap instrumentation, simple and timesaving operation modes. However, a strong overlapping of CC and HQ signals is observed hindering their accurate analysis. In the present work, the combination of differential pulse voltammetry with graphene screen-printed electrodes (allowing detection limits of 2.7, 1.7 and 2.4µmolL(-1) for HQ, CC and RC respectively) and the data analysis by partial least squares calibration (giving root mean square errors of prediction, RMSEP values, of 2.6, 4.1 and 2.3 for HQ, CC and RC respectively) has been proposed as a powerful tool for the quantification of mixtures of these dihydroxybenzene isomers. The commercial availability of the screen-printed devices and the low cost and simplicity of the analysis suggest that the proposed method can be a valuable alternative to chromatographic and electrophoretic methods for the considered species. The method has been applied to the analysis of these isomers in spiked tap water. Copyright © 2016 Elsevier B.V. All rights reserved.

Low-cost and disposable sensors for the simultaneous determination of coenzyme Q10 and α-lipoic acid using manganese (IV) oxide-modified screen-printed graphene electrodes.

PubMed

Charoenkitamorn, Kanokwan; Chaiyo, Sudkate; Chailapakul, Orawon; Siangproh, Weena

2018-04-03

In this work, for the first time, manganese (IV) oxide-modified screen-printed graphene electrodes (MnO 2 /SPGEs) were developed for the simultaneous electrochemical detection of coenzyme Q10 (CoQ10) and α-lipoic acid (ALA). This sensor exhibits attractive benefits such as simplicity, low production costs, and disposability. Cyclic voltammetry (CV) was used to characterize the electrochemical behavior of the analyte and investigate the capacitance and electroactive surface area of the unmodified and modified electrode surfaces. The electrochemical behavior of CoQ10 and ALA on MnO 2 /SPGEs was also discussed. Additionally, square wave anodic stripping voltammetry (SWASV) was used for the quantitative determination of CoQ10 and ALA. Under optimal conditions, the obtained signals are linear in the concentration range from 2.0 to 75.0 μg mL -1 for CoQ10 and 0.3-25.0 μg mL -1 for ALA. The low limits of detection (LODs) were found to be 0.56 μg mL -1 and 0.088 μg mL -1 for CoQ10 and ALA, respectively. Moreover, we demonstrated the utility and applicability of the MnO 2 /SPGE sensor through simultaneous measurements of CoQ10 and ALA in dietary supplements. The sensor provides high accuracy measurements, exhibiting its high potential for practical applications. Copyright © 2017 Elsevier B.V. All rights reserved.

Orthogonal identification of gunshot residue with complementary detection principles of voltammetry, scanning electron microscopy, and energy-dispersive X-ray spectroscopy: sample, screen, and confirm.

PubMed

O'Mahony, Aoife M; Samek, Izabela A; Sattayasamitsathit, Sirilak; Wang, Joseph

2014-08-19

Field-deployable voltammetric screening coupled with complementary laboratory-based analysis to confirm the presence of gunshot residue (GSR) from the hands of a subject who has handled, loaded, or discharged a firearm is described. This protocol implements the orthogonal identification of the presence of GSR utilizing square-wave stripping voltammetry (SWSV) as a rapid screening tool along with scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDX) to confirm the presence of the characteristic morphology and metal composition of GSR particles. This is achieved through the judicious modification of the working electrode of a carbon screen-printed electrode (CSPE) with carbon tape (used in SEM analysis) to fix and retain a sample. A comparison between a subject who has handled and loaded a firearm and a subject who has had no contact with GSR shows the significant variations in voltammetric signals and the presence or absence of GSR-consistent particles and constituent metals. This initial electrochemical screening has no effect on the integrity of the metallic particles, and SEM/EDX analysis conducted prior to and postvoltammetry show no differences in analytical output. The carbon tape is instrumental in retaining the GSR sample after electrochemical analysis, supported by comparison with orthogonal detection at a bare CSPE. This protocol shows great promise as a two-tier detection system for the presence of GSR from the hands of a subject, whereby initial screening can be conducted rapidly onsite by minimally trained operators; confirmation can follow at the same substrate to substantiate the voltammetric results.

Novel and simple electrochemical biosensor monitoring attomolar levels of miRNA-155 in breast cancer.

PubMed

Cardoso, Ana R; Moreira, Felismina T C; Fernandes, Rúben; Sales, M Goreti F

2016-06-15

This work, describes for the first time, a simple biosensing design to yield an ultrasensitive electrochemical biosensor for a cancer biomarker detection, miRNA-155, with linear response down to the attomolar range. MiRNA-155 was selected for being overexpressed in breast cancer. The biosensor was assembled in two stages: (1) the immobilization of the anti-miRNA-155 that was thiol modified on an Au-screen printed electrode (Au-SPE), followed by (2) blocking the areas of non-specific binding with mercaptosuccinic acid. Atomic force microscopy (AFM) and electrochemical techniques including cyclic voltammetry (CV), impedance spectroscopy (EIS) and square wave voltammetry (SWV) confirmed the surface modification of these devices and their ability to hybridize successfully and stably with miRNA-155. The final biosensor provided a sensitive detection of miRNA-155 from 10 aM to 1.0 nM with a low detection limit (LOD) of 5.7 aM in real human serum samples. Good results were obtained in terms of selectivity towards breast cancer antigen CA-15.3 and bovine serum albumin (BSA). Raw fluid extracts from cell-lines of melanoma did not affect the biosensor response (no significant change of the blank), while raw extracts from breast cancer yielded a positive signal against miRNA-155. This simple and sensitive strategy is a promising alternative for simultaneous quantitative analysis of multiple miRNA in physiological fluids for biomedical research and point-of-care (POC) diagnosis. Copyright © 2016 The Authors. Published by Elsevier B.V. All rights reserved.

Direct electrochemistry and electrocatalysis of heme proteins immobilised in carbon-coated nickel magnetic nanoparticle-chitosan-dimethylformamide composite films in room-temperature ionic liquids.

PubMed

Wang, Ting; Wang, Lu; Tu, Jiaojiao; Xiong, Huayu; Wang, Shengfu

2013-12-01

The direct electrochemistry and electrocatalysis of heme proteins entrapped in carbon-coated nickel magnetic nanoparticle-chitosan-dimethylformamide (CNN-CS-DMF) composite films were investigated in the hydrophilic ionic liquid [bmim][BF4]. The surface morphologies of a representative set of films were characterised via scanning electron microscopy. The proteins immobilised in the composite films were shown to retain their native secondary structure using UV-vis spectroscopy. The electrochemical performance of the heme proteins-CNN-CS-DMF films was evaluated via cyclic voltammetry and chronoamperometry. A pair of stable and well-defined redox peaks was observed for the heme protein films at formal potentials of -0.151 V (HRP), -0.167 V (Hb), -0.155 V (Mb) and -0.193 V (Cyt c) in [bmim][BF4]. Moreover, several electrochemical parameters of the heme proteins were calculated by nonlinear regression analysis of the square-wave voltammetry. The addition of CNN significantly enhanced not only the electron transfer of the heme proteins but also their electrocatalytic activity toward the reduction of H2O2. Low apparent Michaelis-Menten constants were obtained for the heme protein-CNN-CS-DMF films, demonstrating that the biosensors have a high affinity for H2O2. In addition, the resulting electrodes displayed a low detection limit and improved sensitivity for detecting H2O2, which indicates that the biocomposite film can serve as a platform for constructing new non-aqueous biosensors for real detection. Copyright © 2013 Elsevier B.V. All rights reserved.

Electrosynthesized MIPs for transferrin: Plastibodies or nano-filters?

PubMed

Zhang, Xiaorong; Yarman, Aysu; Erdossy, Júlia; Katz, Sagie; Zebger, Ingo; Jetzschmann, Katharina J; Altintas, Zeynep; Wollenberger, Ulla; Gyurcsányi, Róbert E; Scheller, Frieder W

2018-05-15

Molecularly imprinted polymer (MIP) nanofilms for transferrin (Trf) have been synthesized on gold surfaces by electro-polymerizing the functional monomer scopoletin in the presence of the protein target or around pre-adsorbed Trf. As determined by atomic force microscopy (AFM) the film thickness was comparable with the molecular dimension of the target. The target (re)binding properties of the electro-synthesized MIP films was evaluated by cyclic voltammetry (CV) and square wave voltammetry (SWV) through the target-binding induced permeability changes of the MIP nanofilms to the ferricyanide redox marker, as well as by surface plasmon resonance (SPR) and surface enhanced infrared absorption spectroscopy (SEIRAS) of the immobilized protein molecules. For Trf a linear concentration dependence in the lower micromolar range and an imprinting factor of ~5 was obtained by SWV and SPR. Furthermore, non-target proteins including the iron-free apo-Trf were discriminated by pronounced size and shape specificity. Whilst it is generally assumed that the rebinding of the target or of cross-reacting proteins exclusively takes place at the polymer here we considered also the interaction of the protein molecules with the underlying gold transducers. We demonstrate by SWV that adsorption of proteins suppresses the signal of the redox marker even at the bare gold surface and by SEIRAS that the treatment of the MIP with proteinase K or NaOH only partially removes the target protein. Therefore, we conclude that when interpreting binding of proteins to directly MIP-covered gold electrodes the interactions between the protein and the gold surface should also be considered. Copyright © 2018 Elsevier B.V. All rights reserved.

[Monitoring of the concentration of lithium and heavy metals in drinking water by the method of stripping voltammetry].

PubMed

Khakhanina, T I; Kovaleva, A Iu; Gurskaia, A A

2007-01-01

A method for monitoring of the concentration of lithium, zinc, cadmium, lead, and copper in drinking water is suggested. Monitoring can be performed within the range of 1.5(10(-8) - 2.0(10(-6) mg/dm3. A new design of the electrochemical cell is suggested. Analysis is performed against the background of 0.02 M dimethylformamide solution of (C4H9)4NCIO4. The time and potential of electrolysis are determined experimentally. The method can be used in medical research.

The Rise of Voltammetry: From Polarography to the Scanning Electrochemical Microscope

ERIC Educational Resources Information Center

Bard, Allen J.

2007-01-01

The drooping mercury electrode (DME) was previously used to carry out electrochemical experiments but invention of polarography technique changed this. Voltammetry with DME was given the term polarography and are used in measurement of current as a function of potential at small electrodes.

Theory of linear sweep voltammetry with diffuse charge: Unsupported electrolytes, thin films, and leaky membranes

NASA Astrophysics Data System (ADS)

Yan, David; Bazant, Martin Z.; Biesheuvel, P. M.; Pugh, Mary C.; Dawson, Francis P.

2017-03-01

Linear sweep and cyclic voltammetry techniques are important tools for electrochemists and have a variety of applications in engineering. Voltammetry has classically been treated with the Randles-Sevcik equation, which assumes an electroneutral supported electrolyte. In this paper, we provide a comprehensive mathematical theory of voltammetry in electrochemical cells with unsupported electrolytes and for other situations where diffuse charge effects play a role, and present analytical and simulated solutions of the time-dependent Poisson-Nernst-Planck equations with generalized Frumkin-Butler-Volmer boundary conditions for a 1:1 electrolyte and a simple reaction. Using these solutions, we construct theoretical and simulated current-voltage curves for liquid and solid thin films, membranes with fixed background charge, and cells with blocking electrodes. The full range of dimensionless parameters is considered, including the dimensionless Debye screening length (scaled to the electrode separation), Damkohler number (ratio of characteristic diffusion and reaction times), and dimensionless sweep rate (scaled to the thermal voltage per diffusion time). The analysis focuses on the coupling of Faradaic reactions and diffuse charge dynamics, although capacitive charging of the electrical double layers is also studied, for early time transients at reactive electrodes and for nonreactive blocking electrodes. Our work highlights cases where diffuse charge effects are important in the context of voltammetry, and illustrates which regimes can be approximated using simple analytical expressions and which require more careful consideration.

Electrode Reactions Coupled with Chemical Reactions of Oxygen, Water and Acetaldehyde in an Ionic Liquid: New Approaches for Sensing Volatile Organic Compounds.

PubMed

Chi, Xiaowei; Tang, Yongan; Zeng, Xiangqun

2016-10-20

Water and oxygen are ubiquitous present in ambient conditions. This work studies the unique oxygen, trace water and a volatile organic compound (VOC) acetaldehyde redox chemistry in a hydrophobic and aprotic ionic liquid (IL), 1-butyl-1-methylpyrrolidinium bis(trifluoromethanesulfonyl)imide ([Bmpy] [NTf 2 ]) by cyclic voltammetry and potential step methods. One electron oxygen reduction leads to superoxide radical formation in the IL. Trace water in the IL acts as a protic species that reacts with the superoxide radical. Acetaldehyde is a stronger protic species than water for reacting with the superoxide radical. The presence of trace water in the IL was also demonstrated to facilitate the electro-oxidation of acetaldehyde, with similar mechanism to that in the aqueous solutions. A multiple-step coupling reaction mechanism between water, superoxide radical and acetaldehyde has been described. The unique characteristics of redox chemistry of acetaldehyde in [Bmpy][NTf 2 ] in the presence of oxygen and trace water can be controlled by electrochemical potentials. By controlling the electrode potential windows, several methods including cyclic voltammetry, potential step methods (single-potential, double-potential and triple-potential step methods) were established for the quantification of acetaldehyde. Instead of treating water and oxygen as frustrating interferents to ILs, we found that oxygen and trace water chemistry in [Bmpy][NTf 2 ] can be utilized to develop innovative electrochemical methods for electroanalysis of acetaldehyde.

Electrode Reactions Coupled with Chemical Reactions of Oxygen, Water and Acetaldehyde in an Ionic Liquid: New Approaches for Sensing Volatile Organic Compounds

PubMed Central

Chi, Xiaowei; Tang, Yongan; Zeng, Xiangqun

2017-01-01

Water and oxygen are ubiquitous present in ambient conditions. This work studies the unique oxygen, trace water and a volatile organic compound (VOC) acetaldehyde redox chemistry in a hydrophobic and aprotic ionic liquid (IL), 1-butyl-1-methylpyrrolidinium bis(trifluoromethanesulfonyl)imide ([Bmpy] [NTf2]) by cyclic voltammetry and potential step methods. One electron oxygen reduction leads to superoxide radical formation in the IL. Trace water in the IL acts as a protic species that reacts with the superoxide radical. Acetaldehyde is a stronger protic species than water for reacting with the superoxide radical. The presence of trace water in the IL was also demonstrated to facilitate the electro-oxidation of acetaldehyde, with similar mechanism to that in the aqueous solutions. A multiple-step coupling reaction mechanism between water, superoxide radical and acetaldehyde has been described. The unique characteristics of redox chemistry of acetaldehyde in [Bmpy][NTf2] in the presence of oxygen and trace water can be controlled by electrochemical potentials. By controlling the electrode potential windows, several methods including cyclic voltammetry, potential step methods (single-potential, double-potential and triple-potential step methods) were established for the quantification of acetaldehyde. Instead of treating water and oxygen as frustrating interferents to ILs, we found that oxygen and trace water chemistry in [Bmpy][NTf2] can be utilized to develop innovative electrochemical methods for electroanalysis of acetaldehyde. PMID:29142331

Introduction of a carbon paste electrode based on nickel carbide for investigation of interaction between warfarin and vitamin K1.

PubMed

Torkashvand, Maryam; Gholivand, Mohammad Bagher; Taherpour, Avat Arman; Boochani, Arash; Akhtar, Arsalan

2017-05-30

In this paper a novel electrochemical sensor based on nickel carbide (Ni 3 C) nanoparticles as a new modifier was constructed. Ni 3 C nanoparticle was synthesized and characterized by scanning electron microscopy, X-ray diffraction and first-principles study. Electrochemical impedance spectroscopy (EIS) and cyclic voltammetry (CV) studies confirmed the electrode modification. Afterwards, the new electrode for the first time was used for interaction study between vitamin K1 and warfarin as an anticoagulant drug by differential pulse voltammetry. The adduct formation between the drug and vitamin K1 was improved by decreasing in anodic peak current of warfarin in the presence of different amounts of vitamin K1. The binding constant between warfarin and vitamin K1 was obtained by voltammetric and UV-vis and fluorescence spectroscopic methods. The molecular modeling method was also performed to explore the structural features and binding mechanism of warfarin to vitamin K1. The different aspects of modeling of vitamin K1 and warfarin and their adduct structures confirmed the adduct formation by hydrogen bonding. Copyright © 2017 Elsevier B.V. All rights reserved.

Magnetic MoS2 on multiwalled carbon nanotubes for sulfide sensing.

PubMed

Li, Chunxiang; Zhang, Dan; Wang, Jiankang; Hu, Pingan; Jiang, Zhaohua

2017-07-04

A novel hybrid metallic cobalt insided in multiwalled carbon nanotubles/molybdenum disulfide (Co@CNT/MoS 2 ) modified glass carbon electrode (GCE) was fabricated with a adhesive of Nafion suspension and used as chemical sensors for sulfide detection. Single-layered MoS 2 was coated on CNTs through magnetic traction force between paramagnetic monolayer MoS 2 and Co particles in CNTs. Co particles faciliated the collection of paramagnetic monolayer MoS 2 exfoliated from bulk MoS 2 in solution. Amperometric analysis, cycle voltammetry, cathodic stripping analysis and linear sweep voltammetry results showed the Co@CNT/MoS 2 modified GCE exhibited excellent electrochemical activity to sulfide in buffer solutions, but amperometric analysis was found to be more sensitive than the other methods. The amperometric response result indicated the Co@CNT/MoS 2 -modified GCE electrode was an excellent electrochemical sensor for detecting S 2- with a detection limit of 7.6 nM and sensitivity of 0.23 mA/μM. The proposed electrode was used for the determination of sulfide levels in hydrogen sulfide-pretreated fruits, and the method was also verified with recovery studies. Copyright © 2017 Elsevier B.V. All rights reserved.

Preparation of Supercapacitors on Flexible Substrates with Electrodeposited PEDOT/Graphene Composites.

PubMed

Lehtimäki, Suvi; Suominen, Milla; Damlin, Pia; Tuukkanen, Sampo; Kvarnström, Carita; Lupo, Donald

2015-10-14

Composite films consisting of poly(3,4-ethylenedioxythiophene) (PEDOT) and graphene oxide (GO) were electrochemically polymerized by electrooxidation of EDOT in ionic liquid (BMIMBF4) onto flexible electrode substrates. Two polymerization approaches were compared, and the cyclic voltammetry (CV) method was found to be superior to potentiostatic polymerization for the growth of PEDOT/GO films. After deposition, incorporated GO was reduced to rGO by a rapid electrochemical method of repetitive cathodic potential cycling, without using any reducing reagents. The films were characterized in 3-electrode configuration in BMIMBF4. Symmetric supercapacitors with aqueous electrolyte were assembled from the composite films and characterized through cyclic voltammetry and galvanostatic discharge tests. It was shown that PEDOT/rGO composites have better capacitive properties than pure PEDOT or the unreduced composite film. The cycling stability of the supercapacitors was also tested, and the results indicate that the specific capacitance still retains well over 90% of the initial value after 2000 consecutive charging/discharging cycles. The supercapacitors were demonstrated as energy storages in a room light energy harvester with a printed organic solar cell and printed electrochromic display. The results are promising for the development of energy-autonomous, low-power, and disposable electronics.

Anodic stripping voltammetry of gold nanoparticles at boron-doped diamond electrodes and its application in immunochromatographic strip tests.

PubMed

Ivandini, Tribidasari A; Wicaksono, Wiyogo P; Saepudin, Endang; Rismetov, Bakhadir; Einaga, Yasuaki

2015-03-01

Anodic stripping voltammetry (ASV) of colloidal gold-nanoparticles (AuNPs) was investigated at boron-doped diamond (BDD) electrodes in 50 mM HClO4. A deposition time of 300 s at-0.2 V (vs. Ag/AgCl) was fixed as the condition for the ASV. The voltammograms showed oxidation peaks that could be attributed to the oxidation of gold. These oxidation peaks were then investigated for potential application in immunochromatographic strip tests for the selective and quantitative detection of melamine, in which AuNPs were used as the label for the antibody of melamine. Linear regression of the oxidation peak currents appeared in the concentration range from 0.05-0.6 μg/mL melamine standard, with an estimated LOD of 0.069 μg/mL and an average relative standard deviation of 8.0%. This indicated that the method could be considered as an alternative method for selective and quantitative immunochromatographic applications. The validity was examined by the measurements of melamine injected into milk samples, which showed good recovery percentages during the measurements. Copyright © 2014 Elsevier B.V. All rights reserved.

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

PubMed

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

2014-08-15

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

Schiff Base modified on CPE electrode and PCB gold electrode for selective determination of silver ion

NASA Astrophysics Data System (ADS)

Leepheng, Piyawan; Suramitr, Songwut; Phromyothin, Darinee

2017-09-01

The schiff base was synthesized by 2,5-thiophenedicarboxaldehyde and 1,2,4-thiadiazole-3,5-diamine with condensation method. There was modified on carbon paste electrode (CPE) and Printed circuit board (PCB) gold electrode for determination silver ion. The schiff base modified electrodes was characterized by atomic force microscopy (AFM) and scanning electron microscopy (SEM), respectively. The electrochemical study was reported by cyclic voltammetry method and impedance spectroscopy using modified electrode as working electrode, platinum wire and Ag/AgCl as counter electrode and reference electrode, respectively. The modified electrodes have suitable detection for Ag+. The determination of silver ions using the modified electrodes depended linearly on Ag+ concentration in the range 1×10-10 M to 1×10-7 M, with cyclic voltammetry sensitivity were 2.51×108 μAM-1 and 1.88×108 μAM-1 for PCB gold electrode and CPE electrode, respectively, limits of detection were 5.33×10-9 M and 1.99×10-8 M for PCB gold electrode and CPE electrode, respectively. The modified electrodes have high accuracy, inexpensive and can applied to detection Ag+ in real samples.

Highly selective determination of amitriptyline using Nafion-AuNPs@branched polyethyleneimine-derived carbon hollow spheres in pharmaceutical drugs and biological fluids.

PubMed

Zad, Zeinab Rezayati; Davarani, Saied Saeed Hosseiny; Taheri, Ali Reza; Bide, Yasamin

2016-12-15

In this paper, AuNPs@Polyethyleneimine-derived carbon hollow spheres were synthesized by a versatile and facile method in three steps and successfully developed and validated as Amitriptyline sensor using cyclic voltammetry (CV), chronoamperometry (CA) and differential pulse voltammetry (DPV) methods. The characterization of the electrode surface has been carried out by means of scanning electron microscopy (SEM), transmission electron microscopy (TEM), x-ray diffraction (XRD), x-ray photo-electron spectrum (XPS), electrochemical impedance spectroscopy (EIS) and chronocoulometry (CC). The obtained negatively charged modified electrode was highly selective to Amitriptyline and it was shown a wide linear range from 0.1 to 700μmolL(-1), with a lower detection limit of 0.034μmolL(-1) (n=5, S/N=3), revealing the high-sensitivity properties. The modified electrode is used to achieve the real-time quantitative detection of AMT for biological applications, and satisfactory results are obtained. Due to the advantages of the sensor, its selectivity, sensitivity and stability, it will have a bright future in the field of medical diagnosis. Copyright © 2016 Elsevier B.V. All rights reserved.

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

PubMed

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

2012-12-01

Electrochemical oxidation of acyclovir at fullerene-C(60)-modified glassy carbon electrode has been investigated using cyclic and differential pulse voltammetry. In pH 7.4 phosphate buffer, acyclovir showed an irreversible oxidation peak at about 0.96V. The cyclic voltammetric results showed that fullerene-C(60)-modified glassy carbon electrode can remarkably enhance electrocatalytic activity towards the oxidation of acyclovir. The electrocatalytic behavior was further exploited as a sensitive detection scheme for the acyclovir determination by differential pulse voltammetry. Effects of anodic peak potential (E(p)/V), anodic peak current (I(p)/μA) and heterogeneous rate constant (k(0)) have been discussed. Under optimized conditions, the concentration range and detection limit were 9.0×10(-8) to 6.0×10(-6)M and 1.48×10(-8)M, respectively. The proposed method was applied to acyclovir determination in pharmaceutical samples and human biological fluids such as urine and blood plasma as a real sample. This method can also be employed in quality control and routine determination of drugs in pharmaceutical formulations. Copyright © 2012 Elsevier B.V. All rights reserved.

An electrochemical genosensor for Salmonella typhi on gold nanoparticles-mercaptosilane modified screen printed electrode.

PubMed

Das, Ritu; Sharma, Mukesh K; Rao, Vepa K; Bhattacharya, B K; Garg, Iti; Venkatesh, V; Upadhyay, Sanjay

2014-10-20

In this work, we fabricated a system of integrated self-assembled layer of organosilane 3-mercaptopropyltrimethoxy silane (MPTS) on the screen printed electrode (SPE) and electrochemically deposited gold nanoparticle for Salmonella typhi detection employing Vi gene as a molecular marker. Thiolated DNA probe was immobilized on a gold nanoparticle (AuNP) modified SPE for DNA hybridization assay using methylene blue as redox (electroactive) hybridization indicator, and signal was monitored by differential pulse voltammetry (DPV) method. The modified SPE was characterized by cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS), and atomic force microscopy (AFM) method. The DNA biosensor showed excellent performances with high sensitivity and good selectivity. The current response was linear with the target sequence concentrations ranging from 1.0 × 10(-11) to 0.5 × 10(-8)M and the detection limit was found to be 50 (± 2.1)pM. The DNA biosensor showed good discrimination ability to the one-base, two-base and three-base mismatched sequences. The fabricated genosensor could also be regenerated easily and reused for three to four times for further hybridization studies. Copyright © 2014 Elsevier B.V. All rights reserved.

Development and Use of an Open-Source, User-Friendly Package to Simulate Voltammetry Experiments

ERIC Educational Resources Information Center

Wang, Shuo; Wang, Jing; Gao, Yanjing

2017-01-01

An open-source electrochemistry simulation package has been developed that simulates the electrode processes of four reaction mechanisms and two typical electroanalysis techniques: cyclic voltammetry and chronoamperometry. Unlike other open-source simulation software, this package balances the features with ease of learning and implementation and…

Cyclic Voltammetry Simulations with DigiSim Software: An Upper-Level Undergraduate Experiment

ERIC Educational Resources Information Center

Messersmith, Stephania J.

2014-01-01

An upper-division undergraduate chemistry experiment is described which utilizes DigiSim software to simulate cyclic voltammetry (CV). Four mechanisms were studied: a reversible electron transfer with no subsequent or proceeding chemical reactions, a reversible electron transfer followed by a reversible chemical reaction, a reversible chemical…

Pseudo-stir bar hollow fiber solid/liquid phase microextraction combined with anodic stripping voltammetry for determination of lead and cadmium in water samples

PubMed Central

Es’haghi, Zarrin; Hoseini, Hasan Ali; Mohammadi-Nokhandani, Saeed; Ebrahimi, Javad

2013-01-01

A new procedure is presented for the determination of low concentrations of lead and cadmium in water samples. Ligand assisted pseudo-stir bar hollow fiber solid/liquid phase microextraction using sol–gel sorbent reinforced with carbon nanotubes was combined with differential pulse anodic stripping voltammetry for simultaneous determination of cadmium and lead in tap water, and Darongar river water samples. In the present work, differential pulse anodic stripping voltammetry (DPASV) using a hanging mercury drop electrode (HMDE) was used in order to determine the ultra trace level of lead and cadmium ions in real samples. This method is based on accumulation of lead and cadmium ions on the electrode using different ligands; Quinolin-8-ol, 5,7-diiodo quinoline-8-ol, 4,5-diphenyl-1H-imidazole-2(3H)-one and 2-{[2-(2-Hydroxy-ethylamino)-ethylamino]-methyl}-phenol as the complexing agent. The optimized conditions were obtained. The relationship between the peak current versus concentration was linear over the range of 0.05–500 ng mL−1 for Cd (II) and Pb (II). The limits of detection for lead and cadmium were 0.015 ng mL−1 and 0.012 ng mL−1, respectively. Under the optimized conditions, the pre-concentration factors are 2440 and 3710 for Cd (II) and Pb (II) in 5 mL of water sample, respectively. PMID:25685537

Examination of Rapid Dopamine Dynamics with Fast Scan Cyclic Voltammetry During Intra-oral Tastant Administration in Awake Rats.

