Polyurethane Ionophore-Based Thin Layer Membranes for Voltammetric Ion Activity Sensing.

Science.gov (United States)

Cuartero, Maria; Crespo, Gaston A; Bakker, Eric

2016-06-07

We report on a plasticized polyurethane ionophore-based thin film material (of hundreds of nanometer thickness) for simultaneous voltammetric multianalyte ion activity detection triggered by the oxidation/reduction of an underlying poly(3-octylthiophene) film. This material provides excellent mechanical, physical, and chemical robustness compared to other polymers. Polyurethane films did not exhibit leaching of lipophilic additives after rinsing with a direct water jet and exhibited resistance to detachment from the underlying electrode surface, resulting in a voltammetric current response with less than acrylate) ionophore-based membranes of the same thickness and composition exhibited a significant deterioration of the signal after identical treatment. While previously reported works emphasized fundamental advancement of multi-ion detection with multi-ionophore-based thin films, polyurethane thin membranes allow one to achieve real world measurements without sacrificing analytical performance. Indeed, polyurethane membranes are demonstrated to be useful for the simultaneous determination of potassium and lithium in undiluted human serum and blood with attractive precision.

Rapid voltammetric monitoring of melatonin in the presence of tablet excipients

International Nuclear Information System (INIS)

Ball, Andrew T.; Patel, Bhavik Anil

2012-01-01

Melatonin is an important neurohormonal chemical that is responsible for regulating sleep. Melatonin dietary supplements are available and utilised to counteract the effects of jet-lag or to aid sleep. Voltammetric detection with a boron-doped diamond electrode was utilised for the rapid monitoring of individual melatonin tablets. Melatonin was oxidised at a potential of +0.8 V vs. Ag|AgCl. Voltammetric measurements were carried out without the need of excessive sample preparation steps such as filtration. However dicalcium phosphate and carboxymethyl cellulose were shown to alter the electrochemical response. Calibration responses were linear over a concentration of 2–4 mg/25 ml of melatonin and a limit of detection of 0.06 mg/25 ml was observed. Volammetric recordings were only stable for one measurement, but the electrode surface could be replenished following a single wipe of an ethanol soaked lens cloth. This new assay was capable of analysing individual melatonin tablets within a total analysis time of 2.5 min. Overall this approach provides the basis for rapid electrochemical monitoring of pharmaceutical and dietary tablets without the need for extensive sample preparation.

Voltammetric quantitation of nitazoxanide by glassy carbon electrode

Directory of Open Access Journals (Sweden)

Rajeev Jain

2013-12-01

Full Text Available The present study reports voltammetric reduction of nitazoxanide in Britton–Robinson (B–R buffer by cyclic and square-wave voltammetry at glassy carbon electrode. A versatile fully validated voltammetric method for quantitative determination of nitazoxanide in pharmaceutical formulation has been proposed. A squrewave peak current was linear over the nitazoxanide concentration in the range of 20–140 µg/mL. The limit of detection (LOD and limit of quantification (LOQ was calculated to be 5.23 μg/mL and 17.45 μg/mL, respectively. Keywords: Nitazoxanide, Squarewave voltammetry, Glassy carbon electrode, Pharmaceutical formulation

New molecular imprinted voltammetric sensor for determination of ochratoxin A.

Science.gov (United States)

Yola, Mehmet Lütfi; Gupta, Vinod Kumar; Atar, Necip

2016-04-01

In this report, a novel molecular imprinted voltammetric sensor based on silver nanoparticles (AgNPs) involved in a polyoxometalate (H3PW12O40, POM) functionalized reduced graphene oxide (rGO) modified glassy carbon electrode (GCE) was presented for determination of ochrattoxin A (OCH). The developed surfaces were characterized using scanning electron microscope (SEM), transmission electron microscope (TEM), X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD) method. OCH imprinted GCE was prepared via electropolymerization process of 100mM phenol as monomer in the presence of phosphate buffer solution (pH6.0) containing 25 mM OCH. The linearity range and the detection limit of the method were calculated as 5.0 × 10(-11) - 1.5 × 10(-9)M and 1.6 × 10(-11) M, respectively. The voltammetric sensor was applied to grape juice and wine samples with good selectivity and recovery. The stability of the voltammetric sensor was also reported. Copyright © 2015 Elsevier B.V. All rights reserved.

Recognizing Single Collisions of PtCl6(2-) at Femtomolar Concentrations on Ultramicroelectrodes by Nucleating Electrocatalytic Clusters.