PubMed

Wickham, Robert J; Park, Jinwoo; Nunes, Eric J; Addy, Nii A

2015-08-12

Rapid, phasic dopamine (DA) release in the mammalian brain plays a critical role in reward processing, reinforcement learning, and motivational control. Fast scan cyclic voltammetry (FSCV) is an electrochemical technique with high spatial and temporal (sub-second) resolution that has been utilized to examine phasic DA release in several types of preparations. In vitro experiments in single-cells and brain slices and in vivo experiments in anesthetized rodents have been used to identify mechanisms that mediate dopamine release and uptake under normal conditions and in disease models. Over the last 20 years, in vivo FSCV experiments in awake, freely moving rodents have also provided insight of dopaminergic mechanisms in reward processing and reward learning. One major advantage of the awake, freely moving preparation is the ability to examine rapid DA fluctuations that are time-locked to specific behavioral events or to reward or cue presentation. However, one limitation of combined behavior and voltammetry experiments is the difficulty of dissociating DA effects that are specific to primary rewarding or aversive stimuli from co-occurring DA fluctuations that mediate reward-directed or other motor behaviors. Here, we describe a combined method using in vivo FSCV and intra-oral infusion in an awake rat to directly investigate DA responses to oral tastants. In these experiments, oral tastants are infused directly to the palate of the rat--bypassing reward-directed behavior and voluntary drinking behavior--allowing for direct examination of DA responses to tastant stimuli.

Dual channel sensitive detection of hsa-miR-21 based on rolling circle amplification and quantum dots tagging.

PubMed

Wangt, Dan-Chen; Hu, Li-Hui; Zhou, Yu-Hui; Huang, Yu-Ting; Li, Xinhua; Zhu, Jun-Jie

2014-04-01

An isothermal, highly sensitive and specific assay for the detection of hsa-miR-21 with the integration of QDs tagging and rolling circle amplification was offered. In addition, a dual channel strategy for miRNA detection was proposed: anodic stripping voltammetry (ASV) and fluorescent method were both performed for the final Cd2+ signal readout. The designed strategy exhibited good specificity to hsa-miR-21 and presented comparable detection results by detection methods.

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

NASA Astrophysics Data System (ADS)

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

2013-01-01

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

Characterization of graphene oxide produced by Hummers method and its supercapacitor applications

DOE Office of Scientific and Technical Information (OSTI.GOV)

Akgül, Ö., E-mail: omeraakgul@gmail.com; Tanrıverdi, A., E-mail: aa.kudret@hotmail.com; Alver, Ü., E-mail: ualver@ktu.edu.tr

2016-03-25

In this study, Graphene Oxide (GO) is produced using Hummers method. The produced GO were investigated by x-ray diffraction (XRD), fourier transform infrared spectroscopy (FTIR), UV-Vis spectrum, Raman spectroscopy and scanning electron microscopy (SEM). GO films on Ni foam were prepared by doctor-blading technique. The electrochemical performances of the as-synthesized GO electrode was evaluated using cyclic voltammetry (CV) in 6 M KOH aqueous solution. Capacitances of GO electrode was measured as 0.76 F/g.

Integrated explosive preconcentrator and electrochemical detection system for 2,4,6-trinitrotoluene (TNT) vapor.

PubMed

Cizek, Karel; Prior, Chad; Thammakhet, Chongdee; Galik, Michal; Linker, Kevin; Tsui, Ray; Cagan, Avi; Wake, John; La Belle, Jeff; Wang, Joseph

2010-02-19

This article reports on an integrated explosive-preconcentration/electrochemical detection system for 2,4,6-trinitrotoluene (TNT) vapor. The challenges involved in such system integration are discussed. A hydrogel-coated screen-printed electrode is used for the detection of the thermally desorbed TNT from a preconcentration device using rapid square wave voltammetry. Optimization of the preconcentration system for desorption of TNT and subsequent electrochemical detection was conducted yielding a desorption temperature of 120 degrees C under a flow rate of 500 mL min(-1). Such conditions resulted in a characteristic electrochemical signal for TNT representing the multi-step reduction process. Quantitative measurements produced a linear signal dependence on TNT quantity exposed to the preconcentrator from 0.25 to 10 microg. Finally, the integrated device was successfully demonstrated using a sample of solid TNT located upstream of the preconcentrator. Copyright 2009 Elsevier B.V. All rights reserved.

Bioelectrochemical Magnetic Immunosensing of Trichloropyridinol: A Potential Insecticide Biomarker

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liu, Guodong; Timchalk, Chuck; Lin, Yuehe

2006-07-01

A magnetic beads-based bioelectrochemical magnetic immunosensor was developed for the fast and sensitive determination of the trichloropyridinol (TCP) biomarker in environmental samples. After liquid phrase competitive immunoreaction among a limited amount of TCP antibody coated-magnetic beads (Ab-MBs), TCP analyte, and horseradish peroxidase (HRP) labeled TCP (HRP-TCP), a magnet/glassy carbon (MGC) electrode was used to collect a TCP-Abs-MBs and a HRP-TCP-Ab-MBs immunocomplex assembly. The activity of HRP tracers bound to the beads was monitored with highly sensitive square wave voltammetry (SWV) by accumulating an electroactive enzymatic product to the MGC electrode surface under constant potential (0.5 V) during enzymatic reaction inmore » the presence of 3’,3’,5’,5’-tetramethylbenzidine (TMB)-H2O2 substrate solution. The electrochemical characteristics of substrate and product were investigated, and the parameters of the immunoassay were optimized.« less

Hg(2+) detection using a disposable and miniaturized screen-printed electrode modified with nanocomposite carbon black and gold nanoparticles.

PubMed

Cinti, Stefano; Santella, Francesco; Moscone, Danila; Arduini, Fabiana

2016-05-01

A miniaturized screen-printed electrode (SPE) modified with a carbon black-gold nanoparticle (CBNP-AuNP) nanocomposite has been developed as an electrochemical sensor for the detection of inorganic mercury ions (Hg(2+)). The working electrode surface has been modified with nanocomposite constituted of CBNPs and AuNPs by an easy drop casting procedure that makes this approach extendible to an automatable mass production of modified SPEs. Square wave anodic stripping voltammetry (SWASV) was adopted to perform Hg(2+) detection, revealing satisfactory sensitivity and detection limit, equal to 14 μA ppb(-1) cm(-2) and 3 ppb, respectively. The applicability of the CBNP-AuNP-SPE for the determination of inorganic mercury has been assessed in river water by a simple filtration and acidification of the sample as well as in soil by means of a facile acidic extraction procedure assisted by ultrasound.

Polymer platforms for selective detection of cocaine in street samples adulterated with levamisole.

PubMed

Florea, Anca; Cowen, Todd; Piletsky, Sergey; De Wael, Karolien

2018-08-15

Accurate drug detection is of utmost importance for fighting against drug abuse. With a high number of cutting agents and adulterants being added to cut or mask drugs in street powders the number of false results is increasing. We demonstrate for the first time the usefulness of employing polymers readily synthesized by electrodeposition to selectively detect cocaine in the presence of the commonly used adulterant levamisole. The polymers were selected by computational modelling to exhibit high binding affinity towards cocaine and deposited directly on the surface of graphene-modified electrodes via electropolymerization. The resulting platforms allowed a distinct electrochemical signal for cocaine, which is otherwise suppressed by levamisole. Square wave voltammetry was used to quantify cocaine alone and in the presence of levamisole. The usefulness of the platforms was demonstrated in the screening of real street samples. Copyright © 2018 Elsevier B.V. All rights reserved.

Direct Electrodeposition of UO2 from Uranyl Bis(trifluoromethanesulfonyl)imide Dissolved in 1-Ethyl-3-methylimidazolium Bis(trifluoromethanesulfonyl)imide Room Temperature Ionic Liquid System

DOE PAGES

Freiderich, John W.; Wanigasekara, Eranda P.; Sun, Xiao-Guang; ...

2013-11-11

Our study demonstrates a direct electrodeposition of UO 2 at a Pt cathode from a solution of uranyl bis(trifluoromethanesulfonyl)imide [UO 2(NTf 2) 2)] in a bulk room-temperature ionic liquid (RTIL), 1-ethyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide (EMIM +NTf 2 –). Cyclic voltammetry (CV) studies revealed two reduction waves corresponding to the conversion of uranium(VI) to uranium(IV), and a mechanism for the overall electroreduction is proposed. A controlled-potential experiment was performed, holding the reduction potential at–1.0 V for 24 h to obtain a brown-black deposit of UO 2 on the Pt cathode. The Faradaic efficiency of the reduction process was determined to be >80%. Themore » UO 2deposit was characterized by powder X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS).« less

Detection of gamma-irradiation effect on DNA and protein using magnetic sensor and cyclic voltammetry.

PubMed

Park, Duck-Gun; Song, Hoon; Kishore, M B; Vértesy, G; Lee, Duk-Hyun

2013-11-01

In this study, a magnetic sensor utilizing Planar Hall Resistance (PHR) and cyclic Voltammetry (CV) for detecting the radiation effect was fabricated. Specifically, we applied in parallel a PHR sensor and CV device to monitor the irradiation effect on DNA and protein respectively. Through parallel measurements, we demonstrated that the PHR sensor and CV are sensitive enough to measure irradiation effect. The PHR voltage decreased by magnetic nanobead labeled DNA was slightly recovered after gamma ray irradiation. The behavior of cdk inhibitor protein p21 having a sandwich structure of Au/protein G/Ab/Ag/Ab was checked by monitoring the cyclic Voltammetry signal in analyzing the gamma ray irradiation effect.

Lead-Testing Service to Elementary and Secondary Schools Using Anodic Stripping Voltammetry

ERIC Educational Resources Information Center

Goebel, Amanda; Vos, Tracy; Louwagie, Anne; Lundbohm, Laura; Brown, Jay H.

2004-01-01

The undergraduate chemistry club of the Southwest Minnesota State University offers assistance in lead-testing through the anodic stripping voltammetry (ASV) technique to elementary and secondary schools. Emphasis is given to this community service activity, which has increased club membership, and promoted discussion of water quality problems in…

Embedded 32-bit Differential Pulse Voltammetry (DPV) Technique for 3-electrode Cell Sensing

NASA Astrophysics Data System (ADS)

N, Aqmar N. Z.; Abdullah, W. F. H.; Zain, Z. M.; Rani, S.

2018-03-01

This paper addresses the development of differential pulse voltammetry (DPV) embedded algorithm using an ARM cortex processor with new developed potentiostat circuit design for in-situ 3-electrode cell sensing. This project is mainly to design a low cost potentiostat for the researchers in laboratories. It is required to develop an embedded algorithm for analytical technique to be used with the designed potentiostat. DPV is one of the most familiar pulse technique method used with 3-electrode cell sensing in chemical studies. Experiment was conducted on 10mM solution of Ferricyanide using the designed potentiostat and the developed DPV algorithm. As a result, the device can generate an excitation signal of DPV from 0.4V to 1.2V and produced a peaked voltammogram with relatively small error compared to the commercial potentiostat; which is only 6.25% difference in peak potential reading. The design of potentiostat device and its DPV algorithm is verified.

Improved Electrochemical Detection of Zinc Ions Using Electrode Modified with Electrochemically Reduced Graphene Oxide

PubMed Central

Kudr, Jiri; Richtera, Lukas; Nejdl, Lukas; Xhaxhiu, Kledi; Vitek, Petr; Rutkay-Nedecky, Branislav; Hynek, David; Kopel, Pavel; Adam, Vojtech; Kizek, Rene

2016-01-01

Increasing urbanization and industrialization lead to the release of metals into the biosphere, which has become a serious issue for public health. In this paper, the direct electrochemical reduction of zinc ions is studied using electrochemically reduced graphene oxide (ERGO) modified glassy carbon electrode (GCE). The graphene oxide (GO) was fabricated using modified Hummers method and was electrochemically reduced on the surface of GCE by performing cyclic voltammograms from 0 to −1.5 V. The modification was optimized and properties of electrodes were determined using electrochemical impedance spectroscopy (EIS) and cyclic voltammetry (CV). The determination of Zn(II) was performed using differential pulse voltammetry technique, platinum wire as a counter electrode, and Ag/AgCl/3 M KCl reference electrode. Compared to the bare GCE the modified GCE/ERGO shows three times better electrocatalytic activity towards zinc ions, with an increase of reduction current along with a negative shift of reduction potential. Using GCE/ERGO detection limit 5 ng·mL−1 was obtained. PMID:28787832

Biosynthesis of Bacterial Cellulose/Carboxylic Multi-Walled Carbon Nanotubes for Enzymatic Biofuel Cell Application

PubMed Central

Lv, Pengfei; Feng, Quan; Wang, Qingqing; Li, Guohui; Li, Dawei; Wei, Qufu

2016-01-01

Novel nanocomposites comprised of bacterial cellulose (BC) with carboxylic multi-walled carbon nanotubes (c-MWCNTs) incorporated into the BC matrix were prepared through a simple method of biosynthesis. The biocathode and bioanode for the enzyme biological fuel cell (EBFC) were prepared using BC/c-MWCNTs composite injected by laccase (Lac) and glucose oxidase (GOD) with the aid of glutaraldehyde (GA) crosslinking. Biosynthesis of BC/c-MWCNTs composite was characterized by digital photos, scanning electron microscope (SEM), and Fourier Transform Infrared (FTIR). The experimental results indicated the successful incorporation of c-MWCNTs into the BC. The electrochemical and biofuel performance were evaluated by cyclic voltammetry (CV) and linear sweep voltammetry (LSV). The power density and current density of EBFCs were recorded at 32.98 µW/cm3 and 0.29 mA/cm3, respectively. Additionally, the EBFCs also showed acceptable stability. Preliminary tests on double cells indicated that renewable BC have great potential in the application field of EBFCs. PMID:28773310

Electrocatalytic oxidation and voltammetric determination of ciprofloxacin employing poly(alizarin red)/graphene composite film in the presence of ascorbic acid, uric acid and dopamine.

PubMed

Zhang, Xin; Wei, Youli; Ding, Yaping

2014-07-04

A glassy carbon electrode modified with poly(alizarin red)/electrodeposited graphene (PAR/EGR) composite film was prepared and applied to detect ciprofloxacin (CPFX) in the presence of ascorbic, uric acid and dopamine. The morphology and interface property of PAR/EGR films were examined by scanning electron microscopy (SEM) and electrochemical impedance spectroscopy (EIS). The electrocatalytic oxidation of CPFX on AR/EGR was investigated by cyclic voltammetry (CV) and differential pulse voltammetry (DPV). The linearity ranged from 4 × 10(-8) to 1.2 × 10(-4) M with a detection limit (S/N=3) of 0.01 μM. The modified electrode could be applied to the individual determination of CPFX as well as the simultaneous determination of CPFX, ascorbic acid, uric acid and dopamine. This method proved to be a simple, selective and rapid way to determine CPFX in pharmaceutical preparation and biological media. Copyright © 2014. Published by Elsevier B.V.

Application of graphene oxide/lanthanum-modified carbon paste electrode for the selective determination of dopamine

NASA Astrophysics Data System (ADS)

Ye, Fengying; Feng, Chenqi; Fu, Ning; Wu, Huihui; Jiang, Jibo; Han, Sheng

2015-12-01

A home-made carbon paste electrode (CPE) was reformed by graphene oxide (GO)/lanthanum (La) complexes, and a modified electrode, called GO-La/CPE, was fabricated for the selective determination of dopamine (DA) by cyclic voltammetry (CV) and differential pulse voltammetry (DPV). Several factors affecting the electrocatalytic performance of the modified sensor were investigated. Owning to the combination of GO and La ions, the GO-La/CPE sensor exhibited large surface area, well selectivity, good repeatability and stability in the oxidation reaction of DA. At optimal conditions, the response of the GO-La/CPE electrode for determining DA was linear in the region of 0.01-0.1 μM and 0.1-400.0 μM. The limit of detection was down to 0.32 nM (S/N = 3). In addition, this modified electrode was successfully applied to the detection of DA in real urine and serum samples by using standard adding method, showing its promising application in the electroanalysis of real samples.

Access to enhanced differences in Marcus-Hush and Butler-Volmer electron transfer theories by systematic analysis of higher order AC harmonics.

PubMed

Stevenson, Gareth P; Baker, Ruth E; Kennedy, Gareth F; Bond, Alan M; Gavaghan, David J; Gillow, Kathryn

2013-02-14

The potential-dependences of the rate constants associated with heterogeneous electron transfer predicted by the empirically based Butler-Volmer and fundamentally based Marcus-Hush formalisms are well documented for dc cyclic voltammetry. However, differences are often subtle, so, presumably on the basis of simplicity, the Butler-Volmer method is generally employed in theoretical-experimental comparisons. In this study, the ability of Large Amplitude Fourier Transform AC Cyclic Voltammetry to distinguish the difference in behaviour predicted by the two formalisms has been investigated. The focus of this investigation is on the difference in the profiles of the first to sixth harmonics, which are readily accessible when a large amplitude of the applied ac potential is employed. In particular, it is demonstrated that systematic analysis of the higher order harmonic responses in suitable kinetic regimes provides predicted deviations of Marcus-Hush from Butler-Volmer behaviour to be established from a single experiment under conditions where the background charging current is minimal.

Enhanced activity of Au-Fe/C anodic electrocatalyst for direct borohydride-hydrogen peroxide fuel cell

NASA Astrophysics Data System (ADS)

Yi, Lanhua; Wei, Wei; Zhao, Caixian; Tian, Li; Liu, Jing; Wang, Xianyou

2015-07-01

Carbon supported Au-Fe bimetallic nanocatalysts (Au-Fe/C) are facilely prepared via a modified NaBH4 reduction method in aqueous solution at room temperature, and used as the anode electrocatalyst of direct borohydride-hydrogen peroxide fuel cell (DBHFC). The physical and electrochemical properties of the Au-Fe/C electrocatalysts are characterized by transmission electron microscopy (TEM), X-ray diffraction (XRD), cyclic voltammetry (CV), rotating disc electrode (RDE) voltammetry, chronoamperometry (CA), chronopotentiometry (CP), and fuel cell test. The results show that Au-Fe/C catalysts display higher catalytic activity for the direct electrooxidation of BH4- than carbon supported pure Au nanocatalyst (Au/C), especially Au50Fe50/C catalyst presents the highest catalytic activity among all as-prepared catalysts. Besides, the single DBHFC with Au50Fe50/C anode and Au/C cathode obtains the maximum power density as high as 34.9 mW cm-2 at 25 °C.

Mono-Mercury Doping of Au25 and the HOMO/LUMO Energies Evaluation Employing Differential Pulse Voltammetry.

PubMed

Liao, Lingwen; Zhou, Shiming; Dai, Yafei; Liu, Liren; Yao, Chuanhao; Fu, Cenfeng; Yang, Jinlong; Wu, Zhikun

2015-08-05

Controlling the bimetal nanoparticle with atomic monodispersity is still challenging. Herein, a monodisperse bimetal nanoparticle is synthesized in 25% yield (on gold atom basis) by an unusual replacement method. The formula of the nanoparticle is determined to be Au24Hg1(PET)18 (PET: phenylethanethiolate) by high-resolution ESI-MS spectrometry in conjunction with multiple analyses including X-ray photoelectron spectroscopy (XPS) and thermogravimetric analysis (TGA). X-ray single-crystal diffraction reveals that the structure of Au24Hg1(PET)18 remains the structural framework of Au25(PET)18 with one of the outer-shell gold atoms replaced by one Hg atom, which is further supported by theoretical calculations and experimental results as well. Importantly, differential pulse voltammetry (DPV) is first employed to estimate the highest occupied molecular orbit (HOMO) and the lowest unoccupied molecular orbit (LUMO) energies of Au24Hg1(PET)18 based on previous calculations.

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

PubMed

Bagheri, Akbar; Hosseini, Hadi

2012-12-01

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

Cyclic voltammetry to evaluate the antioxidant potential in winemaking by-products.

PubMed

José Jara-Palacios, M; Luisa Escudero-Gilete, M; Miguel Hernández-Hierro, J; Heredia, Francisco J; Hernanz, Dolores

2017-04-01

Grape pomace is composed of seeds, skins and stems that are an important source of phenolic substances, which have antioxidant properties and potential benefits to human health. Cyclic voltammetry (CV) has been used to measure the total antioxidant potential of different winemaking by-products. The electrochemical behavior of pomace, seeds, skins and stems was measured by CV and lipid peroxidation inhibition by thiobarbituric acid reactive substances (TBARS) method. Differences for the electrochemical parameter were found between the by-products, pomace and seeds, which presented the greatest voltammetric peak area. Furthermore, the by-products induced inhibition of lipid peroxidation in rat liver homogenates. Pomace and seeds showed higher capacity to inhibit lipid peroxidation than stems and skins, which could be because these by-products are richer in flavanols. Simple regression analyses showed that voltammetric parameters are highly correlated to the values obtained for lipid peroxidation inhibition. CV is a promising technique to estimate the total antioxidant potential of phenolic extract from winemaking by-products. Copyright © 2016 Elsevier B.V. All rights reserved.

Direct electrodeposition of gold nanotube arrays of rough and porous wall by cyclic voltammetry and its applications of simultaneous determination of ascorbic acid and uric acid.

PubMed

Yang, Guangming; Li, Ling; Jiang, Jinhe; Yang, Yunhui

2012-08-01

Gold nanotube arrays of rough and porous wall has been synthesized by direct electrodeposition with cyclic voltammetry utilizing anodic aluminum oxide template (AAO) and polycarbonate membrane (PC) during short time (only 3 min and 2 min, respectively). The mechanism of the direct electrodeposition of gold nanotube arrays by cyclic voltammetry (CV) has been discussed. The morphological characterizations of the gold nanotube arrays have been investigated by scanning electron microscopy (SEM). A simultaneous determination of ascorbic acid (AA) and uric acid (UA) by differential pulse voltammetry (DPV) was constructed by attaching gold nanotube arrays (using AAO) onto the surface of a glassy carbon electrode (GCE). The electrochemical behavior of AA and UA at this modified electrode has been studied by CV and differential pulse voltammetry (DPV). The sensor offers an excellent response for AA and UA and the linear response range for AA and UA were 1.02×10(-7)-5.23×10(-4) mol L(-1) and 1.43×10(-7)-4.64×10(-4) mol L(-1), the detection limits were 1.12×10(-8) mol L(-1) and 2.24×10(-8) mol L(-1), respectively. This sensor shows good regeneration, stability and selectivity and has been used for the determination of AA and UA in real human urine and serum samples with satisfied results. Copyright © 2012 Elsevier B.V. All rights reserved.

Real-time monitoring of electrically evoked catecholamine signals in the songbird striatum using in vivo fast-scan cyclic voltammetry.

PubMed

Smith, Amanda R; Garris, Paul A; Casto, Joseph M

2015-01-01

Fast-scan cyclic voltammetry is a powerful technique for monitoring rapid changes in extracellular neurotransmitter levels in the brain. In vivo fast-scan cyclic voltammetry has been used extensively in mammalian models to characterize dopamine signals in both anesthetized and awake preparations, but has yet to be applied to a non-mammalian vertebrate. The goal of this study was to establish in vivo fast-scan cyclic voltammetry in a songbird, the European starling, to facilitate real-time measurements of extracellular catecholamine levels in the avian striatum. In urethane-anesthetized starlings, changes in catecholamine levels were evoked by electrical stimulation of the ventral tegmental area and measured at carbon-fiber microelectrodes positioned in the medial and lateral striata. Catecholamines were elicited by different stimulations, including trains related to phasic dopamine signaling in the rat, and were analyzed to quantify presynaptic mechanisms governing exocytotic release and neuronal uptake. Evoked extracellular catecholamine dynamics, maximal amplitude of the evoked catecholamine signal, and parameters for catecholamine release and uptake did not differ between striatal regions and were similar to those determined for dopamine in the rat dorsomedial striatum under similar conditions. Chemical identification of measured catecholamine by its voltammogram was consistent with the presence of both dopamine and norepinephrine in striatal tissue content. However, the high ratio of dopamine to norepinephrine in tissue content and the greater sensitivity of the carbon-fiber microelectrode to dopamine compared to norepinephrine favored the measurement of dopamine. Thus, converging evidence suggests that dopamine was the predominate analyte of the electrically evoked catecholamine signal measured in the striatum by fast-scan cyclic voltammetry. Overall, comparisons between the characteristics of these evoked signals suggested a similar presynaptic regulation of dopamine in the starling and rat striatum. Fast-scan cyclic voltammetry thus has the potential to be an invaluable tool for investigating the neural underpinnings of behavior in birds. Copyright © 2015 Elsevier B.V. All rights reserved.

Real-time monitoring of electrically evoked catecholamine signals in the songbird striatum using in vivo fast-scan cyclic voltammetry

PubMed Central

Smith, Amanda R.; Garris, Paul A.; Casto, Joseph M.

2015-01-01

Fast-scan cyclic voltammetry is a powerful technique for monitoring rapid changes in extracellular neurotransmitter levels in the brain. In vivo fast-scan cyclic voltammetry has been used extensively in mammalian models to characterize dopamine signals in both anesthetized and awake preparations, but has yet to be applied to a non-mammalian vertebrate. The goal of this study was to establish in vivo fast-scan cyclic voltammetry in a songbird, the European starling, to facilitate real-time measurements of extracellular catecholamine levels in the avian striatum. In urethane-anesthetized starlings, changes in catecholamine levels were evoked by electrical stimulation of the ventral tegmental area and measured at carbon-fiber microelectrodes positioned in the medial and lateral striata. Catecholamines were elicited by different stimulations, including trains related to phasic dopamine signaling in the rat, and were analyzed to quantify presynaptic mechanisms governing exocytotic release and neuronal uptake. Evoked extracellular catecholamine dynamics, maximal amplitude of the evoked catecholamine signal, and parameters for catecholamine release and uptake did not differ between striatal regions and were similar to those determined for dopamine in the rat dorsomedial striatum under similar conditions. Chemical identification of measured catecholamine by its voltammogram was consistent with the presence of both dopamine and norepinephrine in striatal tissue content. However, the high ratio of dopamine to norepinephrine in tissue content and the greater sensitivity of the carbon-fiber microelectrode to dopamine compared to norepinephrine favored the measurement of dopamine. Thus, converging evidence suggests that dopamine was the predominate analyte of the electrically evoked catecholamine signal measured in the striatum by fast-scan cyclic voltammetry. Overall, comparisons between the characteristics of these evoked signals suggested a similar presynaptic regulation of dopamine in the starling and rat striatum. Fast-scan cyclic voltammetry thus has the potential to be an invaluable tool for investigating the neural underpinnings of behavior in birds. PMID:25900708

Voltammetric determination of arsenic in high iron and manganese groundwaters.

PubMed

Gibbon-Walsh, Kristoff; Salaün, Pascal; Uroic, M Kalle; Feldmann, Joerg; McArthur, John M; van den Berg, Constant M G

2011-09-15

Determination of the speciation of arsenic in groundwaters, using cathodic stripping voltammetry (CSV), is severely hampered by high levels of iron and manganese. Experiments showed that the interference is eliminated by addition of EDTA, making it possible to determine the arsenic speciation on-site by CSV. This work presents the CSV method to determine As(III) in high-iron or -manganese groundwaters in the field with only minor sample treatment. The method was field-tested in West-Bengal (India) on a series of groundwater samples. Total arsenic was subsequently determined after acidification to pH 1 by anodic stripping voltammetry (ASV). Comparative measurements by ICP-MS as reference method for total As, and by HPLC for its speciation, were used to corroborate the field data in stored samples. Most of the arsenic (78±0.02%) was found to occur as inorganic As(III) in the freshly collected waters, in accordance with previous studies. The data shows that the modified on-site CSV method for As(III) is a good measure of water contamination with As. The EDTA was also found to be effective in stabilising the arsenic speciation for longterm sample storage at room temperature. Without sample preservation, in water exposed to air and sunlight, the As(III) was found to become oxidised to As(V), and Fe(II) oxidised to Fe(III), removing the As(V) by adsorption on precipitating Fe(III)-hydroxides within a few hours. Copyright © 2011 Elsevier B.V. All rights reserved.