Science.gov (United States)

Dick, Jeffrey E; Bard, Allen J

2015-11-04

We report the electrodeposition of electrocatalytic clusters of platinum from femtomolar platinate solutions. An inert carbon fiber ultramicroelectrode (UME) was held at a potential where proton reduction was unfavorable on carbon but favorable on platinum in a 1 M sulfuric acid solution. Upon addition of femtomolar amounts of hexachloroplatinic acid, which will also reduce to Pt(0) at the applied potential on the carbon fiber UME, cathodic blips were observed in the amperometric i-t response. These blips correspond to the reduction of protons to molecular hydrogen at the small platinum clusters followed by a rapid deactivation likely due to hydrogen bubble formation. On average, these current spikes occur when five platinum atoms have been formed on the electrode, as determined by a comparative analysis of experimental cathodic blips and calculated hexachloroplatinate molecule collision frequencies.

Electrochemistry of moexipril: experimental and computational approach and voltammetric determination.

Science.gov (United States)

Taşdemir, Hüdai I; Kiliç, E

2014-09-01

The electrochemistry of moexipril (MOE) was studied by electrochemical methods with theoretical calculations performed at B3LYP/6-31 + G (d)//AM1. Cyclic voltammetric studies were carried out based on a reversible and adsorption-controlled reduction peak at -1.35 V on a hanging mercury drop electrode (HMDE). Concurrently irreversible diffusion-controlled oxidation peak at 1.15 V on glassy carbon electrode (GCE) was also employed. Potential values are according to Ag/AgCI, (3.0 M KCI) and measurements were performed in Britton-Robinson buffer of pH 5.5. Tentative electrode mechanisms were proposed according to experimental results and ab-initio calculations. Square-wave adsorptive stripping voltammetric methods have been developed and validated for quantification of MOE in pharmaceutical preparations. Linear working range was established as 0.03-1.35 microM for HMDE and 0.2-20.0 microM for GCE. Limit of quantification (LOQ) was calculated to be 0.032 and 0.47 microM for HMDE and GCE, respectively. Methods were successfully applied to assay the drug in tablets by calibration and standard addition methods with good recoveries between 97.1% and 106.2% having relative standard deviation less than 10%.

Voltammetric determination of nicotine in cigarette tobacco at ...

African Journals Online (AJOL)

The electrochemical behavior of nicotine was investigated using cyclic and square wave voltammetric techniques. Electrochemical activation of glassy carbon electrode significantly increased the oxidation peak current of nicotine compared to the bare glassy carbon. At the activated glassy carbon electrode, the square ...

Application of ascorbic acid 2-phosphate as a new voltammetric substrate for alkaline phosphatase determination in human serum

Directory of Open Access Journals (Sweden)

Wei Sun

2005-12-01

Full Text Available An electrochemical assay of the enzyme alkaline phosphatase (ALP using ascorbic acid 2-phosphate (AAP as a new voltammetric substrate has been described in this paper. In the alkaline buffer solution the ALP enzymatic hydrolysis product of AAP was ascorbic acid (AA, which was an electro-active substance and had a sensitive differential pulse voltammetric (DPV oxidative response on glassy carbon electrode (GCE at +380 mV (versus Ag/AgCl, so the activity of ALP could be monitored voltammetrically of the oxidative peak current of AA. The electrochemical behaviours of AA were carefully studied and the AA standard solution could be measured by DPV method in the linear range from 10.0 to 1000.0 μmol/L with the detection limit of 8.0 μmol/L. The optimal conditions for ALP enzymatic reaction and the voltammetric detection were optimized. Under the optimal conditions the calibration curve for ALP assay exhibited a linear range from 0.4 to 2000.0 U/L with a detection limit of 0.3 U/L. This proposed method was further applied to determine the ALP content in healthy human serum and the results were in good agreement with the traditional p-nitrophenyl phosphate spectrophotometric method. The kinetic constants of enzymatic reaction were also investigated with the apparent kinetic constant Km as 2.77 mmol/L and the maximum velocity Vmax as 0.33 mol/min.

Infrared spectroscopic and voltammetric study of adsorbed CO on stepped surfaces of copper monocrystalline electrodes

International Nuclear Information System (INIS)

Koga, O.; Teruya, S.; Matsuda, K.; Minami, M.; Hoshi, N.; Hori, Y.

2005-01-01

Voltammetric and infrared (IR) spectroscopic measurements were carried out to study adsorbed CO on two series of copper single crystal electrodes n(111)-(111) and n(111)-(100) in 0.1M KH 2 PO 4 +0.1M K 2 HPO 4 at 0 o C. Reversible voltammetric waves were observed below -0.55V versus SHE for adsorption of CO which displaces preadsorbed phosphate anions. The electric charge of the redox waves is proportional to the step atom density for both single crystal series. This fact indicates that phosphate anions are specifically adsorbed on the step sites below -0.55V versus SHE. Voltammetric measurements indicated that (111) terrace of Cu is covered with adsorbed CO below -0.5V versus SHE. Nevertheless, no IR absorption band of adsorbed CO is detected from (111) terrace. Presence of adsorbed CO on (111) terrace is presumed which is not visible by the potential difference spectroscopy used in the present work. IR spectroscopic measurements showed that CO is reversibly adsorbed with an on-top manner on copper single crystal electrodes of n(111)-(111) and n(111)-(100) with approximately same wavenumber of C?O stretching vibration of 2070cm -1 . The IR band intensity is proportional to the step atom density. Thus CO is adsorbed on (111) or (100) steps on the single crystal surfaces. An analysis of the IR band intensity suggested that one CO molecule is adsorbed on every two or more Cu step atom of the monocrystalline surface. The spectroscopic data were compared with those reported for uhv system. The C-O stretching wavenumber of adsorbed CO in the electrode-electrolyte system is 30-40cm -1 lower than those in uhv system

Active voltammetric microsensors with neural signal processing.