Development of electrochemical sensors for trace detection of explosives and for the detection of chemical warfare agents

NASA Astrophysics Data System (ADS)

Berger, T.; Ziegler, H.; Krausa, Michael

2000-08-01

A huge number of chemical sensors are based on electrochemical measurement methods. Particularly amperometric sensorsystems are employed for the fast detection of pollutants in industry and environment as well as for analytic systems in the medical diagnosis. The large number of different applications of electrochemical sensors is based on the high sensitivity of electrochemical methods and on the wide of possibilities to enhance the selectivity by variation of electrochemical and chemical parameters. Besides this, electrochemical sensorsystems are frequently simple to operate, transportable and cheap. Up to now the electrochemical method of cyclic voltammetry is used only seldom for sensors. Clearly the efficiency of cyclic voltammetry can be seen at the sensorsystem for the detection of nitro- and aminotoluenes in solids and waters as presented here. The potentiodynamic sensors system can be employed for the fast and easy risk estimation of contaminated areas. Because of the high sensitivity of electrochemical methods the detection of chemical substances with a low vapor pressure is possible also. The vapor pressure of TNT at room temperature is 7 ppb for instances. With a special electrochemical set-up we were able to measure TNT approximately 10 cm above a TNT-sample. In addition we were able to estimate TNT in the gaseous phase approximately 10 cm above a real plastic mine. Therefore it seems to be possible to develop an electrochemical mien detection. Moreover, we present that the electrochemical detection of RDX, HMX and chemical warfare agents is also possible.

Electrochemical detection of a powerful estrogenic endocrine disruptor: ethinylestradiol in water samples through bioseparation procedure.

PubMed

Martínez, Noelia A; Pereira, Sirley V; Bertolino, Franco A; Schneider, Rudolf J; Messina, Germán A; Raba, Julio

2012-04-20

The synthetic estrogen ethinylestradiol (EE2) is an active component of oral contraceptives (OCs), considered as an endocrine disrupting compound (EDC). It is excreted from humans and released via sewage treatment plant effluents into aquatic environments. EDCs are any environmental pollutant chemical that, once incorporated into an organism, affects the hormonal balance of various species including humans. Its presence in the environment is becoming of great importance in water quality. This paper describes the development of an accurate, sensitive and selective method for capture, preconcentration and determination of EE2 present in water samples using: magnetic particles (MPs) as bioaffinity support for the capture and preconcentration of EE2 and a glassy carbon electrode modified with multi-walled carbon nanotubes (MWCNTs/GCE) as detection system. The capture procedure was based on the principle of immunoaffinity, the EE2 being extracted from the sample using the anti-EE2 antibodies (anti-EE2 Ab) which were previously immobilized on MPs. Subsequently the analyte desorption was done employing a sulfuric acid solution and the determination of the EE2 in the pre-concentrated solution was carried out by square wave voltammetry (SWV). This method can be used to determine EE2 in the range of 0.035-70 ng L(-1) with a detection limit (LOD) of 0.01 ng L(-1) and R.S.D.<4.20%. The proposed method has been successfully applied to the determination of EE2 in water samples and it has promising analytical applications for the direct determination of EE2 at trace levels. Copyright © 2012 Elsevier B.V. All rights reserved.

Electrochemical Quantification of Extracellular Local H2O2 Kinetics Originating from Single Cells.

PubMed

Bozem, Monika; Knapp, Phillip; Mirčeski, Valentin; Slowik, Ewa J; Bogeski, Ivan; Kappl, Reinhard; Heinemann, Christian; Hoth, Markus

2017-05-15

H 2 O 2 is produced by all eukaryotic cells under physiological and pathological conditions. Due to its enormous relevance for cell signaling at low concentrations and antipathogenic function at high concentrations, precise quantification of extracellular local H 2 O 2 concentrations ([H 2 O 2 ]) originating from single cells is required. Using a scanning electrochemical microscope and bare platinum disk ultramicroelectrodes, we established sensitive long-term measurements of extracellular [H 2 O 2 ] kinetics originating from single primary human monocytes (MCs) ex vivo. For the electrochemical techniques square wave voltammetry, cyclic and linear scan voltammetry, and chronoamperometry, detection limits for [H 2 O 2 ] were determined to be 5, 50, and 500 nM, respectively. Following phorbol ester stimulation, local [H 2 O 2 ] 5-8 μm above a single MC increased by 3.4 nM/s within the first 10 min before reaching a plateau. After extracellular addition of H 2 O 2 to an unstimulated MC, the local [H 2 O 2 ] decreased on average by 4.2 nM/s due to degradation processes of the cell. Using the scanning mode of the setup, we found that H 2 O 2 is evenly distributed around the producing cell and can still be detected up to 30 μm away from the cell. The electrochemical single-cell measurements were validated in MC populations using electron spin resonance spectroscopy and the Amplex ® UltraRed assay. Innovation and Conclusion: We demonstrate a highly sensitive, spatially, and temporally resolved electrochemical approach to monitor dynamics of production and degradation processes for H 2 O 2 separately. Local extracellular [H 2 O 2 ] kinetics originating from single cells is quantified in real time. Antioxid. Redox Signal. 00, 000-000.

Hydrogen Bonding Rescues Overpotential in Seven-Coordinated Ru Water Oxidation Catalysts

DOE PAGES

Matheu, Roc; Ertem, Mehmed Z.; Gimbert-Surinach, Carolina; ...

2017-08-15

In this paper, we describe the synthesis, structural characterization, and redox properties of two new Ru complexes containing the dianionic potentially pentadentate [2,2':6',2"-terpyridine]-6,6"-dicarboxylate (tda 2–) ligand that coordinates Ru at the equatorial plane and with additional pyridine or dmso acting as monondentate ligand in the axial positions: [Ru II(tda-κ-N 3O)(py)(dmso)], 1 II and [Ru III(tda-κ-N 3O 2)(py)(H 2O) ax] +, 2 III(H 2O) +. Complex 1 II has been characterized by single-crystal XRD in the solid state and in solution by NMR spectroscopy. The redox properties of 1 II and 2 III(H 2O) + have been thoroughly investigated by meansmore » of cyclic voltammetry and differential pulse voltammetry. Complex 2 II(H 2O) displays poor catalytic activity with regard to the oxidation of water to dioxygen, and its properties have been analyzed on the basis of foot of the wave analysis and catalytic Tafel plots. The activity of 2 II(H 2O) has been compared with related water oxidation catalysts (WOCs) previously described in the literature. Despite its moderate activity, 2 II(H 2O) constitutes the cornerstone that has triggered the rationalization of the different factors that govern overpotentials as well as efficiencies in molecular WOCs. The present work uncovers the interplay between different parameters, namely, coordination number, number of anionic groups bonded to the first-coordination sphere of the metal center, water oxidation catalysis overpotential, p K a and hydrogen bonding, and the performance of a given WOC. It thus establishes the basic principles for the design of efficient WOCs operating at low overpotentials.« less

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

PubMed

Huang, Hsin-Yi; Chen, Po-Yu

2010-12-15

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

Electrodeposited nanostructured MnO{sub 2} for non-enzymatic hydrogen peroxide sensing

DOE Office of Scientific and Technical Information (OSTI.GOV)

Saha, B., E-mail: barnamala.saha@gmail.com; Jana, S. K.; Banerjee, S.

2015-06-24

Electrodeposited MnO{sub 2} nanostructure was synthesized on indium tin oxide coated glass electrode by cyclic voltammetry. The as obtained samples were subsequently characterized by atomic force microscopy and their electro-catalytic response towards hydrogen peroxide in alkaline medium of 0.1M NaOH was studied using cyclic voltammetry and amperometry.

Exfoliated, Nitrogen-Doped Graphene Nanosheet Cathode for Lithium-Oxygen Batteries

DTIC Science & Technology

2014-06-01

scanning electron microscopy; oxygen reduction reaction; cyclic voltammetry ; lithium-oxygen battery. Introduction The continuous...77 K (Micromeritics ASAP 2020). The porosity of cathode material was characterized by a gas pycnometer (Micromeritis, Accu Pyc II 1340). Cyclic ... voltammetry (CV) and galvanostatic charge-discharge measurements of the specimens were conducted using a computer controlled VersaSTAT 4 (Princeton

Instrumentation for fast-scan cyclic voltammetry combined with electrophysiology for behavioral experiments in freely moving animals

NASA Astrophysics Data System (ADS)

Takmakov, Pavel; McKinney, Collin J.; Carelli, Regina M.; Wightman, R. Mark

2011-07-01

Fast-scan cyclic voltammetry is a unique technique for sampling dopamine concentration in the brain of rodents in vivo in real time. The combination of in vivo voltammetry with single-unit electrophysiological recording from the same microelectrode has proved to be useful in studying the relationship between animal behavior, dopamine release and unit activity. The instrumentation for these experiments described here has two unique features. First, a 2-electrode arrangement implemented for voltammetric measurements with the grounded reference electrode allows compatibility with electrophysiological measurements, iontophoresis, and multielectrode measurements. Second, we use miniaturized electronic components in the design of a small headstage that can be fixed on the rat's head and used in freely moving animals.

Instrumentation for fast-scan cyclic voltammetry combined with electrophysiology for behavioral experiments in freely moving animals

PubMed Central

Takmakov, Pavel; McKinney, Collin J.; Carelli, Regina M.; Wightman, R. Mark

2011-01-01

Fast-scan cyclic voltammetry is a unique technique for sampling dopamine concentration in the brain of rodents in vivo in real time. The combination of in vivo voltammetry with single-unit electrophysiological recording from the same microelectrode has proved to be useful in studying the relationship between animal behavior, dopamine release and unit activity. The instrumentation for these experiments described here has two unique features. First, a 2-electrode arrangement implemented for voltammetric measurements with the grounded reference electrode allows compatibility with electrophysiological measurements, iontophoresis, and multielectrode measurements. Second, we use miniaturized electronic components in the design of a small headstage that can be fixed on the rat's head and used in freely moving animals. PMID:21806203

Method development for the determination of arsenic by sequential injection/anodic stripping voltammetry using long-lasting gold-modified screen-printed carbon electrode.

PubMed

Punrat, Eakkasit; Chuanuwatanakul, Suchada; Kaneta, Takashi; Motomizu, Shoji; Chailapakul, Orawon

2013-11-15

An automated method has been developed for determining the concentration of inorganic arsenic. The technique uses sequential injection/anodic stripping voltammetry with a long-lasting gold-modified screen-printed carbon electrode. The long-lasting gold electrode was electrochemically deposited onto a screen-printed carbon electrode at a potential of -0.5 V vs. Ag/AgCl in a supporting electrolyte solution of 1M hydrochloric acid. Under optimal conditions and the applied potentials, the electrode demonstrated that it can be used for a long time without a renewal process. The linear range for the determination of arsenic(III) was 1-100 μg L(-1), and the limit of detection (LOD) in standard solutions was as low as 0.03 μg L(-1) for a deposition time of 120 s and sample volume of 1 mL. This method was used to determine the concentration of arsenic(III) in water samples with satisfactory results. The LOD in real samples was found to be 0.5 μg L(-1). In addition, speciation between arsenic(III) and arsenic(V) has been achieved with the proposed method using deposition potentials of -0.5 V and -1.5 V for the determination of the arsenic(III) concentration and the total arsenic concentration, respectively; the results were acceptable. The proposed method is an automated system that offers a less expensive alternative for determining trace amounts of inorganic arsenic. © 2013 Elsevier B.V. All rights reserved.

Copper Sensing in Alkaline Electrolyte Using Anodic Stripping Voltammetry by Means of a Lead Mediator

DOE PAGES

Duay, Jonathon; Ortiz-Santiago, Joed E.; Lambert, Timothy N.

2017-10-05

Anodic stripping voltammetry (ASV) is an analysis technique that permits the selective and quantitative analysis of metal ion species in solution. It is most commonly applied in neutral to acidic electrolyte largely due to inherent metal ion solubility. Bismuth (Bi) is a common film used for ASV due to its good sensitivity, overall stability and insensitivity to O2. ASV, utilizing a Bi film, along with cadmium (Cd) and lead (Pb) as the plating mediators, has recently been adapted to determine zinc (Zn) concentrations in highly alkaline environments (30 % NaOH or 35 % M KOH). Successful analysis of Zn inmore » alkaline relies on the ability of the hydroxide to form soluble metal anion species, such as Bi(OH) 4 – and Zn(OH) 4 2–. Here, we look to extend this technique to detect and quantify copper (Cu) ions in these highly basic electrolytes. However, in general, the use of ASV to detect and quantify Cu ion concentrations is notoriously difficult as the Cu stripping peak potential overlays with that of Bi from the common Bi film electrode. Here, an ASV method for determining Cu concentration in alkaline solutions is developed utilizing Pb as a deposition mediator. As such, it was found that when analyzing Cu solutions in the presence of Pb, the stripping voltammetry curves present separate and defined Cu stripping peaks. Different analyzes were made to find the best stripping voltammetry performance conditions. As such, an accumulation time of 5 minutes, an accumulation potential of ≤–1.45 V vs. Hg/HgO, and a concentration of 35 wt% KOH were determined to be the conditions that presented the best ASV results. Utilizing these conditions, calibration curves in the presence of 5.0 ppm Pb showed the best linear stripping signal correlation with an r-squared value of 0.991 and a limit of detection (LOD) of 0.67 ppm. Lastly, these results give way to evaluating Cu concentrations using ASV in aqueous alkaline solutions.« less

Copper Sensing in Alkaline Electrolyte Using Anodic Stripping Voltammetry by Means of a Lead Mediator

DOE Office of Scientific and Technical Information (OSTI.GOV)

Duay, Jonathon; Ortiz-Santiago, Joed E.; Lambert, Timothy N.

Anodic stripping voltammetry (ASV) is an analysis technique that permits the selective and quantitative analysis of metal ion species in solution. It is most commonly applied in neutral to acidic electrolyte largely due to inherent metal ion solubility. Bismuth (Bi) is a common film used for ASV due to its good sensitivity, overall stability and insensitivity to O2. ASV, utilizing a Bi film, along with cadmium (Cd) and lead (Pb) as the plating mediators, has recently been adapted to determine zinc (Zn) concentrations in highly alkaline environments (30 % NaOH or 35 % M KOH). Successful analysis of Zn inmore » alkaline relies on the ability of the hydroxide to form soluble metal anion species, such as Bi(OH) 4 – and Zn(OH) 4 2–. Here, we look to extend this technique to detect and quantify copper (Cu) ions in these highly basic electrolytes. However, in general, the use of ASV to detect and quantify Cu ion concentrations is notoriously difficult as the Cu stripping peak potential overlays with that of Bi from the common Bi film electrode. Here, an ASV method for determining Cu concentration in alkaline solutions is developed utilizing Pb as a deposition mediator. As such, it was found that when analyzing Cu solutions in the presence of Pb, the stripping voltammetry curves present separate and defined Cu stripping peaks. Different analyzes were made to find the best stripping voltammetry performance conditions. As such, an accumulation time of 5 minutes, an accumulation potential of ≤–1.45 V vs. Hg/HgO, and a concentration of 35 wt% KOH were determined to be the conditions that presented the best ASV results. Utilizing these conditions, calibration curves in the presence of 5.0 ppm Pb showed the best linear stripping signal correlation with an r-squared value of 0.991 and a limit of detection (LOD) of 0.67 ppm. Lastly, these results give way to evaluating Cu concentrations using ASV in aqueous alkaline solutions.« less

Rapid Two-Millisecond Interrogation of Electrochemical, Aptamer-Based Sensor Response Using Intermittent Pulse Amperometry.

PubMed

Santos-Cancel, Mirelis; Lazenby, Robert A; White, Ryan J

2018-06-22

In this manuscript, we employ the technique intermittent pulse amperometry (IPA) to interrogate equilibrium and kinetic target binding to the surface of electrochemical, aptamer-based (E-AB) sensors, achieving as fast as 2 ms time resolution. E-AB sensors comprise an electrode surface modified with a flexible nucleic acid aptamer tethered at the 3'-terminus with a redox-active molecule. The introduction of a target changes the conformation and flexibility of the nucleic acid, which alters the charge transfer rate of the appended redox molecule. Typically, changes in charge transfer rate within this class of sensor are monitored via voltammetric methods. Here, we demonstrate that the use of IPA enables the detection of changes in charge transfer rates (i.e., current) at times <100 μs after the application of a potential pulse. Changes in sensor current are quantitatively related to target analyte concentration and can be used to create binding isotherms. Furthermore, the application of IPA enables rapid probing of the electrochemical surface with a time resolution equivalent to as low as twice the applied potential pulse width, not previously demonstrated with traditional voltammetric techniques employed with E-AB sensors (alternating current, square wave, cyclic). To visualize binding, we developed false-color plots analogous to those used in the field of fast-scan cyclic voltammetry. The use of IPA is universal, as demonstrated with two representative small molecule E-AB sensors directed against the aminoglycoside antibiotic tobramycin and adenosine triphosphate (ATP). Intermittent pulse amperometry exhibits an unprecedented sub-microsecond temporal response and is a general method for measuring rapid sensor performance.

Enzymatic biosensors based on ingá-cipó peroxidase immobilised on sepiolite for TBHQ quantification.

PubMed

Regina de Oliveira, Tássia; Grawe, Gregory Ferreira; Moccelini, Sally Katiuce; Terezo, Ailton J; Castilho, Marilza

2014-05-07

Sepiolite clay mineral was used as a support for the immobilisation of the peroxidase enzyme from ingá-cipó (Inga edulis Mart.) and was used with graphite powder, multi-walled carbon nanotubes (CNTs), mineral oil, and nafion 0.5% (v/v) in the development of a new biosensor for the determination of the antioxidant tert-butylhydroquinone (TBHQ) by square-wave voltammetry (SWV). For the optimisation and application of the biosensor, several parameters were investigated to determine the optimum experimental conditions using SWV. The best performance was obtained using a 0.1 mol L(-1) phosphate buffer solution (pH 7.0), 4.0 × 10(-4) mol L(-1) hydrogen peroxide, a frequency of 50 Hz, a pulse amplitude of 60 mV, and a scan increment of 6 mV. The biosensor showed good repeatability and reproducibility and remained stable for a period of 20 weeks. The analytical curve revealed a linear response range of 1.65 to 9.82 mg L(-1) (r = 0.994) with detection and quantification limits of 0.41 and 1.25 mg L(-1). A recovery study of TBHQ in salad dressing samples yielded values from 99.6-104.8%. The proposed biosensor was successfully used for the determination of TBHQ in commercial salad dressing samples, giving a relative error of 5.4% in relation to the comparative method (chromatographic).

Spectroelectrochemistry and Electrochemistry of Europium Ions in Alkali Chloride Melts

NASA Astrophysics Data System (ADS)

Uehara, Akihiro; Shirai, Osamu; Nagai, Takayuki; Fujii, Toshiyuki; Yamana, Hajimu

2007-04-01

In order to investigate the redox equilibrium of europium ions in molten NaCl-2CsCl, UV-Vis absorption spectrophotometry measurements were performed for Eu2+ and Eu3+ in molten NaCl- 2CsCl at 923 K under simultaneous electrolytic control of their ratio. Molar absorptivities of EuCl3 and EuCl2 in NaCl-2CsCl at 923 K were determined to be (420±21) M -1cm-1 at 31200 cm-1 and (1130±56) M-1cm-1 at 30300 cm-1, respectively. The formal redox potential of the Eu2+/Eu3+ couple in NaCl-2CsCl melt at 923 K was determined to be (-0.941 ±0.004) V vs. Cl2/Cl- by electromotive force measurements on varying concentration ratios of Eu2+ and Eu3+, which were performed using a technique based on the combination of electrolysis and spectrophotometry. Cyclic voltammetry was also carried out in order to examine the characteristics of the voltammograms for the Eu2+/Eu3+ couple in NaCl-2CsCl melt. The formal redox potential of the Eu2+/Eu3+ couple determined by a spectroelectrochemical method agreed with that determined by cyclic voltammetry [(-0.946±0.008) V vs. Cl2/Cl-]. The effects of temperature on the redox potential of the Eu2+/Eu3+ couple in NaCl-2CsCl, NaCl-KCl, LiCl-KCl, and CsCl melts were studied by cyclic voltammetry in the range from 923 to 1123 K.

Probing Electrode Heterogeneity Using Fourier-Transformed Alternating Current Voltammetry: Application to a Dual-Electrode Configuration.

PubMed

Tan, Sze-Yin; Unwin, Patrick R; Macpherson, Julie V; Zhang, Jie; Bond, Alan M

2017-03-07

Quantitative studies of electron transfer processes at electrode/electrolyte interfaces, originally developed for homogeneous liquid mercury or metallic electrodes, are difficult to adapt to the spatially heterogeneous nanostructured electrode materials that are now commonly used in modern electrochemistry. In this study, the impact of surface heterogeneity on Fourier-transformed alternating current voltammetry (FTACV) has been investigated theoretically under the simplest possible conditions where no overlap of diffusion layers occurs and where numerical simulations based on a 1D diffusion model are sufficient to describe the mass transport problem. Experimental data that meet these requirements can be obtained with the aqueous [Ru(NH 3 ) 6 ] 3+/2+ redox process at a dual-electrode system comprised of electrically coupled but well-separated glassy carbon (GC) and boron-doped diamond (BDD) electrodes. Simulated and experimental FTACV data obtained with this electrode configuration, and where distinctly different heterogeneous charge transfer rate constants (k 0 values) apply at the individual GC and BDD electrode surfaces, are in excellent agreement. Principally, because of the far greater dependence of the AC current magnitude on k 0 , it is straightforward with the FTACV method to resolve electrochemical heterogeneities that are ∼1-2 orders of magnitude apart, as applies in the [Ru(NH 3 ) 6 ] 3+/2+ dual-electrode configuration experiments, without prior knowledge of the individual kinetic parameters (k 0 1 and k 0 2 ) or the electrode size ratio (θ 1 :θ 2 ). In direct current voltammetry, a difference in k 0 of >3 orders of magnitude is required to make this distinction.

Report on Contract W911NF-05-1-0339 (Clarkson University)

DTIC Science & Technology

2012-11-30

voltammetry and impedance spectroscopy: voltage dependent parameters of a silicon solar cell under controlled illumination and temperature, Energy...voltammetry for quantitative evaluation of temperature and voltage dependent parameters of a silicon solar cell , Solar Energy, (11 2011): 0. doi: 10.1016...characterization of silicon solar cells in the electro-analytical approach: Combined measurements of temperature and voltage dependent electrical

A highly sensitive and selective electrochemical sensor for determination of Cr(VI) in the presence of Cr(III) using modified multi-walled carbon nanotubes/quercetin screen-printed electrode.

PubMed

Sadeghi, Susan; Garmroodi, Aziz

2013-12-01

A novel screen-printed carbon electrode modified with quercetin/multi-walled carbon nanotubes was fabricated for determination of Cr(VI) in the presence of excess of Cr(III) without any pretreatment. The method is based on accumulation of the quercetin-Cr(III) complex generated in situ from Cr(VI) at the modified electrode surface in an open circuit followed by differential pulse voltammetry detection. The new method allowed selective determination of Cr(VI) in the presence of Cr(III). The influence of various parameters affecting the adsorptive stripping voltammetry performance was investigated. Under the optimum conditions, the calibration plot was found to be linear in the Cr(VI) concentration range from 1.0 to 200 μmol(-1) with a limit of detection(S/N=3) of 0.3 μmol L(-1). The relative standard deviation (RSD%) of seven replicates of the current measurements for a 50 μmol(-1) of Cr(VI) solution was 3.0%. The developed electrode displayed a very low or no sensitivity to alkali, alkali-earth and transition metal cations and was successfully applied for the determination of Cr(VI) in drinking water samples. © 2013.

[Investigation on simultaneous determination of dihydroxybenzene isomers in water samples using multi-walled carbon nanotube modified screen-printed electrode].

PubMed

Li, Yuan-Ting; Li, Da-Wei; Song, Wei; Long, Yi-Tao

2011-02-01

A disposable electrode, multi-walled carbon nanotube modified screen printed electrode (MWCNT/SPE), had been fabricated using screen printing technology and drop-coating method to determine dihydroxybenzene isomers (hydroquinone, catechol and resorcinol). The cyclic voltammetry behavior of dihydroxybenzene isomers had been investigated with the MWCNT/SPE. The results reveal that MWCNT/SPE, which shows a strong electrocatalytic activity for the oxidation of dihydroxybenzenes, can entirely separate the oxidation peaks of them. According to differential pulse voltammetry tests, the peak currents of dihydroxybenzene isomers are linear to their concentrations at the range of 8.20 x 10(-6) -1.00 x 10(-3), 8.20 x 10(-6) -1.00 x 10(-3) and 1.64 x 10(-5) -1.16 x 10(-3) mol x L(-1), with the detection limits of 4.34 x 10(-6), 3.42 x 10(-6) and 6.70 x 10(-6) mol x L(-1) for hydroquinone, catechol and resorcinol, respectively. For the determination of dihydroxybenzene isomers in water samples, the value of recovery found by standard addition method was in the range of 96.2%-104.9%. These results indicate MWCNT/SPE can be applied to rapid in-situ determination of dihydroxybenzenes-polluted water samples.

Investigation on Electrochemical Properties of Polythiophene Nanocomposite with Graphite Derivatives as Supercapacitor Material on Breath Figure-Decorated PMMA Electrode

NASA Astrophysics Data System (ADS)

Azimi, Mona; Abbaspour, Mohsen; Fazli, Ali; Setoodeh, Hamideh; Pourabbas, Behzad

2018-03-01

Breath figures have been formed by the direct breath figure method on polymethyl methacrylate electrode sand hexagonal oriented holes with 0.5- to 10- μm2 surface area have been created. Deposition of materials on the electrodes has been performed by the spray-coating method. polythiophene (PTh) nanoparticles, polythiophene-graphene oxide (PTh-GO) and polythiophene-reduced graphene oxide (PTh-G) nanocomposites were synthesized by emulsion polymerization, while characterization of synthetic materials have been carried out by Fourier transform infrared, Χ-ray diffraction, transmission electron microscopy, UV-Vis spectroscopy and field emission scanning electron microscopy techniques. Also, the electrochemical properties of the designed electrodes were investigated by cyclic voltammetry, galvanostatic charge-discharge and electrochemical impedance spectroscopy techniques. Specific capacitance of porous electrodes coated by PTh nanoparticles, PTh-GO and PTh-G nanocomposites were calculated from cyclic voltammetry curves at 5 mV/s scan rate, andthe values are 3.5 F/g, 16.39 F/g, and 28.68 F/g, respectively. Also, the energy density of each electrode at 5 mV/s scan rate has been calculated and the results show that incorporation of GO and G nanolayers with PTh nanoparticles enhances the electrochemical properties of electrodes.

Electrochemical properties and electrocatalytic activity of conducting polymer/copper nanoparticles supported on reduced graphene oxide composite

NASA Astrophysics Data System (ADS)

Ehsani, Ali; Jaleh, Babak; Nasrollahzadeh, Mahmoud

2014-07-01

Reduced graphene oxide (rGO) was used to support Cu nanoparticles. As electro-active electrodes for supercapacitors composites of reduced graphene oxide/Cu nanoparticles (rGO/CuNPs) and polytyramine (PT) with good uniformity are prepared by electropolymerization. Composite of rGO/CuNPs-PT was synthesized by cyclic voltammetry (CV) methods and electrochemical properties of film were investigated by using electrochemical techniques. The results show that, the rGO/CuNPs-PT/G has better capacitance performance. This is mainly because of the really large surface area and the better electronic and ionic conductivity of rGO/CuNPs-PT/G, which lead to greater double-layer capacitance and faradic pseudo capacitance. Modified graphite electrodes (rGO/CuNPs-PT/G) were examined for their redox process and electrocatalytic activities towards the oxidation of methanol in alkaline solutions. The methods of cyclic voltammetry (CV), chronoamperometry (CA) and electrochemical impedance spectroscopy (EIS) were employed. In comparison with a Cu-PT/G (Graphite), rGO/CuNPs-PT/G modified electrode shows a significantly higher response for methanol oxidation. A mechanism based on the electro-chemical generation of Cu(III) active sites and their subsequent consumptions by methanol have been discussed.