Energy Technology Data Exchange (ETDEWEB)

Vogt, M. C.

1998-12-11

Many industrial and environmental processes, including bioremediation, would benefit from the feedback and control information provided by a local multi-analyte chemical sensor. For most processes, such a sensor would need to be rugged enough to be placed in situ for long-term remote monitoring, and inexpensive enough to be fielded in useful numbers. The multi-analyte capability is difficult to obtain from common passive sensors, but can be provided by an active device that produces a spectrum-type response. Such new active gas microsensor technology has been developed at Argonne National Laboratory. The technology couples an electrocatalytic ceramic-metallic (cermet) microsensor with a voltammetric measurement technique and advanced neural signal processing. It has been demonstrated to be flexible, rugged, and very economical to produce and deploy. Both narrow interest detectors and wide spectrum instruments have been developed around this technology. Much of this technology's strength lies in the active measurement technique employed. The technique involves applying voltammetry to a miniature electrocatalytic cell to produce unique chemical ''signatures'' from the analytes. These signatures are processed with neural pattern recognition algorithms to identify and quantify the components in the analyte. The neural signal processing allows for innovative sampling and analysis strategies to be employed with the microsensor. In most situations, the whole response signature from the voltammogram can be used to identify, classify, and quantify an analyte, without dissecting it into component parts. This allows an instrument to be calibrated once for a specific gas or mixture of gases by simple exposure to a multi-component standard rather than by a series of individual gases. The sampled unknown analytes can vary in composition or in concentration, the calibration, sensing, and processing methods of these active voltammetric microsensors can

Active voltammetric microsensors with neural signal processing

Science.gov (United States)

Vogt, Michael C.; Skubal, Laura R.

1999-02-01

Many industrial and environmental processes, including bioremediation, would benefit from the feedback and control information provided by a local multi-analyte chemical sensor. For most processes, such a sensor would need to be rugged enough to be placed in situ for long-term remote monitoring, and inexpensive enough to be fielded in useful numbers. The multi-analyte capability is difficult to obtain from common passive sensors, but can be provided by an active device that produces a spectrum-type response. Such new active gas microsensor technology has been developed at Argonne National Laboratory. The technology couples an electrocatalytic ceramic-metallic (cermet) microsensor with a voltammetric measurement technique and advanced neural signal processing. It has been demonstrated to be flexible, rugged, and very economical to produce and deploy. Both narrow interest detectors and wide spectrum instruments have been developed around this technology. Much of this technology's strength lies in the active measurement technique employed. The technique involves applying voltammetry to a miniature electrocatalytic cell to produce unique chemical 'signatures' from the analytes. These signatures are processed with neural pattern recognition algorithms to identify and quantify the components in the analyte. The neural signal processing allows for innovative sampling and analysis strategies to be employed with the microsensor. In most situations, the whole response signature from the voltammogram can be used to identify, classify, and quantify an analyte, without dissecting it into component parts. This allows an instrument to be calibrated once for a specific gas or mixture of gases by simple exposure to a multi-component standard rather than by a series of individual gases. The sampled unknown analytes can vary in composition or in concentration; the calibration, sensing, and processing methods of these active voltammetric microsensors can detect, recognize, and

Discrimination of Rice with Different Pretreatment Methods by Using a Voltammetric Electronic Tongue

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Li Wang

2015-07-01

Full Text Available In this study, an application of a voltammetric electronic tongue for discrimination and prediction of different varieties of rice was investigated. Different pretreatment methods were selected, which were subsequently used for the discrimination of different varieties of rice and prediction of unknown rice samples. To this aim, a voltammetric array of sensors based on metallic electrodes was used as the sensing part. The different samples were analyzed by cyclic voltammetry with two sample-pretreatment methods. Discriminant Factorial Analysis was used to visualize the different categories of rice samples; however, radial basis function (RBF artificial neural network with leave-one-out cross-validation method was employed for prediction modeling. The collected signal data were first compressed employing fast Fourier transform (FFT and then significant features were extracted from the voltammetric signals. The experimental results indicated that the sample solutions obtained by the non-crushed pretreatment method could efficiently meet the effect of discrimination and recognition. The satisfactory prediction results of voltammetric electronic tongue based on RBF artificial neural network were obtained with less than five-fold dilution of the sample solution. The main objective of this study was to develop primary research on the application of an electronic tongue system for the discrimination and prediction of solid foods and provide an objective assessment tool for the food industry.