Fast Selective Detection of Pyocyanin Using Cyclic Voltammetry

PubMed Central

Alatraktchi, Fatima AlZahra’a; Breum Andersen, Sandra; Krogh Johansen, Helle; Molin, Søren; Svendsen, Winnie E.

2016-01-01

Pyocyanin is a virulence factor uniquely produced by the pathogen Pseudomonas aeruginosa. The fast and selective detection of pyocyanin in clinical samples can reveal important information about the presence of this microorganism in patients. Electrochemical sensing of the redox-active pyocyanin is a route to directly quantify pyocyanin in real time and in situ in hospitals and clinics. The selective quantification of pyocyanin is, however, limited by other redox-active compounds existing in human fluids and by other metabolites produced by pathogenic bacteria. Here we present a direct selective method to detect pyocyanin in a complex electroactive environment using commercially available electrodes. It is shown that cyclic voltammetry measurements between −1.0 V to 1.0 V reveal a potential detection window of pyocyanin of 0.58–0.82 V that is unaffected by other redox-active interferents. The linear quantification of pyocyanin has an R2 value of 0.991 across the clinically relevant concentration range of 2–100 µM. The proposed method was tested on human saliva showing a standard deviation of 2.5% ± 1% (n = 5) from the known added pyocyanin concentration to the samples. This inexpensive procedure is suggested for clinical use in monitoring the presence and state of P. aeruginosa infection in patients. PMID:27007376

Fast Selective Detection of Pyocyanin Using Cyclic Voltammetry.

PubMed

Alatraktchi, Fatima AlZahra'a; Andersen, Sandra Breum; Johansen, Helle Krogh; Molin, Søren; Svendsen, Winnie E

2016-03-19

Pyocyanin is a virulence factor uniquely produced by the pathogen Pseudomonas aeruginosa. The fast and selective detection of pyocyanin in clinical samples can reveal important information about the presence of this microorganism in patients. Electrochemical sensing of the redox-active pyocyanin is a route to directly quantify pyocyanin in real time and in situ in hospitals and clinics. The selective quantification of pyocyanin is, however, limited by other redox-active compounds existing in human fluids and by other metabolites produced by pathogenic bacteria. Here we present a direct selective method to detect pyocyanin in a complex electroactive environment using commercially available electrodes. It is shown that cyclic voltammetry measurements between -1.0 V to 1.0 V reveal a potential detection window of pyocyanin of 0.58-0.82 V that is unaffected by other redox-active interferents. The linear quantification of pyocyanin has an R² value of 0.991 across the clinically relevant concentration range of 2-100 µM. The proposed method was tested on human saliva showing a standard deviation of 2.5% ± 1% (n = 5) from the known added pyocyanin concentration to the samples. This inexpensive procedure is suggested for clinical use in monitoring the presence and state of P. aeruginosa infection in patients.

Cyclic voltammetry modeling of proton transport effects on redox charge storage in conductive materials: application to a TiO2 mesoporous film.

PubMed

Kim, Y S; Balland, V; Limoges, B; Costentin, C

2017-07-21

Cyclic voltammetry is a particularly useful tool for characterizing charge accumulation in conductive materials. A simple model is presented to evaluate proton transport effects on charge storage in conductive materials associated with a redox process coupled with proton insertion in the bulk material from an aqueous buffered solution, a situation frequently encountered in metal oxide materials. The interplay between proton transport inside and outside the materials is described using a formulation of the problem through introduction of dimensionless variables that allows defining the minimum number of parameters governing the cyclic voltammetry response with consideration of a simple description of the system geometry. This approach is illustrated by analysis of proton insertion in a mesoporous TiO 2 film.

An experimental comparison of the Marcus-Hush and Butler-Volmer descriptions of electrode kinetics applied to cyclic voltammetry. The one electron reductions of europium (III) and 2-methyl-2-nitropropane studied at a mercury microhemisphere electrode

NASA Astrophysics Data System (ADS)

Henstridge, Martin C.; Wang, Yijun; Limon-Petersen, Juan G.; Laborda, Eduardo; Compton, Richard G.

2011-11-01

We present a comparative experimental evaluation of the Butler-Volmer and Marcus-Hush models using cyclic voltammetry at a microelectrode. Numerical simulations are used to fit experimental voltammetry of the one electron reductions of europium (III) and 2-methyl-2-nitropropane, in water and acetonitrile, respectively, at a mercury microhemisphere electrode. For Eu (III) very accurate fits to experiment were obtained over a wide range of scan rates using Butler-Volmer kinetics, whereas the Marcus-Hush model was less accurate. The reduction of 2-methyl-2-nitropropane was well simulated by both models, however Marcus-Hush required a reorganisation energy lower than expected.

Hawaii Energy and Environmental Technologies (HEET) Initiative

DTIC Science & Technology

2010-08-01

segmented cell system for investigation of PEMFC performance distribution using both cyclic voltammetry (CV) and linear sweep voltammetry (LSV). In...mitigation strategies. Under prior work it was shown that SO2 contamination in the cathode of a PEMFC resulted in a two-stage degradation of cell...emission rate in a PEMFC is an important parameter for monitoring the Nafion degradation. Generally, the Nafion electrolyte degradation is

Nitrogen-doped graphene: effect of graphite oxide precursors and nitrogen content on the electrochemical sensing properties.

PubMed

Megawati, Monica; Chua, Chun Kiang; Sofer, Zdenek; Klímová, Kateřina; Pumera, Martin

2017-06-21

Graphene, produced via chemical methods, has been widely applied for electrochemical sensing due to its structural and electrochemical properties as well as its ease of production in large quantity. While nitrogen-doped graphenes are widely studied materials, the literature showing an effect of graphene oxide preparation methods on nitrogen quantity and chemical states as well as on defects and, in turn, on electrochemical sensing is non-existent. In this study, the properties of nitrogen-doped graphene materials, prepared via hydrothermal synthesis using graphite oxide produced by various classical methods using permanganate or chlorate oxidants Staudenmaier, Hummers, Hofmann and Brodie oxidation methods, were studied; the resulting nitrogen-doped graphene oxides were labeled as ST-GO, HU-GO, HO-GO and BR-GO, respectively. The electrochemical oxidation of biomolecules, such as ascorbic acid, uric acid, dopamine, nicotinamide adenine nucleotide and DNA free bases, was carried out using cyclic voltammetry and differential pulse voltammetry techniques. The nitrogen content in doped graphene oxides increased in the order ST-GO < BR-GO < HO-GO < HU-GO. In the same way, the pyridinic form of nitrogen increased and the electrocatalytic effect of N-doped graphene followed this trend, as shown in the cyclic voltammograms. This is a very important finding that provides insight into the electrocatalytic effect of N-doped graphene. The nitrogen-doped graphene materials exhibited improved sensitivity over bare glassy carbon for ascorbic acid, uric acid and dopamine detection. These studies will enhance our understanding of the effects of graphite oxide precursors on the electrochemical sensing properties of nitrogen-doped graphene materials.

Study of Copper and Purine-Copper Complexes on Modified Carbon Electrodes by Cyclic and Elimination Voltammetry

PubMed Central

Trnkova, Libuse; Zerzankova, Lenka; Dycka, Filip; Mikelova, Radka; Jelen, Frantisek

2008-01-01

Using a paraffin impregnated graphite electrode (PIGE) and mercury-modified pyrolytic graphite electrode with basal orientation (Hg-PGEb) copper(II) and Cu(II)-DNA purine base solutions have been studied by cyclic (CV) and linear sweep voltammetry (LSV) in connection with elimination voltammetry with linear scan (EVLS). In chloride and bromide solutions (pH 6), the redox process of Cu(II) proceeded on PIGE with two cathodic and two anodic potentially separated signals. According to the elimination function E4, the first cathodic peak corresponds to the reduction Cu(II) + e- → Cu(I) with the possibility of fast disproportionation 2Cu(I) → Cu(II)+ Cu(0). The E4 of the second cathodic peak signalized an electrode process controlled by a surface reaction. The electrode system of Cu(II) on Hg-PGEb in borate buffer (pH 9.2) was characterized by one cathodic and one anodic peak. Anodic stripping voltammetry (ASV) on PIGE and cathodic stripping voltammetry (CSV) on Hg-PGEb were carried out at potentials where the reduction of copper ions took place and Cu(I)-purine complexes were formed. By using ASV and CSV in combination with EVLS, the sensitivity of Cu(I)-purine complex detection was enhanced relative to either ASV or CSV alone, resulting in higher peak currents of more than one order of magnitude. The statistical treatment of CE data was used to determine the reproducibility of measurements. Our results show that EVLS in connection with the stripping procedure is useful for both qualitative and quantitative microanalysis of purine derivatives and can also reveal details of studied electrode processes. PMID:27879715

DOE Office of Scientific and Technical Information (OSTI.GOV)

Betancourt, Luis E.; Guzman-Blas, Rolando; Luo, Si

A robust electrodeposition method consisting of the rotating disk slurry electrode (RoDSE) technique to obtain Au nanoparticles highly dispersed on a conductive carbonaceous support, i.e., Vulcan XC-72R, for ethanol electrooxidation reaction in alkaline media was developed. Ceria was used as a cocatalyst using a Ce(III)-EDTA impregnation method in order to enhance the catalytic activity and improve the catalyst’s overall stability. Furthermore, the RoDSE method used to obtain highly dispersed Au nanoparticles does not require the use of a reducing agent or stabilizing agent, and the noble-metal loading was controlled by the addition and tuning of the metal precursor concentration. Inductivelymore » coupled plasma and thermogravimetric analysis indicated that the Au loading in the catalyst was 9 %. We determined the particle size and characteristic Au fcc crystal facets by X-ray diffraction. The morphology of the catalyst was also investigated using electron microscopy techniques. In addition, X-ray absorption spectroscopy was used to corroborate the presence and identify the oxidation state of Ce in the system and to observe if there are any electronic interactions within the 8 % Au/CeO x/C system. Cyclic voltammetry of electrodeposited 9 % Au/C and Ce-promoted 8 % Au/C showed a higher catalytic current density for ethanol oxidation when compared with commercially available catalysts (20 % Au/C) of a higher precious metal loading. Additionally, we report a higher stability toward the ethanol electrooxidation process, which was corroborated by 1 mV/s linear sweep voltammetry and chronoamperometric studies.« less

Low-level determination of silicon in steels by anodic stripping voltammetry on a hanging mercury drop electrode.

PubMed

Rahier, A H; Lunardi, S; Nicolle, F; George, S M

2010-10-15

The sensitive differential pulse anodic stripping voltammetry (DPASV) proposed originally by Ishiyama et al. (2001) has been revised and improved to allow the accurate measurement of silicon on a hanging mercury drop electrode (HMDE) instead of a glassy carbon electrode. We assessed the rate of formation of the partially reduced β-silicododecamolybdate and found that metallic mercury promotes the reaction in the presence of a large concentration of Fe(3+). The scope of the method has been broadened by carrying out the measurements in the presence of a constant amount of Fe(3+). The limit of detection (LOD) of the method described in the present paper is 100 μg Sig(-1) of steel, with a relative precision ranging from 5% to 12%. It can be further enhanced to 700 ng Sig(-1) of steel provided the weight of the sample, the dilution factors, the duration of the electrolysis and the ballast of iron are adequately revised. The tolerance to several interfering species has been examined, especially regarding Al(3+), Cr(3+) and Cr VI species. The method was validated using four low-alloy ferritic steels certified by the National Institute of Standards and Technology (NIST). Its application to nickel base alloys as well as to less complicated matrixes is straightforward. It has also been successfully applied to the determination of free silicon into silicon carbide nano-powder. Copyright © 2010 Elsevier B.V. All rights reserved.

Development of a new paper based nano-biosensor using the co-catalytic effect of tyrosinase from banana peel tissue (Musa Cavendish) and functionalized silica nanoparticles for voltammetric determination of l-tyrosine.

PubMed

Rahimi-Mohseni, Mohadeseh; Raoof, Jahan Bakhsh; Ojani, Reza; Aghajanzadeh, Tahereh A; Bagheri Hashkavayi, Ayemeh

2018-07-01

In this paper, a new and facile method for the electrochemical determination of l-tyrosine was designed. First, 3-mercaptopropyl trimethoxysilane-functionalized silica nanoparticles were added to a paper disc. Then, the banana peel tissue and the mediator potassium hexacyanoferrate were dropped onto the paper, respectively. The modified paper disc was placed on the top of the graphite screen printed electrode and electrochemical characterization of this biosensor was studied by cyclic voltammetry and electrochemical impedance spectroscopy methods. The effective parameters like pH, banana peel tissue percentage, and the amount of mediator loading were optimized. l-tyrosine measurements were done by differential pulse voltammetry with a little sample (3 μL) for analysis. The biosensor showed a linear response for l-tyrosine in the wide concentration range of 0.05-600 μM and a low detection limit about 0.02 μM because of the co-catalytic effect of enzyme and nanoparticles. The stability of the biosensor and its selectivity were evaluated. This biosensor was applied for the voltammetric determination of l-tyrosine in the blood plasma sample. The results of the practical application study were comparable with the standard method (HPLC). In conclusion, a simple, inexpensive, rapid, sensitive and selective technique was successfully applied to the l-tyrosine analysis of the little samples. Copyright © 2018 Elsevier B.V. All rights reserved.

Differential pulse adsorptive stripping voltammetric determination of nanomolar levels of atorvastatin calcium in pharmaceutical and biological samples using a vertically aligned carbon nanotube/graphene oxide electrode.

PubMed

Silva, Tiago Almeida; Zanin, Hudson; Vicentini, Fernando Campanhã; Corat, Evaldo José; Fatibello-Filho, Orlando

2014-06-07

A novel vertically aligned carbon nanotube/graphene oxide (VACNT-GO) electrode is proposed, and its ability to determine atorvastatin calcium (ATOR) in pharmaceutical and biological samples by differential pulse adsorptive stripping voltammetry (DPAdSV) is evaluated. VACNT films were prepared on a Ti substrate by a microwave plasma chemical vapour deposition method and then treated with oxygen plasma to produce the VACNT-GO electrode. The oxygen plasma treatment exfoliates the carbon nanotube tips exposing graphene foils and inserting oxygen functional groups, these effects improved the VACNT wettability (super-hydrophobic) which is crucial for its electrochemical application. The electrochemical behaviour of ATOR on the VACNT-GO electrode was studied by cyclic voltammetry, which showed that it underwent an irreversible oxidation process at a potential of +1.08 V in pHcond 2.0 (0.2 mol L(-1) buffer phosphate solution). By applying DPAdSV under optimized experimental conditions the analytical curve was found to be linear in the ATOR concentration range of 90 to 3.81 × 10(3) nmol L(-1) with a limit of detection of 9.4 nmol L(-1). The proposed DPAdSV method was successfully applied in the determination of ATOR in pharmaceutical and biological samples, and the results were in close agreement with those obtained by a comparative spectrophotometric method at a confidence level of 95%.

Simultaneous extraction and determination of trace amounts of diclofenac from whole blood using supported liquid membrane microextraction and fast Fourier transform voltammetry.

PubMed

Mofidi, Zahra; Norouzi, Parviz; Sajadian, Masumeh; Ganjali, Mohammad Reza

2018-04-01

A novel, simple, and inexpensive analytical technique based on flat sheet supported liquid membrane microextraction coupled with fast Fourier transform stripping cyclic voltammetry on a reduced graphene oxide carbon paste electrode was used for the extraction and online determination of diclofenac in whole blood. First, diclofenac was extracted from blood samples using a polytetrafluoroethylene membrane impregnated with 1-octanol and then into an acceptor solution, subsequently it was oxidized on a carbon paste electrode modified with reduced graphene oxide nanosheets. The optimal values of the key parameters influencing the method were as follows: scan rate, 6 V/s; stripping potential, 200 mV; stripping time, 5 s; pH of the sample solution, 5; pH of the acceptor solution,7; and extraction time, 240 min. The calibration curves were plotted for the whole blood samples and the method was found to have a good linearity within the range of 1-25 μg/mL with a determination coefficient of 0.99. The limits of detection and quantification were 0.1 and 1.0 μg/mL, respectively. Using this coupled method, the extraction and determination were merged into one step. Accordingly, the speed of detection for sensitive determination of diclofenac in complex samples, such as blood, increased considerably. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Cyclic Voltammetry Probe Approach Curves with Alkali Amalgams at Mercury Sphere-Cap Scanning Electrochemical Microscopy Probes.

PubMed

Barton, Zachary J; Rodríguez-López, Joaquín

2017-03-07

We report a method of precisely positioning a Hg-based ultramicroelectrode (UME) for scanning electrochemical microscopy (SECM) investigations of any substrate. Hg-based probes are capable of performing amalgamation reactions with metal cations, which avoid unwanted side reactions and positive feedback mechanisms that can prove problematic for traditional probe positioning methods. However, prolonged collection of ions eventually leads to saturation of the amalgam accompanied by irreversible loss of Hg. In order to obtain negative feedback positioning control without risking damage to the SECM probe, we implement cyclic voltammetry probe approach surfaces (CV-PASs), consisting of CVs performed between incremental motor movements. The amalgamation current, peak stripping current, and integrated stripping charge extracted from a shared CV-PAS give three distinct probe approach curves (CV-PACs), which can be used to determine the tip-substrate gap to within 1% of the probe radius. Using finite element simulations, we establish a new protocol for fitting any CV-PAC and demonstrate its validity with experimental results for sodium and potassium ions in propylene carbonate by obtaining over 3 orders of magnitude greater accuracy and more than 20-fold greater precision than existing methods. Considering the timescales of diffusion and amalgam saturation, we also present limiting conditions for obtaining and fitting CV-PAC data. The ion-specific signals isolated in CV-PACs allow precise and accurate positioning of Hg-based SECM probes over any sample and enable the deployment of CV-PAS SECM as an analytical tool for traditionally challenging conditions.

Determination of caffeic acid in wine using PEDOT film modified electrode.

PubMed

Bianchini, C; Curulli, A; Pasquali, M; Zane, D

2014-08-01

A novel method using PEDOT (poly(3,4-ethylenedioxy) thiophene) modified electrode was developed for the determination of caffeic acid (CA) in wine. Cyclic voltammetry (CV) with the additions standard method was used to quantify the analyte at PEDOT modified electrodes. PEDOT films were electrodeposited on Platinum electrode (Pt) in aqueous medium by galvanostatic method using sodium poly(styrene-4-sulfonate) (PSS) as electrolyte and surfactant. CV allows detecting the analyte over a wide concentration range (10.0nmoll(-1)-6.5mmoll(-1)). The electrochemical method proposed showed good statistical and analytical parameters as linearity range, LOD, LOQ and sensitivity. Copyright © 2014 Elsevier Ltd. All rights reserved.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Benson, David M.; Tsang, Chu F.; Sugar, Joshua Daniel

One method for the formation of nanofilms of materials, is Electrochemical atomic layer deposition (E-ALD), one atomic layer at a time. It uses the galvanic exchange of a less noble metal, deposited using underpotential deposition (UPD), to produce an atomic layer of a more noble element by reduction of its ions. This process is referred to as surface limited redox replacement and can be repeated in a cycle to grow thicker deposits. Previously, we performed it on nanoparticles and planar substrates. In the present report, E-ALD is applied for coating a submicron-sized powder substrate, making use of a new flowmore » cell design. E-ALD is used to coat a Pd powder substrate with different thicknesses of Rh by exchanging it for Cu UPD. Furthermore, cyclic voltammetry and X-ray photoelectron spectroscopy indicate an increasing Rh coverage with increasing numbers of deposition cycles performed, in a manner consistent with the atomic layer deposition (ALD) mechanism. Cyclic voltammetry also indicated increased kinetics of H sorption and desorption in and out of the Pd powder with Rh present, relative to unmodified Pd.« less

Implementation of electrochemical elements for an alternative detection of ochratoxin A

NASA Astrophysics Data System (ADS)

Aristizabal, D. H.; Giraldo, D. A.; Sanchez, S.; Taborda, G.; Baeza, A.

2017-01-01

Ochratoxin A (OTA) is a nephrotoxic metabolite, hepatotoxic and carcinogenic produced mainly by Aspergillus and Penicillium fungi. Usually, the mycotoxin analysed through the technique of high performance liquid chromatography. This method is expensive and takes a lot of time. Therefore, expected to automate a device of low cost, minimal instrumentation micropolarographic (MIMP) for the analysis. For this purpose, the right programming environment and the manufacturing of the software for the graphical user interface selected automation of the MIMP through the design and simulation of the circuit, imprint and assembled in a container with connection ports. Lastly, validation and analysis of Ochratoxin A by cyclic voltammetry from analogous MIMP, automatic MIMP and a potentiostat, in order to corroborate the registered data. This way, voltammetry analysis of coumarin is obtained and the simulation of the MIMP electric circuit. Therefore, this are the key data during the investigation, because the molecule of OTA can be monitored through an acid hydrolysis of amides, composed by a phenylalanine and coumaric acid group, generating the significant decrease in the costs and time of analysis.

A novel lable-free electrochemical immunosensor for carcinoembryonic antigen based on gold nanoparticles-thionine-reduced graphene oxide nanocomposite film modified glassy carbon electrode.

PubMed

Kong, Fen-Ying; Xu, Mao-Tian; Xu, Jing-Juan; Chen, Hong-Yuan

2011-10-15

In this paper, gold nanoparticle-thionine-reduced graphene oxide (GNP-THi-GR) nanocomposites were prepared to design a label-free immunosensor for the sensitive detection of carcinoembryonic antigen (CEA). The nanocomposites with good biocompatibility, excellent redox electrochemical activity and large surface area were coated onto the glassy carbon electrode (GCE) surface and then CEA antibody (anti-CEA) was immobilized on the electrode to construct the immunosensor. The morphologies and electrochemistry of the formed nanocomposites were investigated by using scanning electron microscopy (SEM), ultraviolet-visible (UV-vis) spectrometry, electrochemical impedance spectroscopy (EIS) and cyclic voltammetry (CV). CV and differential pulse voltammetry (DPV) studies demonstrated that the formation of antibody-antigen complexes decreased the peak current of THi in the GNP-THi-GR nanocomposites. The decreased currents were proportional to the CEA concentration in the range of 10-500 pg/mL with a detection limit of 4 pg/mL. The proposed method was simple, fast and inexpensive for the determination of CEA at very low levels. Copyright © 2011 Elsevier B.V. All rights reserved.

Structural comparative studies on new Mn(II), Cr(III) and Ru(III) complexes derived from 2,4,6-tri-(2-pyridyl)-1,3,5-triazine (TPTZ).

PubMed

Al-Assy, Waleed H; El-Askalany, Abdel Moneum H; Mostafa, Mohsen M

2013-12-01

The structure of a new Mn(II) complex, [Mn(TPTZ)Cl2(H2O)]⋅H2O, was established by a single crystal X-ray diffraction. Crystal data are as follow: monoclinic, P21/c,a = 8.7202 (3)Å, b = 11.5712 (4)Å, c = 20.8675 (9)Å, β=11 (18) × 1010, V = 2029.27 (13)Å(3), Z = 4. The HOMO, LUMO and other DFT parameters on the atoms have been calculated to confirm the geometry of the ligand and its complexes using material studio program. The complexes were characterized by elemental analyses, spectral, magnetic, thermal and cyclic voltammetry measurements. Electronic spectra and magnetic moments of the complexes suggest distorted-octahedral structures around the metal ions (Mn(II), Cr(III) and Ru(III)). The redox properties were investigated by cyclic voltammetry. Kinetic parameters were determined using Coats-Redfern and Horowitz-Metzger methods. The results of DNA studies of the metal complexes promised to be effective in tumour treatment. Copyright © 2013 Elsevier B.V. All rights reserved.

Beneficial effects of rhodium and tin oxide on carbon supported platinum catalysts for ethanol electrooxidation

NASA Astrophysics Data System (ADS)

Soares, Layciane A.; Morais, Claudia; Napporn, Teko W.; Kokoh, K. Boniface; Olivi, Paulo

2016-05-01

This work investigates ethanol electrooxidation on Pt/C, PtxRhy/C, Pt-SnO2/C, and PtxRhy-SnO2/C catalysts synthesized by the Pechini and microwave-assisted polyol methods. The catalysts are characterized by energy dispersive X-ray analysis (EDX), transmission electron microscopy (TEM), and X-ray diffraction (XRD) techniques. The electrochemical properties of these electrode materials are examined by cyclic voltammetry and chronoamperometry experiments in acid medium. The products obtained during ethanol electrolysis are identified by high performance liquid chromatography (HPLC). The adsorbed intermediates are evaluated by an in situ reflectance Infrared Spectroscopy technique combined with cyclic voltammetry. Catalysts performance in a direct ethanol fuel cell (DEFC) is also assessed. The electrical performance of the electrocatalysts in a single DEFC at 80 °C decreases in the following order Pt70Rh30SnO2 > Pt80Rh20SnO2 > Pt60Rh40SnO2 ∼ PtSnO2 > PtxRhy ∼ Pt, showing that the presence of SnO2 enhances the ability of Pt to catalyze ethanol electrooxidation.

Anodic stripping voltammetry with carbon paste electrodes for rapid Ag(I) and Cu(II) determinations.

PubMed

Labar, C; Lamberts, L

1997-05-01

The simultaneous determination of silver(I) and copper(II) is realized for the routine analysis of trace levels of these elements by anodic stripping voltammetry (ASV) at the carbon paste electrode (CPE). The electrochemical response is studied in 14 different supporting electrolytes, ranging from acidic solutions (pH 0.1) to neutral and basic (pH 9.7) media, and the parameters governing electrodeposition and stripping steps are characterized for each medium by the use of pseudo-voltammograms. Comparison between different modes of matter transport mechanisms is also given. The dynamic range of the method is 0.05 to 150 mug 1(-1) Ag(I) in the majority of the media studied and can be extended to 400 mug l(-1) in selected media, with a general reproducibility in the +/- 2% range for five replicate measurements. The total analysis time lies between approximately 30 s and 10 min. Activation of the CPE surface has been studied, but this pretreatment is demonstrated to be unfavourable and is replaced by a simpler unique 'cleaning' procedure of dipping the CPE in diluted nitric acid.

Anodic stripping voltammetry enhancement by redox magnetohydrodynamics.

PubMed

Clark, Emily A; Fritsch, Ingrid

2004-04-15

The effect of an external magnetic field on linear scan anodic stripping voltammetry (ASV) in solutions of 10(-6)-10(-7) M concentrations of lead, cadmium, and copper at mercury films on glassy carbon electrodes has been investigated. A high concentration of Hg(2+) was added to the analyte solution to induce a large cathodic current during the deposition step. Therefore, a large Lorentz force from the net flux of charge through the magnetic field resulted in convection due to magnetohydrodynamics. The faster delivery of analytes to the mercury film electrode during deposition caused an increase in the anodic stripping peaks. The effect of varying Hg(2+) concentrations (0-60 mM) and magnetic field strengths (0-1.77 T) on the enhancement of the stripping peaks was investigated. Enhancements as large as 129% for peak currents and 167% for peak areas were observed. An enhancement of approximately 100% was observed when 60 mM Fe(3+) replaced high concentrations of Hg(2+). This method of convection exhibits promise for small-volume ASV analysis with possible improved limits of detection and decreased preconcentration times.

Structural comparative studies on new MnII, CrIII and RuIII complexes derived from 2,4,6-tri-(2-pyridyl)-1,3,5-triazine (TPTZ)

NASA Astrophysics Data System (ADS)

Al-Assy, Waleed H.; El-Askalany, Abdel Moneum H.; Mostafa, Mohsen M.

2013-12-01

The structure of a new MnII complex, [Mn(TPTZ)Cl2(H2O)]ṡH2O, was established by a single crystal X-ray diffraction. Crystal data are as follow: monoclinic, P21/c, a = 8.7202 (3) Å, b = 11.5712 (4) Å, c = 20.8675 (9) Å, β = 11 (18) × 1010, V = 2029.27 (13) Å3, Z = 4. The HOMO, LUMO and other DFT parameters on the atoms have been calculated to confirm the geometry of the ligand and its complexes using material studio program. The complexes were characterized by elemental analyses, spectral, magnetic, thermal and cyclic voltammetry measurements. Electronic spectra and magnetic moments of the complexes suggest distorted-octahedral structures around the metal ions (MnII, CrIII and RuIII). The redox properties were investigated by cyclic voltammetry. Kinetic parameters were determined using Coats-Redfern and Horowitz-Metzger methods. The results of DNA studies of the metal complexes promised to be effective in tumour treatment.

Excimer laser assisted very fast exfoliation and reduction of graphite oxide at room temperature under air ambient for Supercapacitors electrode

NASA Astrophysics Data System (ADS)

Malek Hosseini, S. M. B.; Baizaee, S. M.; Naderi, Hamid Reza; Dare Kordi, Ali

2018-01-01

Excimer laser was used for reduction and exfoliation of graphite oxide (GO) at room temperature under air ambient. The prepared excimer laser reduced graphite oxide (XLRGO) is characterized by scanning electron microscopy (SEM), atomic force microscopy (AFM), nitrogen adsorption/desorption (BET method), X-ray diffraction (XRD), X-ray photoemission spectroscopy (XPS), Fourier transform infrared spectroscopy (FTIR) and UV-vis absorption techniques for surface, structural functional groups and band gap analysis. Electrochemical properties are investigated using cyclic voltammetry, galvanostatic charge-discharge, electrochemical impedance spectroscopy (EIS) and continues cyclic voltammetry (CCV) in 0.5 M Na2SO4 as electrolyte. Electrochemical investigations revealed that XLRGO electrode has enhanced supercapacitive performance including specific capacitance of 299 F/g at a scan rate of 2 mV/s. Furthermore, CCV measurement showed that XLRGO electrode kept 97.8% of its initial capacitance/capacity after 4000 cycles. The obtained results from electrochemical investigations confirm that the reduction of GO by using an excimer laser produces high-quality graphene for supercapacitor applications without the need for additional operations.

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

PubMed

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.

A facile approach to prepare crumpled CoTMPyP/electrochemically reduced graphene oxide nanohybrid as an efficient electrocatalyst for hydrogen evolution reaction

NASA Astrophysics Data System (ADS)

Ma, Juanjuan; Liu, Lin; Chen, Qian; Yang, Min; Wang, Danping; Tong, Zhiwei; Chen, Zhong

2017-03-01

Elaborate design and synthesis of efficient and stable non-Pt electrocatalysts for some renewable energy related conversion/storage processes are one of the major goals of sustainable chemistry. Herein, we report a facile method to fabricate Co porphyrin functionalized electrochemically reduced graphene oxide (CoTMPyP/ERGO) thin film by direct assembly of oppositely charged tetrakis(N-methylpyridyl) porphyrinato cobalt (CoTMPyP) and GO nanosheets under mild conditions followed by an electrochemical reduction procedure. STEM analysis confirms that CoTMPyP nanoaggregates are homogeneously distributed over the graphene surface. The electrochemical properties of CoTMPyP/ERGO were investigated by cyclic voltammetry, linear sweep voltammetry and electrochemical impedance spectroscopy. The results demonstrate that CoTMPyP/ERGO nanohybrid film can serve as excellent electrocatalyst for hydrogen evolution in alkaline solution with high activity and stability. The intimate contact and efficient electron transfer between CoTMPyP and ERGO, as well as the crumpled structure, contribute to the improvement of the electrocatalytic performance.

Identification of lead pigments in nanosamples from ancient paintings and polychromed sculptures using voltammetry of nanoparticles/atomic force microscopy.

PubMed

Doménech-Carbó, Antonio; Doménech-Carbó, María Teresa; Mas-Barberá, Xavier

2007-03-15

Voltammetry of nanoparticles coupled with atomic force microscopy was used to identify lead pigments in nanosamples proceeding from works of art. Upon mechanical attachment of few nanograms of sample to a graphite plate, well-defined voltammetric responses were obtained for lead orange, lead yellow, lead white, litharge, minium, Naples yellow, and tin-lead yellow, allowing for an unambiguous identification of such pigments. Atomic force images provide evidence for the occurrence of pigment-characteristic reduction processes accompanied by metal deposition on the graphite substrate. Electrochemical parameters are used for pigment identification. Application to the method for identifying lead pigments in different model binder+pigment specimens and pictorial samples from the canvas painting collection (anonymous, 17th century) of the Saint Joseph Church in Taormina (Italy), the frescoes painted by Antonio Acisclo Palomino y Velasco (1698) in the vault of the Sant Joan del Mercat church in València (Spain) and an anonymous polychromed sculpture (16th century) representing a Martyr Saint from Alacant (Spain) is described.

Nano Copper Oxide-Modified Carbon Cloth as Cathode for a Two-Chamber Microbial Fuel Cell

PubMed Central

Dong, Feng; Zhang, Peng; Li, Kexun; Liu, Xianhua; Zhang, Pingping

2016-01-01

In this work, Cu2O nanoparticles were deposited on a carbon cloth cathode using a facile electrochemical method. The morphology of the modified cathode, which was characterized by scanning electron microscopy (SEM) and Brunauer-Emmett-Teller (BET) tests, showed that the porosity and specific surface area of the cathode improved with longer deposition times. X-ray photoelectron spectroscopy (XPS) and cyclic voltammetry (CV) results showed that cupric oxide and cuprous oxide coexisted on the carbon cloth, which improved the electrochemical activity of cathode. The cathode with a deposition time of 100 s showed the best performance, with a power density twice that of bare carbon cloth. Linear sweep voltammetry (LSV) and electrochemical impedance spectroscopy (EIS) results revealed that moderate deposition of nano copper oxide on carbon cloth could dramatically reduce the charge transfer resistance, which contributed to the enhanced electrochemical performance. The mediation mechanism of copper oxide nanocatalyst was illustrated by the fact that the recycled conversion between cupric oxide and cuprous oxide accelerated the electron transfer efficiency on the cathode. PMID:28335366

Nano Copper Oxide-Modified Carbon Cloth as Cathode for a Two-Chamber Microbial Fuel Cell.

PubMed

Dong, Feng; Zhang, Peng; Li, Kexun; Liu, Xianhua; Zhang, Pingping

2016-12-09

In this work, Cu₂O nanoparticles were deposited on a carbon cloth cathode using a facile electrochemical method. The morphology of the modified cathode, which was characterized by scanning electron microscopy (SEM) and Brunauer-Emmett-Teller (BET) tests, showed that the porosity and specific surface area of the cathode improved with longer deposition times. X-ray photoelectron spectroscopy (XPS) and cyclic voltammetry (CV) results showed that cupric oxide and cuprous oxide coexisted on the carbon cloth, which improved the electrochemical activity of cathode. The cathode with a deposition time of 100 s showed the best performance, with a power density twice that of bare carbon cloth. Linear sweep voltammetry (LSV) and electrochemical impedance spectroscopy (EIS) results revealed that moderate deposition of nano copper oxide on carbon cloth could dramatically reduce the charge transfer resistance, which contributed to the enhanced electrochemical performance. The mediation mechanism of copper oxide nanocatalyst was illustrated by the fact that the recycled conversion between cupric oxide and cuprous oxide accelerated the electron transfer efficiency on the cathode.

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

NASA Astrophysics Data System (ADS)

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

2017-07-01

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

A voltammetric method for Fe(iii) in blood serum using a screen-printed electrode modified with a Schiff base ionophore.

PubMed

Mittal, Susheel K; Rana, Sonia; Kaur, Navneet; Banks, Craig E

2018-05-23

Herein, a potent electrochemical ionophore (SMS-2) based on a Schiff base has been used for the modification of a screen-printed electrode (SPE). The modified disposable electrode can selectively detect ferric ions in an aqueous medium. Redox behavior of the proposed strip was characterized using cyclic voltammetry (CV) and differential pulse voltammetry (DPV). Incorporation of the ligand in the ink of the SPE enhanced the analytical performance of the electrode, and its surface modification was confirmed by SEM and EDX analysis. Shifting/quenching of the cathodic peak potential of the ionophore after binding with Fe(iii) ions was used to detect and measure the ferric ion concentration. This sensor can identify Fe(iii) in the detection range from 0.625 μM to 7.5 μM. The modified SPE can selectively detect ferric ions in the presence of many other interfering ions and has been successfully used to determine the Fe(iii) content in blood serum samples. The metal-ionophore complex structure was optimized using DFT calculations to study the energetics of the metal-ionophore interactions.

Development of an Electrochemical DNA Biosensor to Detect a Foodborne Pathogen.

PubMed

Nordin, Noordiana; Yusof, Nor Azah; Radu, Son; Hushiarian, Roozbeh

2018-06-03

Vibrio parahaemolyticus (V. parahaemolyticus) is a common foodborne pathogen that contributes to a large proportion of public health problems globally, significantly affecting the rate of human mortality and morbidity. Conventional methods for the detection of V. parahaemolyticus such as culture-based methods, immunological assays, and molecular-based methods require complicated sample handling and are time-consuming, tedious, and costly. Recently, biosensors have proven to be a promising and comprehensive detection method with the advantages of fast detection, cost-effectiveness, and practicality. This research focuses on developing a rapid method of detecting V. parahaemolyticus with high selectivity and sensitivity using the principles of DNA hybridization. In the work, characterization of synthesized polylactic acid-stabilized gold nanoparticles (PLA-AuNPs) was achieved using X-ray Diffraction (XRD), Ultraviolet-visible Spectroscopy (UV-Vis), Transmission Electron Microscopy (TEM), Field-emission Scanning Electron Microscopy (FESEM), and Cyclic Voltammetry (CV). We also carried out further testing of stability, sensitivity, and reproducibility of the PLA-AuNPs. We found that the PLA-AuNPs formed a sound structure of stabilized nanoparticles in aqueous solution. We also observed that the sensitivity improved as a result of the smaller charge transfer resistance (Rct) value and an increase of active surface area (0.41 cm 2 ). The development of our DNA biosensor was based on modification of a screen-printed carbon electrode (SPCE) with PLA-AuNPs and using methylene blue (MB) as the redox indicator. We assessed the immobilization and hybridization events by differential pulse voltammetry (DPV). We found that complementary, non-complementary, and mismatched oligonucleotides were specifically distinguished by the fabricated biosensor. It also showed reliably sensitive detection in cross-reactivity studies against various food-borne pathogens and in the identification of V. parahaemolyticus in fresh cockles.

Electrochemical characterisation and anodic stripping voltammetry at mesoporous platinum rotating disc electrodes.

PubMed

Lozano-Sanchez, Pablo; Elliott, Joanne M

2008-02-01

Using the technique of liquid crystal templating a rotating disc electrode (RDE) was modified with a high surface area mesoporous platinum film. The surface area of the electrode was characterised by acid voltammetry, and found to be very high (ca. 86 cm(2)). Acid characterisation of the electrode produced distorted voltammograms was interpreted as being due to the extremely large surface area which produced a combination of effects such as localised pH change within the pore environment and also ohmic drop effects. Acid voltammetry in the presence of two different types of surfactant, namely Tween 20 and Triton X-100, suggested antifouling properties associated with the mesoporous deposit. Further analysis of the modified electrode using a redox couple in solution showed typical RDE behaviour although extra capacitive currents were observed due to the large surface area of the electrode. The phenomenon of underpotential deposition was exploited for the purpose of anodic stripping voltammetry and results were compared with data collected for microelectrodes. Underpotential deposition of metal ions at the mesoporous RDE was found to be similar to that at conventional platinum electrodes and mesoporous microelectrodes although the rate of surface coverage was found to be slower at a mesoporous RDE. It was found that a mesoporous RDE forms a suitable system for quantification of silver ions in solution.

Partially Reduced Graphene Oxide Modified Tetrahedral Amorphous Carbon Thin-Film Electrodes as a Platform for Nanomolar Detection of Dopamine

DOE PAGES

Wester, Niklas; Sainio, Sami; Palomäki, Tommi; ...

2017-03-16

Here, we present for the first time tetrahedral amorphous carbon (ta-C)—a partially reduced graphene oxide (PRGO) hybrid electrode nanomaterial platform for electrochemical sensing of dopamine (DA). Graphene oxide was synthesized with the modified Hummer’s method. Before modification of ta-C by drop casting, partial reduction of the GO was carried out to improve electrochemical properties and adhesion to the ta-C thin film. A facile nitric acid treatment that slightly reoxidized the surface and modified the surface chemistry was subsequently performed to further improve the electrochemical properties of the electrodes. The largest relative increase was seen in carboxyl groups. The HNO 3more » treatment increased the sensitivity toward DA and AA and resulted in a cathodic shift in the oxidation of AA. The fabricated hybrid electrodes were characterized with scanning electron microscopy (SEM), Raman spectroscopy, Fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), X-ray absorption spectroscopy (XAS), and electrochemical impedance spectroscopy (EIS). Moreover, compared to the plain ta-C electrode the hybrid electrode was shown to exhibit superior sensitivity and selectivity toward DA in the presence of ascorbic acid (AA), enabling simultaneous sensing of AA and DA close to the physiological concentrations by cyclic voltammetry (CV) and by differential pulse voltammetry (DPV). Two linear ranges of 0–1 μM and 1–100 μM and a detection limit (S/N = 3.3) of 2.6 nM for DA were determined by means of cyclic voltammetry. Thus, the current work provides a fully CMOS-compatible carbon based hybrid nanomaterial that shows potential for in vivo measurements of DA.« less

Partially Reduced Graphene Oxide Modified Tetrahedral Amorphous Carbon Thin-Film Electrodes as a Platform for Nanomolar Detection of Dopamine

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wester, Niklas; Sainio, Sami; Palomäki, Tommi

Here, we present for the first time tetrahedral amorphous carbon (ta-C)—a partially reduced graphene oxide (PRGO) hybrid electrode nanomaterial platform for electrochemical sensing of dopamine (DA). Graphene oxide was synthesized with the modified Hummer’s method. Before modification of ta-C by drop casting, partial reduction of the GO was carried out to improve electrochemical properties and adhesion to the ta-C thin film. A facile nitric acid treatment that slightly reoxidized the surface and modified the surface chemistry was subsequently performed to further improve the electrochemical properties of the electrodes. The largest relative increase was seen in carboxyl groups. The HNO 3more » treatment increased the sensitivity toward DA and AA and resulted in a cathodic shift in the oxidation of AA. The fabricated hybrid electrodes were characterized with scanning electron microscopy (SEM), Raman spectroscopy, Fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), X-ray absorption spectroscopy (XAS), and electrochemical impedance spectroscopy (EIS). Moreover, compared to the plain ta-C electrode the hybrid electrode was shown to exhibit superior sensitivity and selectivity toward DA in the presence of ascorbic acid (AA), enabling simultaneous sensing of AA and DA close to the physiological concentrations by cyclic voltammetry (CV) and by differential pulse voltammetry (DPV). Two linear ranges of 0–1 μM and 1–100 μM and a detection limit (S/N = 3.3) of 2.6 nM for DA were determined by means of cyclic voltammetry. Thus, the current work provides a fully CMOS-compatible carbon based hybrid nanomaterial that shows potential for in vivo measurements of DA.« less

Role of Au(NPs) in the enhanced response of Au(NPs)-decorated MWCNT electrochemical biosensor

PubMed Central

Mehmood, Shahid; Ciancio, Regina; Carlino, Elvio; Bhatti, Arshad S

2018-01-01

Background The combination of Au-metallic-NPs and CNTs are a new class of hybrid nanomaterials for the development of electrochemical biosensor. Concentration of Au(nanoparticles [NPs]) in the electrochemical biosensor is crucial for the efficient charge transfer between the Au-NPs-MWCNTs modified electrode and electrolytic solution. Methods In this work, the charge transfer kinetics in the glassy carbon electrode (GCE) modified with Au(NPs)–multiwalled carbon nanotube (MWCNT) nanohybrid with varied concentrations of Au(NPs) in the range 40–100 nM was studied using electrochemical impedance spectroscopy (EIS). Field emission scanning electron microscopy and transmission electron microscopy confirmed the attachment of Au(NPs) on the surface of MWCNTs. Results The cyclic voltammetry and EIS results showed that the charge transfer mechanism was diffusion controlled and the rate of charge transfer was dependent on the concentration of Au(NPs) in the nanohybrid. The formation of spherical diffusion zone, which was dependent on the concentration of Au(NPs) in nanohybrids, was attributed to result in 3 times the increase in the charge transfer rate ks, 5 times increase in mass transfer, and 5% (9%) increase in Ipa (Ipc) observed in cyclic voltammetry in 80 nM Au(NP) nanohybrid-modified GCE from MWCNT-modified GCE. The work was extended to probe the effect of charge transfer rates at various concentrations of Au(NPs) in the nanohybrid-modified electrodes in the presence of Escherichia coli. The cyclic voltammetry results clearly showed the best results for 80 nM Au(NPs) in nanohybrid electrode. Conclusion The present study suggested that the formation of spherical diffusion zone in nanohybrid-modified electrodes is critical for the enhanced electrochemical biosensing applications. PMID:29713161

Novel Imaging Method of Continuous Shear Wave by Ultrasonic Color Flow Mapping

NASA Astrophysics Data System (ADS)

Yamakoshi, Yoshiki; Yamamoto, Atsushi; Yuminaka, Yasushi

Shear wave velocity measurement is a promising method in evaluation of tissue stiffness. Several methods have been developed to measure the shear wave velocity, however, it is difficult to obtain quantitative shear wave image in real-time by low cost system. In this paper, a novel shear wave imaging method for continuous shear wave is proposed. This method uses a color flow imaging which is used in ultrasonic imaging system to obtain shear wave's wavefront map. Two conditions, shear wave frequency condition and shear wave displacement amplitude condition, are required, however, these conditions are not severe restrictions in most applications. Using the proposed method, shear wave velocity of trapezius muscle is measured. The result is consistent with the velocity which is calculated from shear elastic modulus measured by ARFI method.

Integrated circuit-based electrochemical sensor for spatially resolved detection of redox-active metabolites in biofilms.

PubMed

Bellin, Daniel L; Sakhtah, Hassan; Rosenstein, Jacob K; Levine, Peter M; Thimot, Jordan; Emmett, Kevin; Dietrich, Lars E P; Shepard, Kenneth L

2014-01-01

Despite advances in monitoring spatiotemporal expression patterns of genes and proteins with fluorescent probes, direct detection of metabolites and small molecules remains challenging. A technique for spatially resolved detection of small molecules would benefit the study of redox-active metabolites that are produced by microbial biofilms and can affect their development. Here we present an integrated circuit-based electrochemical sensing platform featuring an array of working electrodes and parallel potentiostat channels. 'Images' over a 3.25 × 0.9 mm(2) area can be captured with a diffusion-limited spatial resolution of 750 μm. We demonstrate that square wave voltammetry can be used to detect, identify and quantify (for concentrations as low as 2.6 μM) four distinct redox-active metabolites called phenazines. We characterize phenazine production in both wild-type and mutant Pseudomonas aeruginosa PA14 colony biofilms, and find correlations with fluorescent reporter imaging of phenazine biosynthetic gene expression.

Heavy metal distribution in organic and siliceous marine sponge tissues measured by square wave anodic stripping voltammetry.

PubMed

Illuminati, S; Annibaldi, A; Truzzi, C; Scarponi, G

2016-10-15

May sponge spicules represent a "tank" to accumulate heavy metals? In this study we test this hypothesis determining the distribution of Cd, Pb and Cu concentrations between organic and siliceous tissues in Antarctic Demospongia (Sphaerotylus antarcticus, Kirkpatrikia coulmani and Haliclona sp.) and in the Mediterranean species Petrosia ficiformis. Results show that although, in these sponges, spicules represent about 80% of the mass content, the accumulation of pollutant is lower in the spicules than in the corresponding organic fraction. The contribution of tissues to the total sponge content of Cd, Pb and Cu is respectively 99%, 82% and 97% for Antarctic sponges and 96%, 95% and 96% for P. ficiformis, similar in polar and temperate organisms. These results pave the way to a better understanding of the role of marine sponges in uptaking heavy metals and to their possible use as monitor of marine ecosystems, recommend by the Water Framework Directive. Copyright © 2016 Elsevier Ltd. All rights reserved.

High Performance Fe- and N- Doped Carbon Catalyst with Graphene Structure for Oxygen Reduction

NASA Astrophysics Data System (ADS)

Peng, Hongliang; Mo, Zaiyong; Liao, Shijun; Liang, Huagen; Yang, Lijun; Luo, Fan; Song, Huiyu; Zhong, Yiliang; Zhang, Bingqing

2013-05-01

Proton exchange membrane fuel cells are promising candidates for a clean and efficient energy conversion in the future, the development of carbon based inexpensive non-precious metal ORR catalyst has becoming one of the most attractive topics in fuel cell field. Herein we report a Fe- and N- doped carbon catalyst Fe-PANI/C-Mela with graphene structure and the surface area up to 702 m2 g-1. In 0.1 M HClO4 electrolyte, the ORR onset potential for the catalyst is high up to 0.98 V, and the half-wave potential is only 60 mV less than that of the Pt/C catalyst (Loadings: 51 μg Pt cm-2). The catalyst shows high stability after 10,000 cyclic voltammetry cycles. A membrane electrode assembly made with the catalyst as a cathode is tested in a H2-air single cell, the maximum power density reached ~0.33 W cm2 at 0.47 V.

Electroactive Film of Myoglobin Incorporated in a 3D-porous Calcium Alginate Film with Polyvinyl Alcohol, Glycerin and Gelatin.

PubMed

Zheng, Xueqin; Sun, Hong; Hou, Shifeng

2015-01-01

In this work, an electroactive porous Mb-CA's composite film was fabricated by incorporating myoglobin (Mb) in a three-dimension (3D) porous calcium alginate (CA) film with polyvinyl alcohol, glycerol, and gelatin. The porous Mb-CA's film modified electrodes exhibited a pair of well-defined, quasi-reversible cyclic voltammetric (CV) peaks at about -0.37 V vs. SCE in pH 7.0 buffers, characteristic of Mb heme Fe((III))/Fe((II)) redox couples. The electrochemical parameters, such as formal potentials (E(o')) and apparent heterogeneous electron-transfer rate constants (ks), were estimated by square-wave voltammetry with nonlinear regression analysis. The porous CA's composite film could form hydrogel in aqueous solution. The positions of the Soret absorbance band suggest that Mb in the CA's composite film kept its native states in the medium pH range. Hydrogen peroxide, oxygen, and nitrite were electrochemically catalyzed by the Mb-CA's composite film with significant lowering of the reduction overpotential.

Smart bi-metallic perovskite nanofibers as selective and reusable sensors of nano-level concentrations of non-steroidal anti-inflammatory drugs.

PubMed

Mohamed, Mona A; Hasan, Menna M; Abdullah, Ibrahim H; Abdellah, Ahmed M; Yehia, Ali M; Ahmed, Nashaat; Abbas, Walaa; Allam, Nageh K

2018-08-01

A strategy for trace-level carbon-based electrochemical sensors is investigated via exploring the interesting properties of BaNb 2 O 6 nanofibers (NFs). Utilizing adsorptive stripping square wave voltammetry (ASSWV), an electrochemical sensing platform was developed based on BaNb 2 O 6 nanofibers-modified carbon paste electrode (CPE) for the sensitive detection of lornoxicam (LOR). Different techniques were used to characterize the fabricated BaNb 2 O 6 perovskite NFs. The obtained data show the feasibility to electro-oxidize LOR and paracetamol (PAR) on the surface of the fabricated sensor. The amount of nanofiber and testing conditions were optimized using response surface methodology and ASSWV technique. The optimized BaNb 2 O 6 /CPE sensor exhibits low detection limit of 6.39 × 10 -10 mol L -1 , even in the presence of the co-formulated drug paracetamol (PAR). The sensor was successfully applied for biological applications. Copyright © 2018 Elsevier B.V. All rights reserved.

Voltammetric determination of mixtures of caffeine and chlorogenic acid in beverage samples using a boron-doped diamond electrode.

PubMed

Yardım, Yavuz; Keskin, Ertugrul; Şentürk, Zühre

2013-11-15

Herein, a boron-doped diamond (BDD) electrode that is anodically pretreated was used for the simultaneous determination of caffeine (CAF) and chlorogenic acid (CGA) by cyclic and adsorptive stripping voltammetry. The dependence of peak current and potential on pH, scan rate, accumulation parameters and other experimental variables were studied. By using square-wave stripping mode after 60 s accumulation under open-circuit voltage, the BDD electrode was able to separate the oxidation peak potentials of CAF and CGA present in binary mixtures by about 0.4V in Britton-Robinson buffer at pH 1.0. The limits of detection were 0.107 µg mL(-1) (5.51×10(-7) M) for CAF, and 0.448 µg mL(-1) (1.26×10(-6) M) for CGA. The practical applicability of this methodology was tested in commercially available beverage samples. © 2013 Elsevier B.V. All rights reserved.

Integrated circuit-based electrochemical sensor for spatially resolved detection of redox-active metabolites in biofilms

PubMed Central

Bellin, Daniel L.; Sakhtah, Hassan; Rosenstein, Jacob K.; Levine, Peter M.; Thimot, Jordan; Emmett, Kevin; Dietrich, Lars E. P.; Shepard, Kenneth L.

2014-01-01

Despite advances in monitoring spatiotemporal expression patterns of genes and proteins with fluorescent probes, direct detection of metabolites and small molecules remains challenging. A technique for spatially resolved detection of small molecules would benefit the study of redox-active metabolites produced by microbial biofilms, which can drastically affect colony development. Here we present an integrated circuit-based electrochemical sensing platform featuring an array of working electrodes and parallel potentiostat channels. “Images” over a 3.25 × 0.9 mm area can be captured with a diffusion-limited spatial resolution of 750 μm. We demonstrate that square wave voltammetry can be used to detect, identify, and quantify (for concentrations as low as 2.6 μM) four distinct redox-active metabolites called phenazines. We characterize phenazine production in both wild-type and mutant Pseudomonas aeruginosa PA14 colony biofilms, and find correlations with fluorescent reporter imaging of phenazine biosynthetic gene expression. PMID:24510163

Electrochemical product detection of an asymmetric convective polymerase chain reaction.

PubMed

Duwensee, Heiko; Mix, Maren; Stubbe, Marco; Gimsa, Jan; Adler, Marcel; Flechsig, Gerd-Uwe

2009-10-15

For the first time, we describe the application of heated microwires for an asymmetric convective polymerase chain reaction (PCR) in a modified PCR tube in a small volume. The partly single-stranded product was labeled with the electrochemically active compound osmium tetroxide bipyridine using a partially complementary protective strand with five mismatches compared to the single-stranded product. The labeled product could be successfully detected at a gold electrode modified with a complementary single-stranded capture probe immobilized via a thiol-linker. Our simple thermo-convective PCR yielded electrochemically detectable products after only 5-10 min. A significant discrimination between complementary and non-complementary target was possible using different immobilized capture probes. The total product yield was approx. half the amount of the classical thermocycler PCR. Numerical simulations describing the thermally driven convective PCR explain the received data. Discrimination between complementary capture probes and non-complementary capture probes was performed using square-wave voltammetry. The coupling of asymmetric thermo-convective PCR with electrochemical detection is very promising for future compact DNA sensor devices.

Diagnosis of Helicobacter pylori bacterial infections using a voltammetric biosensor.

PubMed

Ly, Suw Young; Yoo, Hai-Soo; Choa, Sung Hoon

2011-10-01

The voltammetric assay of Helicobacter pylori DNA was investigated using a bismuth-immobilized carbon nanotube electrode (BCNE). The analytical cyclic voltammetry (CV) peak potential was obtained at a 0.4V reduction scan, where the diagnostic optimum square-wave (SW) stripping working range was achieved at 0.72-7.92 μg/mL H. pylori DNA (11 points). A relative standard deviation of 1.68% (RSD, n=5) was obtained with 3.2 mg/mL H. pylori DNA using a 240 s accumulation time. Under optimum conditions, detection limit was 0.06 μg/mL. The developed sensors can be used for clinical application in the 15th doubted human gastric tissues, since the patient's peak current increased a hundred times more than the negative healthy tissue did. The sensing time obtained was only two minutes, and the process was simpler compared to common PCR amplification and electrophoresis photometric detection systems. Copyright © 2011 Elsevier B.V. All rights reserved.