The voltammetric responses of nanometer-sized electrodes in weakly supported electrolyte: A theoretical study

International Nuclear Information System (INIS)

Liu Yuwen; Zhang Qianfan; Chen Shengli

2010-01-01

The effect of the supporting electrolyte concentration on the interfacial profiles and voltammetric responses of nanometer-sized disk electrodes have been investigated theoretically by combining the Poisson-Nernst-Planck (PNP) theory and Butler-Volmer (BV) equation. The PNP-theory is used to treat the nonlinear couplings of electric field, concentration field and dielectric field at electrochemical interface without the electroneutrality assumption that has been long adopted in various voltammetric theories for macro/microelectrodes. The BV equation is modified by using the Frumkin correction to account for the effect of the diffuse double layer potential on interfacial electron-transfer (ET) rate and by including a distance-dependent ET probability in the expression of rate constant to describe the radial heterogeneity of the ET rate constant at nanometer-sized disk electrodes. The computed voltammetric responses for disk electrodes larger than 200 nm in radii in the absence of the excess of the supporting electrolyte using the present theoretical scheme show reasonable agreements with the predications of the conventional microelectrode voltammetric theory which uses the combined Nernst-Planck equation and electroneutrality equation to describe the mixed electromigration-diffusion mass transport without including the possible effects of the diffuse double layer (Amatore et al. ). For electrodes smaller than 200 nm, however, the voltammetric responses predicated by the present theory exhibit significant deviation from the microelectrode theory. It is shown that the deviations are mainly resulted from the overlap between the diffuse double layer and the concentration depletion layer (CDL) at nanoscale electrochemical interfaces in weakly supported media, which will result in the invalidation of the electroneutrality condition in CDL, and from the radial inhomogeneity of ET probability at nanometer-sized disk electrodes.

The voltammetric responses of nanometer-sized electrodes in weakly supported electrolyte: A theoretical study

Energy Technology Data Exchange (ETDEWEB)

Liu Yuwen; Zhang Qianfan [Hubei Electrochemical Power Sources Key Laboratory, Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), Department of Chemistry, Wuhan University, Wuhan 430072 (China); Chen Shengli, E-mail: slchen@whu.edu.c [Hubei Electrochemical Power Sources Key Laboratory, Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), Department of Chemistry, Wuhan University, Wuhan 430072 (China)

2010-11-30

The effect of the supporting electrolyte concentration on the interfacial profiles and voltammetric responses of nanometer-sized disk electrodes have been investigated theoretically by combining the Poisson-Nernst-Planck (PNP) theory and Butler-Volmer (BV) equation. The PNP-theory is used to treat the nonlinear couplings of electric field, concentration field and dielectric field at electrochemical interface without the electroneutrality assumption that has been long adopted in various voltammetric theories for macro/microelectrodes. The BV equation is modified by using the Frumkin correction to account for the effect of the diffuse double layer potential on interfacial electron-transfer (ET) rate and by including a distance-dependent ET probability in the expression of rate constant to describe the radial heterogeneity of the ET rate constant at nanometer-sized disk electrodes. The computed voltammetric responses for disk electrodes larger than 200 nm in radii in the absence of the excess of the supporting electrolyte using the present theoretical scheme show reasonable agreements with the predications of the conventional microelectrode voltammetric theory which uses the combined Nernst-Planck equation and electroneutrality equation to describe the mixed electromigration-diffusion mass transport without including the possible effects of the diffuse double layer (Amatore et al. ). For electrodes smaller than 200 nm, however, the voltammetric responses predicated by the present theory exhibit significant deviation from the microelectrode theory. It is shown that the deviations are mainly resulted from the overlap between the diffuse double layer and the concentration depletion layer (CDL) at nanoscale electrochemical interfaces in weakly supported media, which will result in the invalidation of the electroneutrality condition in CDL, and from the radial inhomogeneity of ET probability at nanometer-sized disk electrodes.

New molecular imprinted voltammetric sensor for determination of ochratoxin A

Energy Technology Data Exchange (ETDEWEB)

Yola, Mehmet Lütfi, E-mail: mehmetyola@gmail.com [Department of Metallurgical and Materials Engineering, Faculty of Engineering, Sinop University, Sinop (Turkey); Gupta, Vinod Kumar, E-mail: vinodfcy@iitr.ac.in [Indian Institute of Technology, Department of Chemistry, Roorkee, Roorkee 247667 (India); Department of Applied Chemistry, University of Johannesburg, Johannesburg (South Africa); Atar, Necip [Department of Chemical Engineering, Faculty of Engineering, Pamukkale University, Denizli (Turkey)

2016-04-01

In this report, a novel molecular imprinted voltammetric sensor based on silver nanoparticles (AgNPs) involved in a polyoxometalate (H{sub 3}PW{sub 12}O{sub 40}, POM) functionalized reduced graphene oxide (rGO) modified glassy carbon electrode (GCE) was presented for determination of ochrattoxin A (OCH). The developed surfaces were characterized using scanning electron microscope (SEM), transmission electron microscope (TEM), X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD) method. OCH imprinted GCE was prepared via electropolymerization process of 100 mM phenol as monomer in the presence of phosphate buffer solution (pH 6.0) containing 25 mM OCH. The linearity range and the detection limit of the method were calculated as 5.0 × 10{sup −11} − 1.5 × 10{sup −9} M and 1.6 × 10{sup −11} M, respectively. The voltammetric sensor was applied to grape juice and wine samples with good selectivity and recovery. The stability of the voltammetric sensor was also reported. - Highlights: • Ochratoxin A-imprinted electrochemical sensor is developed for the sensitive detection of ochratoxin A • The nanomaterial and ochratoxin A-imprinted surfaces were characterized by several methods • Ochratoxin A-imprinted electrochemical sensor is sensitive and selective in analysis of food • Ochratoxin A-imprinted electrochemical sensor is preferred to the other methods.

New molecular imprinted voltammetric sensor for determination of ochratoxin A

International Nuclear Information System (INIS)

Yola, Mehmet Lütfi; Gupta, Vinod Kumar; Atar, Necip

2016-01-01

In this report, a novel molecular imprinted voltammetric sensor based on silver nanoparticles (AgNPs) involved in a polyoxometalate (H_3PW_1_2O_4_0, POM) functionalized reduced graphene oxide (rGO) modified glassy carbon electrode (GCE) was presented for determination of ochrattoxin A (OCH). The developed surfaces were characterized using scanning electron microscope (SEM), transmission electron microscope (TEM), X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD) method. OCH imprinted GCE was prepared via electropolymerization process of 100 mM phenol as monomer in the presence of phosphate buffer solution (pH 6.0) containing 25 mM OCH. The linearity range and the detection limit of the method were calculated as 5.0 × 10"−"1"1 − 1.5 × 10"−"9 M and 1.6 × 10"−"1"1 M, respectively. The voltammetric sensor was applied to grape juice and wine samples with good selectivity and recovery. The stability of the voltammetric sensor was also reported. - Highlights: • Ochratoxin A-imprinted electrochemical sensor is developed for the sensitive detection of ochratoxin A • The nanomaterial and ochratoxin A-imprinted surfaces were characterized by several methods • Ochratoxin A-imprinted electrochemical sensor is sensitive and selective in analysis of food • Ochratoxin A-imprinted electrochemical sensor is preferred to the other methods

Voltammetric estimation of the content of antibiotics in veterinary preparations

Directory of Open Access Journals (Sweden)

Slepchenko Galina

2016-01-01

Full Text Available The voltammetric method for determination of tylosin tartrate, gentamicin sulfate, and cefalexin in veterinary preparations was for the first time developed. Electrochemical behavior of these antibiotics on the mercury film electrode was studied, and the working conditions (background electrolyte, deposition potential were defined for getting analytical signals using the voltammetry. The methods of real objects preparation for determination of tylosin tartrate, gentamicin sulfate, and cefalexin were offered. The techniques for the voltammetric determination of antibiotics in the veterinary preparations may be used in cefalexin ranging from 0.1 to 2.0 g/dm3, tylosin tartrate in the range from 0.1 to 1.7 g/dm3, and gentamicin sulfate from 0.1 to 1.5 g/dm3 (Sr is not more than 25 %

Comparison of nanostructured silver-modified silver and carbon ultramicroelectrodes for electrochemical detection of nitrate.

Science.gov (United States)

Lotfi Zadeh Zhad, Hamid R; Lai, Rebecca Y

2015-09-10

We report the use of silver (Ag)-modified carbon and Ag ultramicroelectrodes (UMEs) for electrochemical detection of nitrate. We investigated several methods for electrodeposition of Ag; our results show that the addition of a complexation agent (ammonium sulfate) in the Ag deposition solution is necessary for electrodeposition of nanostructured Ag that adheres well to the electrode. The electrodeposited Ag on both types of electrodes has branch-like structures that are well-suited for electrocatalytic reduction of nitrate. The use of UMEs is advantageous; the sigmoidal-shaped cyclic voltammogram allows for sensitive detection of nitrate by reducing the capacitive current, as well as enabling easy quantification of the nitrate reduction current. Both cyclic voltammetry and chronoamperometry were used to characterize the electrodes; and independent of the electrochemical interrogation technique, both UMEs were found to have a wide linear dynamic range (4-1000 μM) and a low limit of detection (3.2-5.1 μM). More importantly, they are reusable up to ∼100 interrogation cycles and are selective enough to be used for direct detection of nitrate in a synthetic aquifer sample without any sample pretreatment and/or pH adjustment. Copyright © 2015 Elsevier B.V. All rights reserved.