Electrochemical reduction of carbon fluorine bond in 4-fluorobenzonitrile Mechanistic analysis employing Marcus Hush quadratic activation-driving force relation

NASA Astrophysics Data System (ADS)

Muthukrishnan, A.; Sangaranarayanan, M. V.

2007-10-01

The reduction of carbon-fluorine bond in 4-fluorobenzonitrile in acetonitrile as the solvent, is analyzed using convolution potential sweep voltammetry and the dependence of the transfer coefficient on potential is investigated within the framework of Marcus-Hush quadratic activation-driving force theory. The validity of stepwise mechanism is inferred from solvent reorganization energy estimates as well as bond length calculations using B3LYP/6-31g(d) method. A novel method of estimating the standard reduction potential of the 4-fluorobenzonitrile in acetonitrile is proposed.

A glassy carbon electrode modified with cerium phosphate nanotubes for the simultaneous determination of hydroquinone, catechol and resorcinol.

PubMed

Li, Zhen; Yue, Yuhua; Hao, Yanjun; Feng, Shun; Zhou, Xianli

2018-03-12

A nafion film containing cerium phosphate nanotubes was pasted onto a glassy carbon electrode (GCE) to obtain a sensor for hydroquinone (HQ). The morphologies and components of the coating were characterized by transmission electron microscopy, scanning electron microscopy and energy-dispersive spectroscopy. Cyclic voltammetry and differential pulse voltammetry (DPV) showed the specific surface of the electrode to be significantly increased and the electron transfer rate to be accelerated. The modified GCE was applied to the determination of hydroquinone (HQ) via DPV. The oxidation current increases linearly in the 0.23 μM to 16 mM HQ concentration range which is as wide as five orders of magnitude. The limit of detection is 0.12 μM (based on a signal-to-noise ratio of 3), and the sensitivity is 1.41 μA·μM -1  cm -2 . The method was further applied to the simultaneous determination of HQ, catechol and resorcinol. The potentials for the three species are well separated (20, 134, and 572 mV vs SCE). Average recoveries from (spiked) real water samples are between 95.2 and 107.0%, with relative standard deviations of 0.9~2.7% (for n = 3) at three spiking levels. The method was validated by independent assays using HPLC. Graphical abstract ᅟ.

Computational design and multivariate optimization of an electrochemical metoprolol sensor based on molecular imprinting in combination with carbon nanotubes.

PubMed

Nezhadali, Azizollah; Mojarrab, Maliheh

2016-06-14

This work describes the development of an electrochemical sensor based on a new molecularly imprinted polymer for detection of metoprolol (MTP) at ultra-trace level. The polypyrrole (PPy) was electrochemically synthesized on the tip of a pencil graphite electrode (PGE) which modified whit functionalized multi-walled carbon nanotubes (MWCNTs). The fabrication process of the sensor was characterized by cyclic voltammetry (CV) and the measurement process was carried out by differential pulse voltammetry (DPV). A computational approach was used to screening functional monomers and polymerization solvent for rational design of molecularly imprinted polymer (MIP). Based on computational results, pyrrole and water were selected as functional monomer and polymerization solvent, respectively. Several significant parameters controlling the performance of the MIP sensor were examined and optimized using multivariate optimization methods such as Plackett-Burman design (PBD) and central composite design (CCD). Under the selected optimal conditions, MIP sensor was showed a linear range from 0.06 to 490 μmol L(-1) MTP, a limit of detection of 2.88 nmol L(-1), a highly reproducible response (RSD 3.9%) and a good selectivity in the presence of structurally related molecules. Furthermore, the applicability of the method was successfully tested with determination of MTP in real samples (tablet, and serum). Copyright © 2016 Elsevier B.V. All rights reserved.

Synthesis and characterization of manganese diselenide nanoparticles (MnSeNPs): Determination of capsaicin by using MnSeNP-modified glassy carbon electrode.

PubMed

Sukanya, Ramaraj; Sakthivel, Mani; Chen, Shen-Ming; Chen, Tse-Wei; Al-Hemaid, Fahad M A; Ajmal Ali, M; Elshikh, Mohamed Soliman

2018-06-02

A new type of manganese diselenide nanoparticles (MnSeNPs) was synthesized by using a hydrothermal method. Their surface morphology, crystallinity and elemental distribution were characterized by using transmission electron microscopy, X-ray diffraction, energy dispersive X-ray spectroscopy, and X-ray photoelectron spectroscopy which scrutinize the formation of the NPs. The NPs were coated on a glassy carbon electrode (GCE), and electrochemical impedance spectroscopy, cyclic voltammetry and differential pulse voltammetry were applied to study the electroanalytical properties towards the oxidation of the food additive capsaicin. The modified GCE displays lower charge transfer resistance (R ct  = 29.52 Ω), a larger active surface area (0.089 cm 2 /g, and more efficient electrochemical oxidation of capsaicin compared to a MnS 2 /GCE and a bare GCE. The oxidation peak potential is 0.43 V (vs. Ag/AgCl) which is lower than that of previously reported GCEs. The sensor has a detection limit as low as 0.05 μM and an electrochemical sensitivity of 2.41 μA μM -1  cm -2 . The method was applied to the determination of capsaicin in pepper samples. Graphical abstract Electrochemical determination of capsaicin in pepper extract by using MnSeNPs modified electrode.

Preparation and characterization of reduced graphene oxide supported nickel oxide nanoparticle-based platform for sensor applications

NASA Astrophysics Data System (ADS)

Roychoudhury, Appan; Prateek, Arneish; Basu, Suddhasatwa; Jha, Sandeep Kumar

2018-03-01

A nanostructured composite film comprising reduced graphene oxide (rGO) and nickel oxide (NiO) nanoparticles (NPs) has been prepared and utilized for development of a simple yet efficient sensor for detection of dopamine and epinephrine in a single run. The hybrid material rGO-NiO nanocomposite was synthesized chemically, and the formation of nanocomposite was confirmed via X-ray diffraction (XRD), transmission electron microscopy (TEM), Raman, UV-Vis, and Fourier transform infrared (FTIR) spectroscopic techniques. The incorporation of NiO NPs on rGO support was found to provide improved sensing characteristics at electrode interface due to enhanced electron mobility on rGO sheet and high catalytic activity of NiO NPs. Subsequently, the synthesized rGO-NiO nanocomposite was deposited onto indium tin oxide (ITO)-coated glass substrate by simple drop-casting method, and the electrode was characterized through atomic force microscopy (AFM) and scanning electron microscopic (SEM) studies. After optimization of experimental conditions electrochemically for its high sensitivity, the fabricated rGO-NiO/ITO electrode was used for simultaneous detection of dopamine and epinephrine by square wave voltammetry (SWV) method. The results showed high sensitivity of 0.545 and 0.638 μA/μM for dopamine and epinephrine respectively in a broad linear range of 0.5-50 μM. Moreover, remarkable detection limits of 0.495 and 0.423 μM were found for dopamine and epinephrine, and the developed sensor exhibited a wide separation of 380 mV between the respective detection peaks of dopamine and epinephrine. Beside this, the proposed sensor was successfully applied in presence of high concentration of interfering agents, ascorbic acid and uric acid, and validated with real serum samples.

Effects of Nano-CeO₂ with Different Nanocrystal Morphologies on Cytotoxicity in HepG2 Cells.

PubMed

Wang, Lili; Ai, Wenchao; Zhai, Yanwu; Li, Haishan; Zhou, Kebin; Chen, Huiming

2015-09-02

Cerium oxide nanoparticles (nano-CeO₂) have been reported to cause damage and apoptosis in human primary hepatocytes. Here, we compared the toxicity of three types of nano-CeO₂ with different nanocrystal morphologies (cube-, octahedron-, and rod-like crystals) in human hepatocellular carcinoma cells (HepG2). The cells were treated with the nano-CeO₂ at various concentrations (6.25, 12.5, 25, 50, 100 μg/mL). The crystal structure, size and morphology of nano-CeO₂ were investigated by X-ray diffractometry and transmission electron microscopy. The specific surface area was detected using the Brunauer, Emmet and Teller method. The cellular morphological and internal structure were observed by microscopy; apoptotic alterations were measured using flow cytometry; nuclear DNA, mitochondrial membrane potential (MMP), reactive oxygen species (ROS) and glutathione (GSH) in HepG2 cells were measured using high content screening technology. The scavenging ability of hydroxyl free radicals and the redox properties of the nano-CeO₂ were measured by square-wave voltammetry and temperature-programmed-reduction methods. All three types of nano-CeO₂ entered the HepG2 cells, localized in the lysosome and cytoplasm, altered cellular shape, and caused cytotoxicity. The nano-CeO₂ with smaller specific surface areas induced more apoptosis, caused an increase in MMP, ROS and GSH, and lowered the cell's ability to scavenge hydroxyl free radicals and antioxidants. In this work, our data demonstrated that compared with cube-like and octahedron-like nano-CeO₂, the rod-like nano-CeO₂ has lowest toxicity to HepG2 cells owing to its larger specific surface areas.

Highly efficient electrocatalytic vapor generation of methylmercury based on the gold particles deposited glassy carbon electrode: A typical application for sensitive mercury speciation analysis in fish samples.

PubMed

Shi, Meng-Ting; Yang, Xin-An; Qin, Li-Ming; Zhang, Wang-Bing

2018-09-26

A gold particle deposited glassy carbon electrode (Au/GCE) was first used in electrochemical vapor generation (ECVG) technology and demonstrated to have excellent catalytic property for the electrochemical conversion process of aqueous mercury, especially for methylmercury (CH 3 Hg + ), to gaseous mercury. Systematical research has shown that the highly consistent or distinct difference between the atomic fluorescence spectroscopy signals of CH 3 Hg + and Hg 2+ can be achieved by controlling the electrolytic parameters of ECVG. Hereby, a new green and accurate method for mercury speciation analysis based on the distinguishing electrochemical reaction behavior of Hg 2+ and CH 3 Hg +  on the modified electrode was firstly established. Furthermore, electrochemical impedance spectra and the square wave voltammetry displayed that the ECVG reaction of CH 3 Hg +  may belong to the electrocatalytic mechanism. Under the selected conditions, the limits of detection of Hg 2+ and CH 3 Hg +  are 5.3 ng L -1 and 4.4 ng L -1 for liquid samples and 0.53 pg mg -1 and 0.44 pg mg -1 for solid samples, respectively. The precision of the 5 measurements is less than 6% within the concentration of Hg 2+ and CH 3 Hg +  ranging from 0.2 to 15.0 μg L -1 . The accuracy and practicability of the proposed method was verified by analyzing the mercury content in the certified reference material and several fish as well as water samples. Copyright © 2018 Elsevier B.V. All rights reserved.

Electrochemical biosensor for carbofuran pesticide based on esterases from Eupenicillium shearii FREI-39 endophytic fungus.

PubMed

Grawe, Gregory Ferreira; de Oliveira, Tássia Regina; de Andrade Narciso, Esther; Moccelini, Sally Katiuce; Terezo, Ailton José; Soares, Marcos Antonio; Castilho, Marilza

2015-01-15

In this work, a biosensor was constructed by physical adsorption of the isolated endophytic fungus Eupenicillium shearii FREI-39 esterase on halloysite, using graphite powder, multi-walled carbon nanotubes and mineral oil for the determination of carbofuran pesticide by inhibition of the esterase using square-wave voltammetry (SWV). Specific esterase activities were determined each 2 days over a period of 15 days of growth in four different inoculation media. The highest specific activity was found on 6th day, with 33.08 U on PDA broth. The best performance of the proposed biosensor was obtained using 0.5 U esterase activity. The carbofuran concentration response was linear in the range from 5.0 to 100.0 µg L(-1) (r=0.9986) with detection and quantification limits of 1.69 µg L(-1) and 5.13 µg L(-1), respectively. A recovery study of carbofuran in spiked water samples showed values ranging from 103.8±6.7% to 106.7±9.7%. The biosensor showed good repeatability and reproducibility and remained stable for a period of 20 weeks. The determination of carbofuran in spiked water samples using the proposed biosensor was satisfactory when compared to the chromatographic reference method. The results showed no significant difference at the 95% confidence level with t-test statistics. The application of enzymes from endophytic fungi in constructing biosensors broadens the biotechnological importance of these microorganisms. Copyright © 2014 Elsevier B.V. All rights reserved.

Pre-clinical validation study of a miniaturized electrochemical immunoassay based on square wave voltammetry for early detection of carcinoembryonic antigen in human serum.

PubMed

Martínez-Mancera, Flavio Dolores; García-López, Patricia; Hernández-López, José Luis

2015-04-15

The ELISA format for measuring carcinoembryonic antigen (CEA) serves as a reference standard against which other assays are compared. Because the World Health Organization (WHO) increasingly recommends the use of serum CEA as a diagnostic tool for cancer, it is relevant to explore the reliability of the new decentralized CEA point-of-care-testing (POCT) technologies that are available to physicians and patients, in compliance with mandates of the clinical laboratories' regulatory agencies. Electrochemical immunoassay (ECIA) based on trace lead (Pb) analysis by anodic stripping techniques using sandwich-type immunocomplex conjugates: (MB)Ab/AgCEA/Ab(PbS), and a commercial ELISA test system with optical transmission. The ECIA provides better analytical performance than does the ELISA. The within assay precision coefficient of variance (%CVw) of the ECIA is lower than the value recommended by the Hong Kong Association of Medical Laboratories (HKAML), and the recoveries of CEA at 1.0, 5.0, 10.0, 25.0 and 50.0 ng/ml are in the range of 99-110% for control serum samples. The ECIA showed a minimal positive bias of 0.0267 ± 0.3270 ng/ml (P=0.9389). The proposed CEA screening technology can be practically employed for decentralized clinical analysis of CEA in human serum. Therefore, it can be viewed as a control method for personalized therapy. Copyright © 2015 Elsevier B.V. All rights reserved.

Optimization of Stripping Voltammetric Sensor by a Back Propagation Artificial Neural Network for the Accurate Determination of Pb(II) in the Presence of Cd(II).

PubMed

Zhao, Guo; Wang, Hui; Liu, Gang; Wang, Zhiqiang

2016-09-21

An easy, but effective, method has been proposed to detect and quantify the Pb(II) in the presence of Cd(II) based on a Bi/glassy carbon electrode (Bi/GCE) with the combination of a back propagation artificial neural network (BP-ANN) and square wave anodic stripping voltammetry (SWASV) without further electrode modification. The effects of Cd(II) in different concentrations on stripping responses of Pb(II) was studied. The results indicate that the presence of Cd(II) will reduce the prediction precision of a direct calibration model. Therefore, a two-input and one-output BP-ANN was built for the optimization of a stripping voltammetric sensor, which considering the combined effects of Cd(II) and Pb(II) on the SWASV detection of Pb(II) and establishing the nonlinear relationship between the stripping peak currents of Pb(II) and Cd(II) and the concentration of Pb(II). The key parameters of the BP-ANN and the factors affecting the SWASV detection of Pb(II) were optimized. The prediction performance of direct calibration model and BP-ANN model were tested with regard to the mean absolute error (MAE), root mean square error (RMSE), average relative error (ARE), and correlation coefficient. The results proved that the BP-ANN model exhibited higher prediction accuracy than the direct calibration model. Finally, a real samples analysis was performed to determine trace Pb(II) in some soil specimens with satisfactory results.

Hairy carbon electrodes studied by cyclic voltammetry and battery discharge testing

NASA Technical Reports Server (NTRS)

Chung, Deborah D. L.; Shui, Xiaoping; Frysz, Christine A.

1993-01-01

Hairy carbon is a new material developed by growing submicron carbon filaments on conventional carbon substrates. Typical substrate materials include carbon black, graphite powder, carbon fibers, and glassy carbon. A catalyst is used to initiate hair growth with carbonaceous gases serving as the carbon source. To study the electrochemical behavior of hairy carbons, cyclic voltammetry (CV) and discharge testing were conducted. In both cases, hairy carbon results surpassed those of the substrate material alone.

Quasi-steady-state voltammetry of rapid electron transfer reactions at the macroscopic substrate of the scanning electrochemical microscope.

PubMed

Nioradze, Nikoloz; Kim, Jiyeon; Amemiya, Shigeru

2011-02-01

We report on a novel theory and experiment for scanning electrochemical microscopy (SECM) to enable quasi-steady-state voltammetry of rapid electron transfer (ET) reactions at macroscopic substrates. With this powerful approach, the substrate potential is cycled widely across the formal potential of a redox couple while the reactant or product of a substrate reaction is amperometrically detected at the tip in the feedback or substrate generation/tip collection mode, respectively. The plot of tip current versus substrate potential features the retraceable sigmoidal shape of a quasi-steady-state voltammogram although a transient voltammogram is obtained at the macroscopic substrate. Finite element simulations reveal that a short tip-substrate distance and a reversible substrate reaction (except under the tip) are required for quasi-steady-state voltammetry. Advantageously, a pair of quasi-steady-state voltammograms is obtained by employing both operation modes to reliably determine all transport, thermodynamic, and kinetic parameters as confirmed experimentally for rapid ET reactions of ferrocenemethanol and 7,7,8,8-tetracyanoquinodimethane at a Pt substrate with ∼0.5 μm-radius Pt tips positioned at 90 nm-1 μm distances. Standard ET rate constants of ∼7 cm/s were obtained for the latter mediator as the largest determined for a substrate reaction by SECM. Various potential applications of quasi-steady-state voltammetry are also proposed.

Structural transformation during Li/Na insertion and theoretical cyclic voltammetry of the δ-NH4V4O10 electrode: a first-principles study.

PubMed

Sarkar, Tanmay; Kumar, Parveen; Bharadwaj, Mridula Dixit; Waghmare, Umesh

2016-04-14

A double layer δ-NH4V4O10, due to its high energy storage capacity and excellent rate capability, is a very promising cathode material for Li-ion and Na-ion batteries for large-scale renewable energy storage in transportation and smart grids. While it possesses better stability, and higher ionic and electronic conductivity than the most widely explored V2O5, the mechanisms of its cyclability are yet to be understood. Here, we present a theoretical cyclic voltammetry as a tool based on first-principles calculations, and uncover structural transformations that occur during Li(+)/Na(+) insertion (x) into (Lix/Nax)NH4V4O10. Structural distortions associated with single-phase and multi-phase structural changes during the insertion of Li(+)/Na(+), identified through the analysis of voltage profile and theoretical cyclic voltammetry are in agreement with the reported experimental electrochemical measurements on δ-NH4V4O10. We obtain an insight into its electronic structure with a lower band gap that is responsible for the high rate capability of (Lix/Nax) δ-NH4V4O10. The scheme of theoretical cyclic voltammetry presented here will be useful for addressing issues of cyclability and energy rate in other electrode materials.

Rotating Disk Slurry Au Electrodeposition at Unsupported Carbon Vulcan XC-72 and Ce 3+ Impregnation for Ethanol Oxidation in Alkaline Media

DOE PAGES

Betancourt, Luis E.; Guzman-Blas, Rolando; Luo, Si; ...

2016-11-19

A robust electrodeposition method consisting of the rotating disk slurry electrode (RoDSE) technique to obtain Au nanoparticles highly dispersed on a conductive carbonaceous support, i.e., Vulcan XC-72R, for ethanol electrooxidation reaction in alkaline media was developed. Ceria was used as a cocatalyst using a Ce(III)-EDTA impregnation method in order to enhance the catalytic activity and improve the catalyst’s overall stability. Furthermore, the RoDSE method used to obtain highly dispersed Au nanoparticles does not require the use of a reducing agent or stabilizing agent, and the noble-metal loading was controlled by the addition and tuning of the metal precursor concentration. Inductivelymore » coupled plasma and thermogravimetric analysis indicated that the Au loading in the catalyst was 9 %. We determined the particle size and characteristic Au fcc crystal facets by X-ray diffraction. The morphology of the catalyst was also investigated using electron microscopy techniques. In addition, X-ray absorption spectroscopy was used to corroborate the presence and identify the oxidation state of Ce in the system and to observe if there are any electronic interactions within the 8 % Au/CeO x/C system. Cyclic voltammetry of electrodeposited 9 % Au/C and Ce-promoted 8 % Au/C showed a higher catalytic current density for ethanol oxidation when compared with commercially available catalysts (20 % Au/C) of a higher precious metal loading. Additionally, we report a higher stability toward the ethanol electrooxidation process, which was corroborated by 1 mV/s linear sweep voltammetry and chronoamperometric studies.« less

Optimizing the Temporal Resolution of Fast-Scan Cyclic Voltammetry

PubMed Central

2012-01-01

Electrochemical detection with carbon-fiber microelectrodes has become an established method to monitor directly the release of dopamine from neurons and its uptake by the dopamine transporter. With constant potential amperometry (CPA), the measured current provides a real time view of the rapid concentration changes, but the method lacks chemical identification of the monitored species and markedly increases the difficulty of signal calibration. Monitoring with fast-scan cyclic voltammetry (FSCV) allows species identification and concentration measurements but often exhibits a delayed response time due to the time-dependent adsorption/desorption of electroactive species at the electrode. We sought to improve the temporal resolution of FSCV to make it more comparable to CPA by increasing the waveform repetition rate from 10 to 60 Hz with uncoated carbon-fiber electrodes. The faster acquisition led to diminished time delays of the recordings that tracked more closely with CPA measurements. The measurements reveal that FSCV at 10 Hz underestimates the normal rate of dopamine uptake by about 18%. However, FSCV collection at 10 and 60 Hz provide identical results when a dopamine transporter (DAT) blocker such as cocaine is bath applied. To verify further the utility of this method, we used transgenic mice that overexpress DAT. After accounting for the slight adsorption delay time, FSCV at 60 Hz adequately monitored the increased uptake rate that arose from overexpression of DAT and, again, was similar to CPA results. Furthermore, the utility of collecting data at 60 Hz was verified in an anesthetized rat by using a higher scan rate (2400 V/s) to increase sensitivity and the overall signal. PMID:22708011

A baseline drift detrending technique for fast scan cyclic voltammetry.

PubMed

DeWaele, Mark; Oh, Yoonbae; Park, Cheonho; Kang, Yu Min; Shin, Hojin; Blaha, Charles D; Bennet, Kevin E; Kim, In Young; Lee, Kendall H; Jang, Dong Pyo

2017-11-06

Fast scan cyclic voltammetry (FSCV) has been commonly used to measure extracellular neurotransmitter concentrations in the brain. Due to the unstable nature of the background currents inherent in FSCV measurements, analysis of FSCV data is limited to very short amounts of time using traditional background subtraction. In this paper, we propose the use of a zero-phase high pass filter (HPF) as the means to remove the background drift. Instead of the traditional method of low pass filtering across voltammograms to increase the signal to noise ratio, a HPF with a low cutoff frequency was applied to the temporal dataset at each voltage point to remove the background drift. As a result, the HPF utilizing cutoff frequencies between 0.001 Hz and 0.01 Hz could be effectively used to a set of FSCV data for removing the drifting patterns while preserving the temporal kinetics of the phasic dopamine response recorded in vivo. In addition, compared to a drift removal method using principal component analysis, this was found to be significantly more effective in reducing the drift (unpaired t-test p < 0.0001, t = 10.88) when applied to data collected from Tris buffer over 24 hours although a drift removal method using principal component analysis also showed the effective background drift reduction. The HPF was also applied to 5 hours of FSCV in vivo data. Electrically evoked dopamine peaks, observed in the nucleus accumbens, were clearly visible even without background subtraction. This technique provides a new, simple, and yet robust, approach to analyse FSCV data with an unstable background.

Electrodeposited Mn-Sn-X Alloys for Corrosion Protection Coatings

DTIC Science & Technology

2002-09-30

amount of tin and oxygen (Figure 7, right), and possess an amorphous structure. The addition of tartrate , EDTA or gluconate suppresses Mn reduction...pH 6.4-6.6 and 2.6-2.8, and at different cupric ion concentrations is conducted by using cathodic potentiodynamic and cyclic voltammetry methods...in the form of MnOx(OH)2-x⋅nH2O, where x increases and n decreases with depth. The effect of the variation of cupric ion concentration ([Cu2+]) on

Investigation on VOX/CNTS Nanocomposites Act as Electrode of Supercapacitors

NASA Astrophysics Data System (ADS)

Zhu, Quanyao; Li, Zhaolong; Zhang, Xiaoyan; Huang, Shengnan; Yu, Yue; Chen, Wen; Zakharova, Galina S.

2013-07-01

The VOx/CNTs nanocomposites were synthesized by the hydrothermal method. The structure and morphologies of the nanocomposites were characteristic by XRD, SEM and TEM. The electrochemical properties of the nanocomposites were explored by cyclic voltammetry, constant current charge/discharge testing and electrochemical impedance spectroscopy in 1M KNO3 aqueous solution. The results showed that the nanocomposites perform characteristics of electrical both double-layer capacitance and pseudocapacitance. The specific capacitances were 136.5F/g, when the current density was 0.15A/g.

Study of influence of various factors on electrochemical signal of lead in water solutions

NASA Astrophysics Data System (ADS)

Zhikharev, Yu N.; Andrianova, L. I.; Ogudova, E. V.

2018-05-01

The conditions for obtaining a reproducible signal of lead in water solutions of indifferent electrolytes on various substrates (working electrodes) for analytical purposes were studied. Attention was also paid to studying the regularities of the initial stage of formation of lead sediments by the method of inversion voltammetry. The possibility of using different working electrodes to obtain stable current-potential curves is shown depending on the conditions of electrolysis, pH of the medium, the electrolysis potential and impurities.

Theoretical and experimental prediction of the redox potentials of metallocene compounds

NASA Astrophysics Data System (ADS)

Li, Ya-Ping; Liu, Hai-Bo; Liu, Tao; Yu, Zhang-Yu

2017-11-01

The standard redox electrode potential ( E°) values of metallocene compounds are obtained theoretically with density functional theory (DFT) method at B3LYP/6-311++G( d, p) level and experimentally with cyclic voltammetry (CV). The theoretical E° values of metallocene compounds are in good agreement with experimental ones. We investigate the substituent effects on the redox properties of metallocene compounds. Among the four metallocene compounds, the E° values is largest for titanocene dichloride and smallest for ferrocene.

Linear-sweep voltammetry of a soluble redox couple in a cylindrical electrode

NASA Technical Reports Server (NTRS)

Weidner, John W.

1991-01-01

An approach is described for using the linear sweep voltammetry (LSV) technique to study the kinetics of flooded porous electrodes by assuming a porous electrode as a collection of identical noninterconnected cylindrical pores that are filled with electrolyte. This assumption makes possible to study the behavior of this ideal electrode as that of a single pore. Alternatively, for an electrode of a given pore-size distribution, it is possible to predict the performance of different pore sizes and then combine the performance values.

Channel microband electrode arrays for mechanistic electrochemistry. Two-dimensional voltammetry:  transport-limited currents.

PubMed

Alden, J A; Feldman, M A; Hill, E; Prieto, F; Oyama, M; Coles, B A; Compton, R G; Dobson, P J; Leigh, P A

1998-05-01

A channel electrode array, with electrodes ranging in size from the millimeter to the submicrometer scale, is used for the amperometric interrogation of mechanistically complex electrode processes. In this way, the transport-limited current, measured as a function of both electrode size and electrolyte flow rate (convection), is shown to provide a highly sensitive probe of mechanism and kinetics. The application of "two-dimensional voltammetry" to diverse electrode processes, including E, ECE, ECEE, EC', and DISP2 reactions, is reported.