Voltammetric determination of zirconium using azo compounds

International Nuclear Information System (INIS)

Orshulyak, O.O.; Levitskaya, G.D.

2008-01-01

The optimum conditions for zirconium complexation with azo compounds are found. The applicability of Eriochrome Red B, Calcon, and Calcion to the voltammetric determination of zirconium, total Zr(IV) and Hf(IV), and Zr(IV) in the presence of Zn(II), Cu(II), Cd(II), Ni(II), or Ti(IV) is demonstrated. The developed procedures are used to determine zirconium in a terbium alloy and in an alloy for airplane wheel drums [ru

Voltammetric method to determine chromium (III) in potable water at level of ultra plans

International Nuclear Information System (INIS)

Jimenez B, Irene; Alvarado G, Ana L.

2004-01-01

It was established an analytical methodology to determine Cr (III) in drinking water using a voltammetric technique of Differential Pulse Cathodic Stripping Voltammetry with an Adsorptive Preconcentration of a complex Cr(III)-diethiltriaminpentaceticacid (Cr-DTPA) in a mercury drop. A dissolution of sodium nitrate was used as a supporting electrolyte. The optimized voltammetric parameters were: adsorption time, scan rate, absorption potential, p H, complex agent and sodium nitrate concentration. The linear range of the methodology is between 20 ng/L and 60 ng/L and the detection and quantification limits are 13 ng/L and 20 ng/L respectively. (Author) [es

Anodic Voltammetric determination of gemifloxacin using screen-printed carbon electrode

Directory of Open Access Journals (Sweden)

Abd-Elgawad Radi

2013-04-01

Full Text Available The electrochemical oxidation behavior and voltammetric assay of gemifloxacin were investigated using differential-pulse and cyclic voltammetry on a screen-printed carbon electrode. The effects of pH, scan rates, and concentration of the drug on the anodic peak current were studied. Voltammograms of gemifloxacin in Tris–HCl buffer (pH 7.0 exhibited a well-defined single oxidation peak. A differential-pulse voltammetric procedure for the quantitation of gemifloxacin has been developed and suitably validated with respect to linearity, limits of detection and quantification, accuracy, precision, specificity, and robustness. The calibration was linear from 0.5 to 10.0 μM, and the limits of detection and quantification were 0.15 and 5.0 μM. Recoveries ranging from 96.26% to 103.64% were obtained. The method was successfully applied to the determination of gemifloxacin in pharmaceutical tablets without any pre-treatment. Excipients present in the tablets did not interfere in the assay. Keywords: Screen-printed carbon electrode, Voltammetry, Gemifloxacin, Pharmaceutical analysis

Determination of total polyphenol index in wines employing a voltammetric electronic tongue

International Nuclear Information System (INIS)

Cetó, Xavier; Gutiérrez, Juan Manuel; Gutiérrez, Manuel; Céspedes, Francisco; Capdevila, Josefina; Mínguez, Santiago; Jiménez-Jorquera, Cecilia; Valle, Manel del

2012-01-01

Highlights: ► Array of voltammetric sensors modified with nanoparticles or conducting polymers. ► It has been applied in wine analysis to predict polyphenol content index. ► Uses data processing tools such as discrete wavelet transform and artificial neural network. ► Identification of phenolics like gallic acid, catechin, caffeic acid, catechol. ► Predicted polyphenol index agrees with Folin–Ciocalteau method and I 280 index. - Abstract: This work reports the application of a voltammetric electronic tongue system (ET) made from an array of modified graphite-epoxy composites plus a gold microelectrode in the qualitative and quantitative analysis of polyphenols found in wine. Wine samples were analyzed using cyclic voltammetry without any sample pretreatment. The obtained responses were preprocessed employing discrete wavelet transform (DWT) in order to compress and extract significant features from the voltammetric signals, and the obtained approximation coefficients fed a multivariate calibration method (artificial neural network-ANN-or partial least squares-PLS-) which accomplished the quantification of total polyphenol content. External test subset samples results were compared with the ones obtained with the Folin–Ciocalteu (FC) method and UV absorbance polyphenol index (I 280 ) as reference values, with highly significant correlation coefficients of 0.979 and 0.963 in the range from 50 to 2400 mg L −1 gallic acid equivalents, respectively. In a separate experiment, qualitative discrimination of different polyphenols found in wine was also assessed by principal component analysis (PCA).

Fusion of Potentiometric & Voltammetric Electronic Tongue for Classification of Black Tea Taste based on Theaflavins (TF) Content

Science.gov (United States)

Bhattacharyya, Nabarun; Legin, Andrey; Papieva, Irina; Sarkar, Subrata; Kirsanov, Dmitry; Kartsova, Anna; Ghosh, Arunangshu; Bandyopadhyay, Rajib

2011-09-01

Black tea is an extensively consumed beverage worldwide with an expanding market. The final quality of black tea depends upon number of chemical compounds present in the tea. Out of these compounds, theaflavins (TF), which is responsible for astringency in black tea, plays an important role in determining the final taste of the finished black tea. The present paper reports our effort to correlate the theaflavins contents with the voltammetric and potentiometric electronic tongue (e-tongue) data. Noble metal-based electrode array has been used for collecting data though voltammetric electronic tongue where as liquid filled membrane based electrodes have been used for potentiometric electronic tongue. Black tea samples with tea taster score and biochemical results have been collected from Tea Research Association, Tocklai, India for the analysis purpose. In this paper, voltammetric and potentiometric e-tongue responses are combined to demonstrate improvement of cluster formation among tea samples with different ranges of TF values.

Determination of total polyphenol index in wines employing a voltammetric electronic tongue

Energy Technology Data Exchange (ETDEWEB)

Ceto, Xavier [Sensors and Biosensors Group, Department of Chemistry, Universitat Autonoma de Barcelona, Edifici Cn, 08193 Bellaterra (Spain); Gutierrez, Juan Manuel [Bioelectronics Section, Department of Electrical Engineering, CINVESTAV, 07360 Mexico D.F. (Mexico); Gutierrez, Manuel [Instituto de Microelectronica de Barcelona (IMB-CNM), CSIC, 08193 Bellaterra (Spain); Cespedes, Francisco [Sensors and Biosensors Group, Department of Chemistry, Universitat Autonoma de Barcelona, Edifici Cn, 08193 Bellaterra (Spain); Capdevila, Josefina; Minguez, Santiago [Estacio de Viticultura i Enologia, INCAVI, Vilafranca del Penedes (Spain); Jimenez-Jorquera, Cecilia [Instituto de Microelectronica de Barcelona (IMB-CNM), CSIC, 08193 Bellaterra (Spain); Valle, Manel del, E-mail: manel.delvalle@uab.cat [Sensors and Biosensors Group, Department of Chemistry, Universitat Autonoma de Barcelona, Edifici Cn, 08193 Bellaterra (Spain)

2012-06-30

Highlights: Black-Right-Pointing-Pointer Array of voltammetric sensors modified with nanoparticles or conducting polymers. Black-Right-Pointing-Pointer It has been applied in wine analysis to predict polyphenol content index. Black-Right-Pointing-Pointer Uses data processing tools such as discrete wavelet transform and artificial neural network. Black-Right-Pointing-Pointer Identification of phenolics like gallic acid, catechin, caffeic acid, catechol. Black-Right-Pointing-Pointer Predicted polyphenol index agrees with Folin-Ciocalteau method and I{sub 280} index. - Abstract: This work reports the application of a voltammetric electronic tongue system (ET) made from an array of modified graphite-epoxy composites plus a gold microelectrode in the qualitative and quantitative analysis of polyphenols found in wine. Wine samples were analyzed using cyclic voltammetry without any sample pretreatment. The obtained responses were preprocessed employing discrete wavelet transform (DWT) in order to compress and extract significant features from the voltammetric signals, and the obtained approximation coefficients fed a multivariate calibration method (artificial neural network-ANN-or partial least squares-PLS-) which accomplished the quantification of total polyphenol content. External test subset samples results were compared with the ones obtained with the Folin-Ciocalteu (FC) method and UV absorbance polyphenol index (I{sub 280}) as reference values, with highly significant correlation coefficients of 0.979 and 0.963 in the range from 50 to 2400 mg L{sup -1} gallic acid equivalents, respectively. In a separate experiment, qualitative discrimination of different polyphenols found in wine was also assessed by principal component analysis (PCA).

Preparation and voltammetric characterization of electrodes coated with Langmuir-Schaefer ultrathin films of Nafion®

Directory of Open Access Journals (Sweden)

Bertoncello Paolo

2003-01-01

Full Text Available Ultrathin films of Nafion® perfluorinated polymer were deposited on indium-tin oxide electrodes (ITO by using Langmuir-Schaefer (LS technique, after optimization of the subphase composition conditions. Morphological characteristics of these coatings were obtained by Atomic Force Microscopy (AFM. Nafion® LS films showed a good uniformity and complete coverage of the electrode surface, however a different organization degree of the polymer layer was evidenced with respect to thin films deposited by spin-coating. ITO electrodes modified with Nafion® LS coatings preconcentrate by ion-exchange electroactive cations, such as Ru[(NH36]3+, dissolved in diluted solutions. The electroactive species is retained by the Nafion® LS coated ITO also after transfer of the modified electrode into pure supporting electrolyte. This allowed the use of the ruthenium complex as voltammetric probe to test diffusion phenomena within the Nafion® LS films. Apparent diffusion coefficients (Dapp of Ru[(NH36]3+ incorporated in Nafion® LS films were obtained by voltammetric measurements. Dapp values decrease slightly by increasing the amount of ruthenium complex incorporated in the ultrathin film. They are significantly lower than values typical for recasted Nafion® films, in agreement with the highly condensed nature of the Nafion® LS fims.