Probing biological redox chemistry with large amplitude Fourier transformed ac voltammetry

PubMed Central

Adamson, Hope

2017-01-01

Biological electron-exchange reactions are fundamental to life on earth. Redox reactions underpin respiration, photosynthesis, molecular biosynthesis, cell signalling and protein folding. Chemical, biomedical and future energy technology developments are also inspired by these natural electron transfer processes. Further developments in techniques and data analysis are required to gain a deeper understanding of the redox biochemistry processes that power Nature. This review outlines the new insights gained from developing Fourier transformed ac voltammetry as a tool for protein film electrochemistry. PMID:28804798

Fabrication of Porous Carbon-based Nanostructure for Energy Storage and Transfer Applications

DTIC Science & Technology

2014-06-09

in the voltage range of 3.0 to 0.005 V (versus Li/Li+). Cyclic voltammetry (CV) was performed on a computer controlled MacPile II unit (Biological...performed at current density of 37mAg–1, voltage: 3.0-0.005V vs. Li/Li+. Cyclic voltammetry was performed at a scan rate of 58 µs/V. Red plots...pseudocapacitve storage behaviour of the electrode.19 The Li storage mechanism of both electrodes can also be studied carefully by slow scanning cyclic

Detection of the Pseudomonas Quinolone Signal (PQS) by cyclic voltammetry and amperometry using a boron doped diamond electrode.

PubMed

Zhou, Lin; Glennon, Jeremy D; Luong, John H T; Reen, F Jerry; O'Gara, Fergal; McSweeney, Christina; McGlacken, Gerard P

2011-10-07

2-Heptyl-3-hydroxy-4-quinolone, known as the Pseudomonas Quinolone Signal, is a key regulator of bacterial cooperative behaviour known as quorum sensing. A simple electrochemical strategy was employed for its sensitive detection using a bare boron-doped diamond electrode by cyclic voltammetry and amperometry. PQS (and potentially other quinolones) was then detected in cultures of P. aeruginosa pqsL(-) mutant strains. This journal is © The Royal Society of Chemistry 2011

GEOPHYSICS, ASTRONOMY AND ASTROPHYSICS: Numerical method of studying nonlinear interactions between long waves and multiple short waves

NASA Astrophysics Data System (ADS)

Xie, Tao; Kuang, Hai-Lan; William, Perrie; Zou, Guang-Hui; Nan, Cheng-Feng; He, Chao; Shen, Tao; Chen, Wei

2009-07-01

Although the nonlinear interactions between a single short gravity wave and a long wave can be solved analytically, the solution is less tractable in more general cases involving multiple short waves. In this work we present a numerical method of studying nonlinear interactions between a long wave and multiple short harmonic waves in infinitely deep water. Specifically, this method is applied to the calculation of the temporal and spatial evolutions of the surface elevations in which a given long wave interacts with several short harmonic waves. Another important application of our method is to quantitatively analyse the nonlinear interactions between an arbitrary short wave train and another short wave train. From simulation results, we obtain that the mechanism for the nonlinear interactions between one short wave train and another short wave train (expressed as wave train 2) leads to the energy focusing of the other short wave train (expressed as wave train 3). This mechanism occurs on wave components with a narrow frequency bandwidth, whose frequencies are near that of wave train 3.

Application of a palladium hexacyanoferrate film-modified aluminum electrode to electrocatalytic oxidation of hydrazine.

PubMed

Razmi, Habib; Azadbakht, Azadeh; Sadr, Moayad Hossaini

2005-11-01

A palladium hexacyanoferrate (PdHCF) film as an electrocatalytic material was obtained at an aluminum (Al) electrode by a simple electroless dipping method. The modified Al electrode demonstrated a well-behaved redox couple due to the redox reaction of the PdHCF film. The PdHCF film showed an excellent electrocatalytic activity toward the oxidation of hydrazine. The electrocatalytic oxidation of hydrazine was studied by cyclic voltammetry and rotating disk electrode voltammetry techniques. A calibration graph obtained for the hydrazine consisted of two segments (localized at concentration ranges 0.39-10 and 20-75 mM). The rate constant k and transfer coefficient alpha for the catalytic reaction and the diffusion coefficient of hydrazine in the solution D, were found to be 3.11 x 10(3) M(-1) s(-1), 0.52 and 8.03 x 10(-6) cm2 s(-1) respectively. The modified electrode was used to amperometric determination of hydrazine in photographic developer. The interference of ascorbic acid and thiosulfate were investigated and greatly reduced using a thin film of Nafion on the modified electrode. The modified electrode indicated reproducible behavior and a high level of stability during electrochemical experiments, making it particularly suitable for analytical purposes.

An Investigation of Methyl Viologen Functionalized Reduced Graphene Oxide: Chitosan as a Support for Pt Nanoparticles Towards Ethanol Electrooxidation

NASA Astrophysics Data System (ADS)

Ekrami-Kakhki, Mehri-Saddat; Farzaneh, Nahid; Abbasi, Sedigheh; Beitollahi, Hadi; Ekrami-Kakhki, Seyed Ali

2018-05-01

In this research, graphene oxide was prepared by a modified Hummers' method, and then functionalized with 1, 1'-dimethyl-4, 4'-bipyridinium dichloride (MV), and chitosan (CH) to get a MV-RGO-CH support. Pt nanoparticles were prepared on this support to get Pt/MV-RGO-CH catalyst. The morphology and microstructure of Pt/MV-RGO-CH catalyst were characterized with transmission electron microscopy image and X-ray diffraction analysis. The electrocatalytic activity of the prepared catalyst towards ethanol oxidation was investigated by carbon monoxide stripping voltammetry, cyclic voltammetry, and electrochemical impedance spectroscopy techniques. The effects of some experimental parameters such as scan rate, ethanol concentration, and temperature were investigated for ethanol electrooxidation at Pt/MV-RGO-CH catalyst. Durability of the catalyst was also investigated. The electrocatalytic performance of Pt/MV-RGO-CH catalyst for ethanol oxidation was compared with those of Pt/CH and Pt/MV-RGO catalysts. The higher electrocatalytic performance of Pt/MV-RGO-CH than Pt/CH and Pt/MV-RGO catalysts towards ethanol electrooxidation indicated that Pt/MV-RGO-CH could be a promising catalyst for application in direct ethanol fuel cells.

Synergetic signal amplification of multi-walled carbon nanotubes-Fe3O4 hybrid and trimethyloctadecylammonium bromide as a highly sensitive detection platform for tetrabromobisphenol A

PubMed Central

Zhou, Feng; Wang, Yue; Wu, Wei; Jing, Tao; Mei, Surong; Zhou, Yikai

2016-01-01

In this work, we fabricated an electrochemical sensor based on trimethyloctadecylammonium bromide and multi-walled carbon nanotubes-Fe3O4 hybrid (TOAB/MWCNTs-Fe3O4) for sensitive detection of tetrabromobisphenol A (TBBPA). The nanocomposite was characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and Fourier transform infrared spectroscopy (FT-IR) techniques. The electrochemical behaviors of TBBPA on TOAB/MWCNTs-Fe3O4 composite film modified glassy carbon electrode (GCE) were investigated by cyclic voltammetry (CV), differential pulse voltammetry (DPV) and electrochemical impedance spectroscopy (EIS) method. The experimental results indicated that the incorporation of MWCNTs-Fe3O4 with TOAB greatly enhanced the electrochemical response of TBBPA. This fabricated sensor displayed excellent analytical performance for TBBPA detection over a range from 3.0 nM to 1000.0 nM with a detection limit of 0.73 nM (S/N = 3). Moreover, the proposed electrochemical sensor exhibited good reproducibility and stability, and could be successfully applied to detect TBBPA in water samples with satisfactory results. PMID:27897238

Synthesis, characterization and DNA-binding studies of mono and heterobimetallic complexes Cu sbnd Sn 2/Zn sbnd Sn 2 and their DNA cleavage activity

NASA Astrophysics Data System (ADS)

Arjmand, Farukh; Sayeed, Fatima

2010-02-01

Heterobimetallic complexes C 6H 24N 4O 6CuSn 2Cl 63, C 6H 24N 4O 6ZnSn 2Cl 64 have been synthesized from their monometallic analogs C 6H 16N 4O 2CuCl 21, C 6H 16N 4O 2ZnCl 22, and were characterized by various spectroscopic and analytical methods. The complexes 1-4 reveal an octahedral geometry for both central metal ions Cu/Zn as well as for Sn metal ion. The interaction of complexes 1-4 with CT-DNA, were investigated by using absorption, emission, cyclic voltammetry, viscometry and DNA cleavage studies. The emission quenching of 3 and 4 by [Fe(CN) 6] 4- depressed greatly when bound to CT-DNA. The results of spectroscopic, viscometric and cyclic voltammetry of complexes 3 and 4 revealed electrostatic mode of binding of the complexes with CT-DNA. These results revealed that 4 bind more avidly in comparison to 3 with CT-DNA. Gel electrophoresis of DNA with complexes 3 and 4 demonstrated that the complexes exhibit excellent cleavage activity under physiological conditions.

Preparation of TiO2-Decorated Boron Particles by Wet Ball Milling and their Photoelectrochemical Hydrogen and Oxygen Evolution Reactions

PubMed Central

Jung, Hye Jin; Nam, Kyusuk; Sung, Hong-Gye; Hyun, Hyung Soo; Sohn, Youngku; Shin, Weon Gyu

2016-01-01

TiO2-coated boron particles were prepared by a wet ball milling method, with the particle size distribution and average particle size being easily controlled by varying the milling operation time. Based on the results from X-ray photoelectron spectroscopy, transmission electron microscopy, energy dispersive X-ray analysis, and Fourier transform infrared spectroscopy, it was confirmed that the initial oxide layer on the boron particles surface was removed by the wet milling process, and that a new B–O–Ti bond was formed on the boron surface. The uniform TiO2 layer on the 150 nm boron particles was estimated to be 10 nm thick. Based on linear sweep voltammetry, cyclic voltammetry, current-time amperometry, and electrochemical impedance analyses, the potential for the application of TiO2-coated boron particles as a photoelectrochemical catalyst was demonstrated. A current of 250 μA was obtained at a potential of 0.5 V for hydrogen evolution, with an onset potential near to 0.0 V. Finally, a current of 220 μA was obtained at a potential of 1.0 V for oxygen evolution. PMID:28774132

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

PubMed

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

2014-06-01

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

Preparation of NiCoP Hollow Quasi-Polyhedra and Their Electrocatalytic Properties for Hydrogen Evolution in Alkaline Solution.

PubMed

Li, Yapeng; Liu, Jindou; Chen, Chen; Zhang, Xiaohua; Chen, Jinhua

2017-02-22

Double metal phosphide (NiCoP) with hollow quasi-polyhedron structure was prepared by acidic etching and precipitation of ZIF-67 polyhedra and further phosphorization treatment with NaH 2 PO 2 . The morphology and microstructure of NiCoP quasi-polyhedron and its precursors were investigated by scanning electron microscopy, transmission electron microscopy, X-ray diffraction, and a micropore and chemisorption analyzer. Electrocatalytic properties were examined by typical electrochemical methods, such as linear sweep voltammetry, cyclic voltammetry, chronoamperometry, and electrochemical impedance spectroscopy in 1.0 M KOH aqueous solution. Results reveal that, compared with CoP hollow polyhedra, NiCoP hollow quasi-polyhedra exhibit better electrochemical properties for hydrogen evolution with a low onset overpotential of 74 mV and a small Tafel slope of 42 mV dec -1 . When the current density is 10 mA cm -2 , the corresponding overpotential is merely 124 mV, and 93% of its electrocatalytic activity can be maintained for 12 h. This indicates that NiCoP with hollow quasi-polyhedron structure, bimetallic merit, and low cost may be a good candidate as electrocatalyst in the practical application of hydrogen evolution.

A new electrochemical sensor for the simultaneous determination of acetaminophen and codeine based on porous silicon/palladium nanostructure.

PubMed

Ensafi, Ali A; Ahmadi, Najmeh; Rezaei, Behzad; Abarghoui, Mehdi Mokhtari

2015-03-01

A porous silicon/palladium nanostructure was prepared and used as a new electrode material for the simultaneous determination of acetaminophen (ACT) and codeine (COD). Palladium nanoparticles were assembled on porous silicon (PSi) microparticles by a simple redox reaction between the Pd precursor and PSi in an aqueous solution of hydrofluoric acid. This novel nanostructure was characterized by different spectroscopic and electrochemical techniques including scanning electron microscopy, X-ray diffraction, energy dispersive X-ray spectroscopy, fourier transform infrared spectroscopy and cyclic voltammetry. The high electrochemical activity, fast electron transfer rate, high surface area and good antifouling properties of this nanostructure enhanced the oxidation peak currents and reduced the peak potentials of ACT and COD at the surface of the proposed sensor. Simultaneous determination of ACT and COD was explored using differential pulse voltammetry. A linear range of 1.0-700.0 µmol L(-1) was achieved for ACT and COD with detection limits of 0.4 and 0.3 µmol L(-1), respectively. Finally, the proposed method was used for the determination of ACT and COD in blood serum, urine and pharmaceutical compounds. Copyright © 2014 Elsevier B.V. All rights reserved.

The nanostructure of microbially-reduced graphene oxide fosters thick and highly-performing electrochemically-active biofilms

NASA Astrophysics Data System (ADS)

Virdis, Bernardino; Dennis, Paul G.

2017-07-01

Biofilms of electrochemically-active organisms are used in microbial electrochemical technologies (METs) to catalyze bioreactions otherwise not possible at bare electrodes. At present, however, achievable current outputs are still below levels considered sufficient for economic viability of large-scale METs implementations. Here, we report three-dimensional, self-aggregating biofilm composites comprising of microbial cells embedded with microbially-reduced graphene oxide (rGO) nanoparticles to form a thick macro-porous network with superior electrochemical properties. In the presence of metabolic substrate, these hybrid biofilms are capable of producing up to five times more catalytic current than the control biofilms. Cyclic voltammetry, linear sweep voltammetry, and electrochemical impedance spectroscopy, show that in spite of the increased thickness, the biofilms amended with GO display lower polarization/charge transfer resistance compared to the controls, which we ascribe to the incorporation of rGO into the biofilms, which (1) promotes fast electron transfer, yet conserving a macroporous structure that allows free diffusion of reactants and products, and (2) enhances the interfacial dynamics by allowing a higher load of microbial cells per electrode surface area. These results suggest an easy-to-apply and cost-effective method to produce high-performing electrochemically-active biofilms in situ.

Improvement of amperometric transducer selectivity using nanosized phenylenediamine films

NASA Astrophysics Data System (ADS)

Soldatkina, O. V.; Kucherenko, I. S.; Pyeshkova, V. M.; Alekseev, S. A.; Soldatkin, O. O.; Dzyadevych, S. V.

2017-11-01

In this work, we studied the conditions of deposition of a semipermeable polyphenylenediamine (PPD)-based membrane on amperometric disk platinum electrodes. Restricting an access of interfering substances to the electrode surface, the membrane prevents their impact on the sensor operation. Two methods of membrane deposition by electropolymerization were compared—at varying potential (cyclic voltammetry) and at constant potential. The cyclic voltammetry was shown to be easier in performing and providing better properties of the membrane. The dependence of PPD membrane effectiveness on the number of cyclic voltammograms and phenylenediamine concentration was analyzed. It was shown that the impact of interfering substances (ascorbic acid, dopamine, cysteine, uric acid) on sensor operation could be completely avoided using three cyclic voltammograms in 30 mM phenylenediamine. On the other hand, when working with diluted samples, i.e., at lower concentrations of electroactive substances, it is reasonable to decrease the phenylenediamine concentration to 5 mM, which would result in a higher sensitivity of transducers to hydrogen peroxide due to a thinner PPD layer. The PPD membrane was tested during continuous operation and at 8-day storage and turned out to be efficient in sensor and biosensors.

An electrocatalytic oxidation and voltammetric method using a chemically reduced graphene oxide film for the determination of caffeic acid.

PubMed

Vilian, A T Ezhil; Chen, Shen-Ming; Chen, Ying-Hui; Ali, M Ajmal; Al-Hemaid, Fahad M A

2014-06-01

The present work describes the characterization of a chemically reduced graphene oxide (CRGO) modified glassy carbon electrode (GCE) for electrochemical investigation of caffeic acid (CA). Cyclic voltammetry (CV), differential pulse voltammetry (DPV), amperometry, and electrochemical impedance spectroscopy (EIS) techniques were used to characterize the properties of the electrode. There was an obvious enhancement of the current response and a decreased over potential for the oxidation of CA. The interfacial electron transfer rate of CA was studied by EIS. Under optimal conditions, the CRGO displayed a linear response range of 1×10(-8) to 8×10(-4) M and the detection limit was 2×10(-9) M (S/N=3), with a sensitivity of 192.21 μA mM(-1) cm(-2) at an applied potential of +0.2V (vs. Ag/AgCl reference), which suggests that the CRGO is a promising sensing materials for the electrochemical investigation of CA. The results showed the good sensitivity, selectivity and high reproducibility of the CRGO modified electrode. Moreover, this modified electrode was further applied to investigate the CA in real samples of wine with satisfactory results. Copyright © 2014 Elsevier Inc. All rights reserved.

Enhanced Kinetics of Electrochemical Hydrogen Uptake and Release by Palladium Powders Modified by Electrochemical Atomic Layer Deposition

DOE PAGES

Benson, David M.; Tsang, Chu F.; Sugar, Joshua Daniel; ...

2017-04-28

One method for the formation of nanofilms of materials, is Electrochemical atomic layer deposition (E-ALD), one atomic layer at a time. It uses the galvanic exchange of a less noble metal, deposited using underpotential deposition (UPD), to produce an atomic layer of a more noble element by reduction of its ions. This process is referred to as surface limited redox replacement and can be repeated in a cycle to grow thicker deposits. Previously, we performed it on nanoparticles and planar substrates. In the present report, E-ALD is applied for coating a submicron-sized powder substrate, making use of a new flowmore » cell design. E-ALD is used to coat a Pd powder substrate with different thicknesses of Rh by exchanging it for Cu UPD. Furthermore, cyclic voltammetry and X-ray photoelectron spectroscopy indicate an increasing Rh coverage with increasing numbers of deposition cycles performed, in a manner consistent with the atomic layer deposition (ALD) mechanism. Cyclic voltammetry also indicated increased kinetics of H sorption and desorption in and out of the Pd powder with Rh present, relative to unmodified Pd.« less

Amplified and in situ detection of redox-active metabolite using a biobased redox capacitor.

PubMed

Kim, Eunkyoung; Gordonov, Tanya; Bentley, William E; Payne, Gregory F

2013-02-19

Redox cycling provides a mechanism to amplify electrochemical signals for analyte detection. Previous studies have shown that diverse mediators/shuttles can engage in redox-cycling reactions with a biobased redox capacitor that is fabricated by grafting redox-active catechols onto a chitosan film. Here, we report that redox cycling with this catechol-chitosan redox capacitor can amplify electrochemical signals for detecting a redox-active bacterial metabolite. Specifically, we studied the redox-active bacterial metabolite pyocyanin that is reported to be a virulence factor and signaling molecule for the opportunistic pathogen P. aeruginosa. We demonstrate that redox cycling can amplify outputs from various electrochemical methods (cyclic voltammetry, chronocoulometry, and differential pulse voltammetry) and can lower the detection limit of pyocyanin to 50 nM. Further, the compatibility of this biobased redox capacitor allows the in situ monitoring of the production of redox-active metabolites (e.g., pyocyanin) during the course of P. aeruginosa cultivation. We anticipate that the amplified output of redox-active virulence factors should permit an earlier detection of life-threatening infections by the opportunistic pathogen P. aeruginosa while the "bio-compatibility" of this measurement approach should facilitate in situ study of the spatiotemporal dynamics of bacterial redox signaling.

Gold-mercaptopropionic acid-polyethylenimine composite based DNA sensor for early detection of rheumatic heart disease.

PubMed

Singh, Swati; Kaushal, Ankur; Khare, Shashi; Kumar, Pradeep; Kumar, Ashok

2014-07-21

The first gold-mercaptopropionic acid-polyethylenimine composite based electrochemical DNA biosensor was fabricated for the early detection of Streptococcus pyogenes infection in humans causing rheumatic heart disease (heart valve damage). No biosensor is available for the detection of rheumatic heart disease (RHD). Therefore, the mga gene based sensor was developed by the covalent immobilization of a 5'-carboxyl modified single stranded DNA probe onto the gold composite electrode. The immobilized probe was hybridized with the genomic DNA (G-DNA) of S. pyogenes from throat swabs and the electrochemical response was measured by cyclic voltammetry (CV), differential pulse voltammetry (DPV) and electrochemical impedance (EI). Covalent immobilization of the probe onto the gold composite and its hybridization with G-DNA was characterized by FTIR and SEM. The sensitivity of the sensor was 110.25 μA cm(-2) ng(-1) with DPV and the lower limit of detection was 10 pg per 6 μL. The sensor was validated with patient throat swab samples and results were compared with available methods. The sensor is highly specific to S. pyogenes and can prevent damage to heart valves by the early detection of the infection in only 30 min.

Intramolecular proton transfer boosts water oxidation catalyzed by a Ru complex

DOE Office of Scientific and Technical Information (OSTI.GOV)

Matheu, Roc; Ertem, Mehmed Z.; Benet-Buchholz, J.

We introduce a new family of complexes with the general formula [Ru n(tda)(py)2] m+ (n = 2, m = 0, 1; n = 3, m = 1, 2 +; n = 4, m = 2, 3 2+), with tda 2– being [2,2':6',2"-terpyridine]-6,6"-dicarboxylate, including complex [Ru IV(OH)(tda-κ-N 3O)(py) 2] +, 4H +, which we find to be an impressive water oxidation catalyst, formed by hydroxo coordination to 3 2+ under basic conditions. The complexes are synthesized, isolated, and thoroughly characterized by analytical, spectroscopic (UV–vis, nuclear magnetic resonance, electron paramagnetic resonance), computational, and electrochemical techniques (cyclic voltammetry, differential pulse voltammetry, coulometry), includingmore » solid-state monocrystal X-ray diffraction analysis. In oxidation state IV, the Ru center is seven-coordinated and diamagnetic, whereas in oxidation state II, the complex has an unbonded dangling carboxylate and is six-coordinated while still diamagnetic. With oxidation state III, the coordination number is halfway between the coordination of oxidation states II and IV. Species generated in situ have also been characterized by spectroscopic, computational, and electrochemical techniques, together with the related species derived from a different degree of protonation and oxidation states. 4H + can be generated potentiometrically, or voltammetrically, from 3 2+, and both coexist in solution. While complex 3 2+ is not catalytically active, the catalytic performance of complex 4H + is characterized by the foot of the wave analysis, giving an impressive turnover frequency record of 8000 s –1 at pH 7.0 and 50,000 s –1 at pH 10.0. Density functional theory calculations provide a complete description of the water oxidation catalytic cycle of 4H +, manifesting the key functional role of the dangling carboxylate in lowering the activation free energies that lead to O–O bond formation.« less

Intramolecular proton transfer boosts water oxidation catalyzed by a Ru complex

DOE PAGES

Matheu, Roc; Ertem, Mehmed Z.; Benet-Buchholz, J.; ...

2015-07-30

We introduce a new family of complexes with the general formula [Ru n(tda)(py)2] m+ (n = 2, m = 0, 1; n = 3, m = 1, 2 +; n = 4, m = 2, 3 2+), with tda 2– being [2,2':6',2"-terpyridine]-6,6"-dicarboxylate, including complex [Ru IV(OH)(tda-κ-N 3O)(py) 2] +, 4H +, which we find to be an impressive water oxidation catalyst, formed by hydroxo coordination to 3 2+ under basic conditions. The complexes are synthesized, isolated, and thoroughly characterized by analytical, spectroscopic (UV–vis, nuclear magnetic resonance, electron paramagnetic resonance), computational, and electrochemical techniques (cyclic voltammetry, differential pulse voltammetry, coulometry), includingmore » solid-state monocrystal X-ray diffraction analysis. In oxidation state IV, the Ru center is seven-coordinated and diamagnetic, whereas in oxidation state II, the complex has an unbonded dangling carboxylate and is six-coordinated while still diamagnetic. With oxidation state III, the coordination number is halfway between the coordination of oxidation states II and IV. Species generated in situ have also been characterized by spectroscopic, computational, and electrochemical techniques, together with the related species derived from a different degree of protonation and oxidation states. 4H + can be generated potentiometrically, or voltammetrically, from 3 2+, and both coexist in solution. While complex 3 2+ is not catalytically active, the catalytic performance of complex 4H + is characterized by the foot of the wave analysis, giving an impressive turnover frequency record of 8000 s –1 at pH 7.0 and 50,000 s –1 at pH 10.0. Density functional theory calculations provide a complete description of the water oxidation catalytic cycle of 4H +, manifesting the key functional role of the dangling carboxylate in lowering the activation free energies that lead to O–O bond formation.« less

Influence of the different carbon nanotubes on the development of electrochemical sensors for bisphenol A.

PubMed

Goulart, Lorena Athie; de Moraes, Fernando Cruz; Mascaro, Lucia Helena

2016-01-01

Different methods of functionalisation and the influence of the multi-walled carbon nanotube sizes were investigated on the bisphenol A electrochemical determination. Samples with diameters of 20 to 170 nmwere functionalized in HNO3 5.0 mol L(-1) and a concentrated sulphonitric solution. The morphological characterisations before and after acid treatment were carried out by scanning electron microscopy and cyclic voltammetry. The size and acid treatment affected the oxidation of bisphenol A. The multi-walled carbon nanotubes with a 20-40 nm diameter improved the method sensitivity and achieved a detection limit for determination of bisphenol A at 84.0 nmol L(-1).

Sol gel method for synthesis of semiconducting ferrite and the study of FTIR, DTA, SEM and CV

NASA Astrophysics Data System (ADS)

Alva, Sagir; Hua, Tang Ing; Kalmar Nizar, Umar; Wahyudi, Haris; Sundari, Rita

2018-03-01

In this study, a sol gel method using citric acid as anionic surfactant is used for synthesis of magnesium ferrite. Calcinations of magnesium ferrite at temperature (300°C, 600°C and 800°C) have been conducted after sol gel process. Characterization study of the prepared magnesium ferrite related to calcinations using Fourier transform infrared spectrometry (FTIR), Differential thermogravic analysis (DTA), and Scanning electron microscope (SEM) has been discussed. The study of Cyclic voltammetry (CV) of the prepared magnesium ferrite has been examined to assay the semiconducting behavior of magnesium ferrite in relation to its electrochemical behavior.

A joint method to retrieve directional ocean wave spectra from SAR and wave spectrometer data

NASA Astrophysics Data System (ADS)

Ren, Lin; Yang, Jingsong; Zheng, Gang; Wang, Juan

2016-07-01

This paper proposes a joint method to simultaneously retrieve wave spectra at different scales from spaceborne Synthetic Aperture Radar (SAR) and wave spectrometer data. The method combines the output from the two different sensors to overcome retrieval limitations that occur in some sea states. The wave spectrometer sensitivity coefficient is estimated using an effective significant wave height (SWH), which is an average of SAR-derived and wave spectrometer-derived SWH. This averaging extends the area of the sea surface sampled by the nadir beam of the wave spectrometer to improve the accuracy of the estimated sensitivity coefficient in inhomogeneous sea states. Wave spectra are then retrieved from SAR data using wave spectrometer-derived spectra as first guess spectra to complement the short waves lost in SAR data retrieval. In addition, the problem of 180° ambiguity in retrieved spectra is overcome using SAR imaginary cross spectra. Simulated data were used to validate the joint method. The simulations demonstrated that retrieved wave parameters, including SWH, peak wave length (PWL), and peak wave direction (PWD), agree well with reference parameters. Collocated data from ENVISAT advanced SAR (ASAR), the airborne wave spectrometer STORM, the PHAROS buoy, and the European Centre for Medium-Range Weather Forecasting (ECMWF) were then used to verify the proposed method. Wave parameters retrieved from STORM and two ASAR images were compared to buoy and ECMWF wave data. Most of the retrieved parameters were comparable to reference parameters. The results of this study show that the proposed joint retrieval method could be a valuable complement to traditional methods used to retrieve directional ocean wave spectra, particularly in inhomogeneous sea states.

Ocean Wave Separation Using CEEMD-Wavelet in GPS Wave Measurement.

PubMed

Wang, Junjie; He, Xiufeng; Ferreira, Vagner G

2015-08-07

Monitoring ocean waves plays a crucial role in, for example, coastal environmental and protection studies. Traditional methods for measuring ocean waves are based on ultrasonic sensors and accelerometers. However, the Global Positioning System (GPS) has been introduced recently and has the advantage of being smaller, less expensive, and not requiring calibration in comparison with the traditional methods. Therefore, for accurately measuring ocean waves using GPS, further research on the separation of the wave signals from the vertical GPS-mounted carrier displacements is still necessary. In order to contribute to this topic, we present a novel method that combines complementary ensemble empirical mode decomposition (CEEMD) with a wavelet threshold denoising model (i.e., CEEMD-Wavelet). This method seeks to extract wave signals with less residual noise and without losing useful information. Compared with the wave parameters derived from the moving average skill, high pass filter and wave gauge, the results show that the accuracy of the wave parameters for the proposed method was improved with errors of about 2 cm and 0.2 s for mean wave height and mean period, respectively, verifying the validity of the proposed method.

A New Sensitive Sensor for Simultaneous Differential Pulse Voltammetric Determination of Codeine and Acetaminophen Using a Hydroquinone Derivative and Multiwall Carbon Nanotubes Carbon Paste Electrode

PubMed Central

Garazhian, Elahe; Shishehbore, M. Reza

2015-01-01

A new sensitive sensor was fabricated for simultaneous determination of codeine and acetaminophen based on 4-hydroxy-2-(triphenylphosphonio)phenolate (HTP) and multiwall carbon nanotubes paste electrode at trace levels. The sensitivity of codeine determination was deeply affected by spiking multiwall carbon nanotubes and a modifier in carbon paste. Electron transfer coefficient, α, catalytic electron rate constant, k, and the exchange current density, j 0, for oxidation of codeine at the HTP-MWCNT-CPE were calculated using cyclic voltammetry. The calibration curve was linear over the range 0.2–844.7 μM with two linear segments, and the detection limit of 0.063 μM of codeine was obtained using differential pulse voltammetry. The modified electrode was separated codeine and acetaminophen signals by differential pulse voltammetry. The modified electrode was applied for the determination of codeine and acetaminophen in biological and pharmaceutical samples with satisfactory results. PMID:25945094

The effects of cations and anions on hydrogen chemisorption at Pt

NASA Technical Reports Server (NTRS)

Huang, J. C.; Ogrady, W. E.; Yeager, E.

1977-01-01

Experimental evidence based on linear sweep voltammetry is presented to substantiate the view that ionic adsorption substantially shifts electrode potentials in addition to the relative heights of the hydrogen adsorption peaks. HClO4 and HF are chosen as better reference electrolytes for anion studies. The voltammetry curves for 0.1M HF and 0.1M HClO4 as well as the effect of adding successively increasing amounts of H2SO4 to these electrolytes are discussed. The measurements are also extended to alkaline solutions. Mechanisms whereby the addition of various cations and anions to electrolytes such as HF and HClO4 can induce changes in the structure of the hydrogen adsorption region in the voltammetry curves are identified: (1) blocking of sites by anion adsorption and coupling of hydrogen adsorption and anion desorption, (2) modification in the hydrogen adsorption energies for sites adjacent to adsorbed anions, (3) changes in the potential distribution across the interface, and (4) surface restructuring.

Thin-layer voltammetry of soluble species on screen-printed electrodes: proof of concept.

PubMed

Botasini, S; Martí, A C; Méndez, E

2016-10-17

Thin-layer diffusion conditions were accomplished on screen-printed electrodes by placing a controlled-weight onto the cast solution and allowing for its natural spreading. The restricted diffusive conditions were assessed by cyclic voltammetry at low voltage scan rates and electrochemical impedance spectroscopy. The relationship between the weight exerted over the drop and the thin-layer thickness achieved was determined, in such a way that the simple experimental set-up designed for this work could be developed into a commercial device with variable control of the thin-layer conditions. The experimental results obtained resemble those reported for the voltammetric features of electroactive soluble species employing electrodes modified with carbon nanotubes or graphene layers, suggesting that the attainment of the benefits reported for these nanomaterials could be done simply by forcing the solution to spread over the screen-printed electrodic system to form a thin layer solution. The advantages of thin-layer voltammetry in the kinetic characterization of quasi-reversible and irreversible processes are highlighted.

Determination of the wine preservative sulphur dioxide with cyclic voltammetry using inkjet printed electrodes.

PubMed

Schneider, Marion; Türke, Alexander; Fischer, Wolf-Joachim; Kilmartin, Paul A

2014-09-15

During winemaking sulphur dioxide is added to prevent undesirable reactions. However, concerns over the harmful effects of sulphites have led to legal limits being placed upon such additives. There is thus a need for simple and selective determinations of sulphur dioxide in wine, especially during winemaking. The simultaneous detection of polyphenols and sulphur dioxide, using cyclic voltammetry at inert electrodes is challenging due to close oxidation potentials. In the present study, inkjet printed electrodes were developed with a suitable voltammetric signal on which the polyphenol oxidation is suppressed and the oxidation peak height for sulphur dioxide corresponds linearly to the concentration. Different types of working electrodes were printed. Electrodes consisting of gold nanoparticles mixed with silver showed the highest sensitivity towards sulphur dioxide. Low cost production of the sensor elements and ultra fast determination of sulphur dioxide by cyclic voltammetry makes this technique very promising for the wine industry. Copyright © 2014 Elsevier Ltd. All rights reserved.

Study on evaluation methods for Rayleigh wave dispersion characteristic

USGS Publications Warehouse

Shi, L.; Tao, X.; Kayen, R.; Shi, H.; Yan, S.

2005-01-01

The evaluation of Rayleigh wave dispersion characteristic is the key step for detecting S-wave velocity structure. By comparing the dispersion curves directly with the spectra analysis of surface waves (SASW) method, rather than comparing the S-wave velocity structure, the validity and precision of microtremor-array method (MAM) can be evaluated more objectively. The results from the China - US joint surface wave investigation in 26 sites in Tangshan, China, show that the MAM has the same precision with SASW method in 83% of the 26 sites. The MAM is valid for Rayleigh wave dispersion characteristic testing and has great application potentiality for site S-wave velocity structure detection.

A functional graphene oxide-ionic liquid composites-gold nanoparticle sensing platform for ultrasensitive electrochemical detection of Hg2+.

PubMed

Zhou, Na; Li, Jinhua; Chen, Hao; Liao, Chunyang; Chen, Lingxin

2013-02-21

A simple and sensitive electrochemical assay strategy of stripping voltammetry for mercury ions (Hg(2+)) detection is described based on the synergistic effect between ionic liquid functionalized graphene oxide (GO-IL) and gold nanoparticles (AuNPs). The AuNPs-GO-IL modified onto glassy carbon electrode (GCE) resulted in highly enhanced electron conductive nanostructured membrane and large electroactive surface area, which was excellently examined by scanning electron microscopy and cyclic voltammetry. After accumulating Hg(2+), anodic stripping voltammetry (ASV) was performed, and differential pulse voltammetry (DPV) was employed for signal recording of Hg(2+). Several main experimental parameters were optimized, i.e., deposition potential and time of AuNPs were -0.2 V and 180 s, respectively, and accumulation potential and time of Hg(2+) were -0.3 V and 660 s, respectively. Under the optimal conditions, this AuNPs-GO-IL-GCE sensor attained a good linearity in a wide range of 0.1-100 nM (R = 0.9808) between the concentration of the Hg(2+) standard and peak current. The limit of detection was estimated to be 0.03 nM at a signal-to-noise ratio of 3σ. A variety of common coexistent ions in water samples were investigated, showing no obvious interferences on the Hg(2+) detection. The practical application of the proposed sensor has been carried out and demonstrated as feasible for determination of trace levels of Hg(2+) in drinking and environmental water samples.

Large amplitude Fourier transformed ac voltammetry at a rotating disc electrode: a versatile technique for covering Levich and flow rate insensitive regimes in a single experiment.

PubMed

Bano, Kiran; Kennedy, Gareth F; Zhang, Jie; Bond, Alan M

2012-04-14

The theory for large amplitude Fourier transformed ac voltammetry at a rotating disc electrode is described. Resolution of time domain data into dc and ac harmonic components reveals that the mass transport for the dc component is controlled by convective-diffusion, while the background free higher order harmonic components are flow rate insensitive and mainly governed by linear diffusion. Thus, remarkable versatility is available; Levich behaviour of the dc component limiting current provides diffusion coefficient values and access to higher harmonics allows fast electrode kinetics to be probed. Two series of experiments (dc and ac voltammetry) have been required to extract these parameters; here large amplitude ac voltammetry with RDE methodology is used to demonstrate that kinetics and diffusion coefficient information can be extracted from a single experiment. To demonstrate the power of this approach, theoretical and experimental comparisons of data obtained for the reversible [Ru(NH(3))(6)](3+/2+) and quasi-reversible [Fe(CN)(6)](3-/4-) electron transfer processes are presented over a wide range of electrode rotation rates and with different concentrations and electrode materials. Excellent agreement of experimental and simulated data is achieved, which allows parameters such as electron transfer rate, diffusion coefficient, uncompensated resistance and others to be determined using a strategically applied approach that takes into account the different levels of sensitivity of each parameter to the dc or the ac harmonic.

One-Step Electrochemical Fabrication of Reduced Graphene Oxide/Gold Nanoparticles Nanocomposite-Modified Electrode for Simultaneous Detection of Dopamine, Ascorbic Acid, and Uric Acid

PubMed Central

Lee, Chang-Seuk; Yu, Su Hwan; Kim, Tae Hyun

2017-01-01

Here, we introduce the preparation of the hybrid nanocomposite-modified electrode consisting of reduced graphene oxide (RGO) and gold nanoparticles (AuNPs) using the one-step electrochemical method, allowing for the simultaneous and individual detection of dopamine (DA), ascorbic acid (AA), and uric acid (UA). RGO/AuNPs nanocomposite was formed on a glassy carbon electrode by the co-reduction of GO and Au3+ using the potentiodynamic method. The RGO/AuNPs nanocomposite-modified electrode was produced by subjecting a mixed solution of GO and Au3+ to cyclic sweeping from −1.5 V to 0.8 V (vs. Ag/AgCl) at a scan rate 10 mV/s for 3 cycles. The modified electrode was characterized by scanning electron microscopy, Raman spectroscopy, contact angle measurement, electrochemical impedance spectroscopy, and cyclic voltammetry. Voltammetry results confirm that the RGO/AuNPs nanocomposite-modified electrode has high catalytic activity and good resolution for the detection of DA, AA, and UA. The RGO/AuNPs nanocomposite-modified electrode exhibits stable amperometric responses for DA, AA, and UA, respectively, and its detection limits were estimated to be 0.14, 9.5, and 25 μM. The modified electrode shows high selectivity towards the determination of DA, AA, or UA in the presence of potentially active bioelements. In addition, the resulting sensor exhibits many advantages such as fast amperometric response, excellent operational stability, and appropriate practicality. PMID:29301209

Synthesis of Nano-Ilmenite (FeTiO3) doped TiO2/Ti Electrode for Photoelectrocatalytic System

NASA Astrophysics Data System (ADS)

Hikmawati; Watoni, A. H.; Wibowo, D.; Maulidiyah; Nurdin, M.

2017-11-01

Ilmenite (FeTiO3) doped on Ti and TiO2/Ti electrodes were successfully prepared by using the sol-gel method. The structure, morphology, and optical properties of FeTiO3 are characterized by XRD, UV-Vis DRS, and SEM. The FeTiO3 and TiO2 greatly affect the photoelectrocatalysis performance characterized by Linear Sweep Voltammetry (LSV) and Cyclic Voltammetry (CV). The characterization result shows a band gap of FeTiO3 is 2.94 eV. XRD data showed that FeTiO3 formed at 2θ were 35.1° (110), 49.9° (024), and 61.2° (214). The morphology of FeTiO3/Ti and FeTiO3.TiO2/Ti using SEM shows that the formation of FeTiO3 thin layer signifies the Liquid Phase Deposition method effectively in the coating process. Photoelectrochemical (PEC) test showed that FeTiO3.TiO2/Ti electrode was highly oxidation responsive under visible light compared to the FeTiO3/Ti electrodes i.e. 7.87×10-4 A and 9.87×10-5 A. Degradation test of FeTiO3/Ti and FeTiO3.TiO2/Ti electrodes on titan yellow showed that the percentages of degradation with photoelectrocatalysis at 0.5 mg/L were 41% and 43%, respectively.

Copper(II) binding by dissolved organic matter: Importance of the copper-to-dissolved organic matter ratio and implications for the Biotic Ligand Model

USGS Publications Warehouse

Craven, Alison M.; Aiken, George R.; Ryan, Joseph N.

2012-01-01

The ratio of copper to dissolved organic matter (DOM) is known to affect the strength of copper binding by DOM, but previous methods to determine the Cu2+–DOM binding strength have generally not measured binding constants over the same Cu:DOM ratios. In this study, we used a competitive ligand exchange–solid-phase extraction (CLE-SPE) method to determine conditional stability constants for Cu2+–DOM binding at pH 6.6 and 0.01 M ionic strength over a range of Cu:DOM ratios that bridge the detection windows of copper-ion-selective electrode and voltammetry measurements. As the Cu:DOM ratio increased from 0.0005 to 0.1 mg of Cu/mg of DOM, the measured conditional binding constant (cKCuDOM) decreased from 1011.5 to 105.6 M–1. A comparison of the binding constants measured by CLE-SPE with those measured by copper-ion-selective electrode and voltammetry demonstrates that the Cu:DOM ratio is an important factor controlling Cu2+–DOM binding strength even for DOM isolates of different types and different sources and for whole water samples. The results were modeled with Visual MINTEQ and compared to results from the biotic ligand model (BLM). The BLM was found to over-estimate Cu2+ at low total copper concentrations and under-estimate Cu2+ at high total copper concentrations.

Facile fabrication of novel silver-polypyrrole-multiwall carbon nanotubes nanocomposite for replacement of platinum in dye-sensitized solar cell

DOE Office of Scientific and Technical Information (OSTI.GOV)

Rafique, Shaista; Sharif, Rehana; Ghani, Sheeba

This paper demonstrates the facile synthesis of high performance silver-polypyrrole-multiwall carbon nanotubes (Ag-PPy-FMWCNTS) nanocomposites via electrodeposition method on stainless steel substrate and its application as a low cost counter electrode (CE) for the precious platinum (Pt) free DSSC. The nanocomposites were characterized by variety of techniques such as Fourier transforms infrared (FTIR), X-ray diffraction, Scanning electron microscope (SEM), cyclic voltammetry (CV) and Four probe technique respectively. The cyclic voltammetry and Tafel polymerization measurements of Ag-PPy-FMWCNTS nanocomposites CE reveal the favorable electrocatalytic activity and low charge transfer resistance R{sub ct}(2.50 Ω cm{sup 2}) for I{sub 3}{sup −}/I{sup −} redox solution. Themore » four probe studies showed the large electrical conductivity (226S cm{sup −1}) of Ag-PPy-FMWCNTS nanocomposite. The DSSC assembled with Ag-PPy-FMWCNTS nanocomposites CE display the considerable short circuit current density (13.95 mA cm{sup −2}) and acceptable solar to electrical conversion efficiency of 7.6%, which is higher to the efficiency of DSSC with thermally decomposed Pt reference electrode 7.1%. The excellent conversion efficiency, rapid charge transfer in combination with low cost and simple fabrication method of Ag-PPy-FMWCNTS nanocomposites can be exploited as an efficient and potential candidate to replace the Pt CE for large scale production of DSSC.« less

Removal of Differential Capacitive Interferences in Fast-Scan Cyclic Voltammetry.

PubMed

Johnson, Justin A; Hobbs, Caddy N; Wightman, R Mark

2017-06-06

Due to its high spatiotemporal resolution, fast-scan cyclic voltammetry (FSCV) at carbon-fiber microelectrodes enables the localized in vivo monitoring of subsecond fluctuations in electroactive neurotransmitter concentrations. In practice, resolution of the analytical signal relies on digital background subtraction for removal of the large current due to charging of the electrical double layer as well as surface faradaic reactions. However, fluctuations in this background current often occur with changes in the electrode state or ionic environment, leading to nonspecific contributions to the FSCV data that confound data analysis. Here, we both explore the origin of such shifts seen with local changes in cations and develop a model to account for their shape. Further, we describe a convolution-based method for removal of the differential capacitive contributions to the FSCV current. The method relies on the use of a small-amplitude pulse made prior to the FSCV sweep that probes the impedance of the system. To predict the nonfaradaic current response to the voltammetric sweep, the step current response is differentiated to provide an estimate of the system's impulse response function and is used to convolute the applied waveform. The generated prediction is then subtracted from the observed current to the voltammetric sweep, removing artifacts associated with electrode impedance changes. The technique is demonstrated to remove select contributions from capacitive characteristics changes of the electrode both in vitro (i.e., in flow-injection analysis) and in vivo (i.e., during a spreading depression event in an anesthetized rat).

Quantitation of bacteria through adsorption of intracellular biomolecules on carbon paste and screen-printed carbon electrodes and voltammetry of redox-active probes.

PubMed

Obuchowska, Agnes

2008-03-01

A new electrochemical method for the quantitation of bacteria that is rapid, inexpensive, and amenable to miniaturization is reported. Cyclic voltammetry was used to quantitate M. luteus, C. sporogenes, and E. coli JM105 in exponential and stationary phases, following exposure of screen-printed carbon working electrodes (SPCEs) to lysed culture samples. Ferricyanide was used as a probe. The detection limits (3s) were calculated and the dynamic ranges for E. coli (exponential and stationary phases), M. luteus (exponential and stationary phases), and C. sporogenes (exponential phase) lysed by lysozyme were 3 x 10(4) to 5 x 10(6) colony-forming units (CFU) mL(-1), 5 x 10(6) to 2 x 10(8) CFU mL(-1) and 3 x 10(3) to 3 x 10(5) CFU mL(-1), respectively. Good overlap was obtained between the calibration curves when the electrochemical signal was plotted against the dry bacterial weight, or between the protein concentration in the bacterial lysate. In contrast, unlysed bacteria did not change the electrochemical signal of ferricyanide. The results indicate that the reduction of the electrochemical signal in the presence of the lysate is mainly due to the fouling of the electrode by proteins. Similar results were obtained with carbon-paste electrodes although detection limits were better with SPCEs. The method described herein was applied to quantitation of bacteria in a cooling tower water sample.

Comparison of recent S-wave indicating methods

NASA Astrophysics Data System (ADS)

Hubicka, Katarzyna; Sokolowski, Jakub

2018-01-01

Seismic event consists of surface waves and body waves. Due to the fact that the body waves are faster (P-waves) and more energetic (S-waves) in literature the problem of their analysis is taken more often. The most universal information that is received from the recorded wave is its moment of arrival. When this information is obtained from at least four seismometers in different locations, the epicentre of the particular event can be estimated [1]. Since the recorded body waves may overlap in signal, the problem of wave onset moment is considered more often for faster P-wave than S-wave. This however does not mean that the issue of S-wave arrival time is not taken at all. As the process of manual picking is time-consuming, methods of automatic detection are recommended (these however may be less accurate). In this paper four recently developed methods estimating S-wave arrival are compared: the method operating on empirical mode decomposition and Teager-Kaiser operator [2], the modification of STA/LTA algorithm [3], the method using a nearest neighbour-based approach [4] and the algorithm operating on characteristic of signals' second moments. The methods will be also compared to wellknown algorithm based on the autoregressive model [5]. The algorithms will be tested in terms of their S-wave arrival identification accuracy on real data originating from International Research Institutions for Seismology (IRIS) database.

A Revised Method of Presenting Wavenumber-Frequency Power Spectrum Diagrams That Reveals the Asymmetric Nature of Tropical Large-scale Waves

NASA Technical Reports Server (NTRS)

Chao, Winston C.; Yang, Bo; Fu, Xiouhua

2007-01-01

The popular method of presenting wavenumber-frequency power spectrum diagrams for studying tropical large-scale waves in the literature is shown to give an incomplete presentation of these waves. The so-called "convectively-coupled Kelvin (mixed Rossby-gravity) waves" are presented as existing only in the symmetric (antisymmetric) component of the diagrams. This is obviously not consistent with the published composite/regression studies of "convectively-coupled Kelvin waves," which illustrate the asymmetric nature of these waves. The cause of this inconsistency is revealed in this note and a revised method of presenting the power spectrum diagrams is proposed. When this revised method is used, "convectively-coupled Kelvin waves" do show anti-symmetric components, and "convectively-coupled mixed Rossby-gravity waves (also known as Yanai waves)" do show a hint of symmetric components. These results bolster a published proposal that these waves be called "chimeric Kelvin waves," "chimeric mixed Rossby-gravity waves," etc. This revised method of presenting power spectrum diagrams offers a more rigorous means of comparing the General Circulation Models (GCM) output with observations by calling attention to the capability of GCMs in correctly simulating the asymmetric characteristics of the equatorial waves.

Time-domain separation of interfering waves in cancellous bone using bandlimited deconvolution: simulation and phantom study.

PubMed

Wear, Keith A

2014-04-01

In through-transmission interrogation of cancellous bone, two longitudinal pulses ("fast" and "slow" waves) may be generated. Fast and slow wave properties convey information about material and micro-architectural characteristics of bone. However, these properties can be difficult to assess when fast and slow wave pulses overlap in time and frequency domains. In this paper, two methods are applied to decompose signals into fast and slow waves: bandlimited deconvolution and modified least-squares Prony's method with curve-fitting (MLSP + CF). The methods were tested in plastic and Zerdine(®) samples that provided fast and slow wave velocities commensurate with velocities for cancellous bone. Phase velocity estimates were accurate to within 6 m/s (0.4%) (slow wave with both methods and fast wave with MLSP + CF) and 26 m/s (1.2%) (fast wave with bandlimited deconvolution). Midband signal loss estimates were accurate to within 0.2 dB (1.7%) (fast wave with both methods), and 1.0 dB (3.7%) (slow wave with both methods). Similar accuracies were found for simulations based on fast and slow wave parameter values published for cancellous bone. These methods provide sufficient accuracy and precision for many applications in cancellous bone such that experimental error is likely to be a greater limiting factor than estimation error.

Ocean Wave Separation Using CEEMD-Wavelet in GPS Wave Measurement

PubMed Central

Wang, Junjie; He, Xiufeng; Ferreira, Vagner G.

2015-01-01

Monitoring ocean waves plays a crucial role in, for example, coastal environmental and protection studies. Traditional methods for measuring ocean waves are based on ultrasonic sensors and accelerometers. However, the Global Positioning System (GPS) has been introduced recently and has the advantage of being smaller, less expensive, and not requiring calibration in comparison with the traditional methods. Therefore, for accurately measuring ocean waves using GPS, further research on the separation of the wave signals from the vertical GPS-mounted carrier displacements is still necessary. In order to contribute to this topic, we present a novel method that combines complementary ensemble empirical mode decomposition (CEEMD) with a wavelet threshold denoising model (i.e., CEEMD-Wavelet). This method seeks to extract wave signals with less residual noise and without losing useful information. Compared with the wave parameters derived from the moving average skill, high pass filter and wave gauge, the results show that the accuracy of the wave parameters for the proposed method was improved with errors of about 2 cm and 0.2 s for mean wave height and mean period, respectively, verifying the validity of the proposed method. PMID:26262620

The local properties of ocean surface waves by the phase-time method

NASA Technical Reports Server (NTRS)

Huang, Norden E.; Long, Steven R.; Tung, Chi-Chao; Donelan, Mark A.; Yuan, Yeli; Lai, Ronald J.

1992-01-01

A new approach using phase information to view and study the properties of frequency modulation, wave group structures, and wave breaking is presented. The method is applied to ocean wave time series data and a new type of wave group (containing the large 'rogue' waves) is identified. The method also has the capability of broad applications in the analysis of time series data in general.

Electrochemistry in supercritical fluids

PubMed Central

Branch, Jack A.; Bartlett, Philip N.

2015-01-01

A wide range of supercritical fluids (SCFs) have been studied as solvents for electrochemistry with carbon dioxide and hydrofluorocarbons (HFCs) being the most extensively studied. Recent advances have shown that it is possible to get well-resolved voltammetry in SCFs by suitable choice of the conditions and the electrolyte. In this review, we discuss the voltammetry obtained in these systems, studies of the double-layer capacitance, work on the electrodeposition of metals into high aspect ratio nanopores and the use of metallocenes as redox probes and standards in both supercritical carbon dioxide–acetonitrile and supercritical HFCs. PMID:26574527

A one-dimensional stochastic approach to the study of cyclic voltammetry with adsorption effects

DOE Office of Scientific and Technical Information (OSTI.GOV)

Samin, Adib J.

In this study, a one-dimensional stochastic model based on the random walk approach is used to simulate cyclic voltammetry. The model takes into account mass transport, kinetics of the redox reactions, adsorption effects and changes in the morphology of the electrode. The model is shown to display the expected behavior. Furthermore, the model shows consistent qualitative agreement with a finite difference solution. This approach allows for an understanding of phenomena on a microscopic level and may be useful for analyzing qualitative features observed in experimentally recorded signals.

The Influence of Uncompensated Solution Resistance on the Determination and Standard Electrochemical Rate Constants Using Cyclic Voltammetry, and Some Comparisons with AC Voltammetry.

DTIC Science & Technology

1987-09-25

rate constants, k2r using cyclic voltametry . The res tss are expressed in terms of systematic deviations oP sapparent measured" rate constants, k~b(app...concentration was taken to be lum unless otherwise noted. The voltammetric sweep rate was set at 20 V sŕ unless specified otherwise. The general procedure...peaks for the negative- and positive-going potential sweeps have opposite signs, the measured cathodic-anodic peak separation, AEp, will clearly be

Redox protein noncovalent functionalization of double-wall carbon nanotubes: electrochemical binder-less glucose biosensor.

PubMed

Pumera, Martin; Smíd, Bretislav

2007-10-01

Double wall carbon nanotubes are noncovalently functionalized with redox protein and such assembly is used for construction of electrochemical binder-less glucose biosensor. Redox protein glucose oxidase performs as biorecognition element and double wall carbon nanotubes act both as immobilization platform for redox enzyme and as signal transducer. The double carbon nanotubes are characterized by cyclic voltammetry and specific surface area measurements; the redox protein noncovalently functionalized double wall carbon nanotubes are characterized in detail by X-ray photoelectron spectroscopy, cyclic voltammetry, amperometry, and transmission electron microscopy.

Studies on niobium triselenide cathode material for lithium rechargeable cells

NASA Technical Reports Server (NTRS)

Ratnakumar, B. V.; Ni, C. L.; Distefano, S.; Somoano, R. B.; Bankston, C. P.

1988-01-01

NbSe3 exhibits superior characteristics such as high capacity, high volumetric and gravimetric energy densities, and high discharge rate capability, as compared to other intercalating cathodes. This paper reports the preparation, characterization, and performance of NbSe3. Several electrochemical techniques, such as cyclic voltammetry, constant-current/constant-potential discharges, dc potentiodynamic scans, ac impedance, and ac voltammetry, have been used to give insight to the mechanisms of intercalation of three lithiums with NbSe3 and also into the rate determining process in the reduction of NbSe3.

The Influence of Acidity on Microbial Fuel Cells Containing Shewanella Oneidensis (PREPRINT)

DTIC Science & Technology

2008-09-01

d a fi b i s a h t s p t o m d C H p F 8 ig. 4. Cyclic voltammetry of filter sterilized media after 4 days of growth of S. neidensis MR-1 or S...of autologous mediators in the rowthmedium changeswith pH.We analyzed filter sterilized cul- ure supernatants by cyclic voltammetry (Fig. 4), and HPLC...Marsili et al., 2008). Cyclic voltammetrywas used to detect redox-active compounds n growthmedia supernatants fromMR-1 andDSP10 cultures. Fig. 4 hows

A one-dimensional stochastic approach to the study of cyclic voltammetry with adsorption effects

NASA Astrophysics Data System (ADS)

Samin, Adib J.

2016-05-01

In this study, a one-dimensional stochastic model based on the random walk approach is used to simulate cyclic voltammetry. The model takes into account mass transport, kinetics of the redox reactions, adsorption effects and changes in the morphology of the electrode. The model is shown to display the expected behavior. Furthermore, the model shows consistent qualitative agreement with a finite difference solution. This approach allows for an understanding of phenomena on a microscopic level and may be useful for analyzing qualitative features observed in experimentally recorded signals.