Direct voltammetric analysis of DNA modified with enzymatically incorporated 7-deazapurines

Czech Academy of Sciences Publication Activity Database

Pivoňková, Hana; Horáková Brázdilová, Petra; Fojtová, Miloslava; Fojta, Miroslav

2010-01-01

Roč. 82, č. 16 (2010), s. 6807-6813 ISSN 0003-2700 R&D Projects: GA AV ČR(CZ) IAA400040901; GA MŠk(CZ) LC06035 Institutional research plan: CEZ:AV0Z50040507; CEZ:AV0Z50040702 Keywords : modified DNA * 7-deazapurines * voltammetric analysis Subject RIV: BO - Biophysics Impact factor: 5.874, year: 2010

Voltammetric, in-situ spectroelectrochemical and in-situ electrocolorimetric characterization of phthalocyanines

Energy Technology Data Exchange (ETDEWEB)

Koca, Atif [Department of Chemical Engineering, Faculty of Engineering, Marmara University, Goeztepe, 34722 Istanbul (Turkey)], E-mail: akoca@eng.marmara.edu.tr; Bayar, Serife; Dincer, Hatice A. [Department of Chemistry, Technical University of Istanbul, Maslak, 34469 Istanbul (Turkey); Gonca, Erguen [Department of Chemistry, Fatih University, TR34500 B.Cekmece, Istanbul (Turkey)

2009-04-01

In this work, electrochemical, and in-situ spectroelectrochemical characterization of the metallophthalocyanines bearing tetra-(1,1-(dicarbethoxy)-2-(2-methylbenzyl))-ethyl 3,10,17,24-tetra chloro groups were performed. Voltammetric and in-situ spectroelectrochemical measurements show that while cobalt phthalocyanine complex gives both metal-based and ring-based redox processes, zinc and copper phthalocyanines show only ring-based reduction and oxidation processes. The redox processes are generally diffusion-controlled, reversible and one-electron transfer processes. Differently lead phthalocyanine demetallized during second oxidation reaction while it was stable during reduction processes. An in-situ electrocolorimetric method, based on the 1931 CIE (Commission Internationale de l'Eclairage) system of colorimetry, has been applied to investigate the color of the electro-generated anionic and cationic forms of the complexes for the first time in this study.

Adsorptive stripping voltammetric determination of trace amounts of lead in environmental water samples with complicated matrix

Directory of Open Access Journals (Sweden)

Grabarczyk M.

2013-04-01

Full Text Available A sensitive, simple and fast adsorptive stripping voltammetric procedure for trace determination of lead in environmental water samples has been developed. The method is based on adsorptive accumulation of the Pb(II-cupferron complex onto a hanging mercury drop electrode, followed by the reduction of the adsorbed species by a voltammetric scan using differential pulse modulation. The interference from surface active substances was eliminated by adsorption of interferents onto an Amberlite XAD-16 resin. Optimumconditions for removing the surfactants by mixing the analysed sample with resin were evaluated. The accuracy of the method was tested by analyzing certified reference material (SPS-WW1 Waste Water.

Using of multi-walled carbon nanotubes electrode for adsorptive stripping voltammetric determination of ultratrace levels of RDX explosive in the environmental samples.

Science.gov (United States)

Rezaei, Behzad; Damiri, Sajjad

2010-11-15

A study of the electrochemical behavior and determination of RDX, a high explosive, is described on a multi-walled carbon nanotubes (MWCNTs) modified glassy carbon electrode (GCE) using adsorptive stripping voltammetry and electrochemical impedance spectroscopy (EIS) techniques. The results indicated that MWCNTs electrode remarkably enhances the sensitivity of the voltammetric method and provides measurements of this explosive down to the sub-mg/l level in a wide pH range. The operational parameters were optimized and a sensitive, simple and time-saving cyclic voltammetric procedure was developed for the analysis of RDX in ground and tap water samples. Under optimized conditions, the reduction peak have two linear dynamic ranges of 0.6-20.0 and 8.0-200.0 mM with a detection limit of 25.0 nM and a precision of <4% (RSD for 8 analysis). Copyright © 2010 Elsevier B.V. All rights reserved.

Voltammetric behavior of amfepramone (diethylpropion) at the hanging mercury drop electrode and its analytical determination in pharmaceutical formulations

OpenAIRE

Carvalho, Leandro M. de; Nascimento, Paulo C. do; Bohrer, Denise; Correia, Daniele; Bairros, André V. de; Pomblum, Valdeci J.; Pomblum, Solange G.

2007-01-01

This paper describes a systematic study of the voltammetric behavior of amfepramone at the hanging mercury drop electrode (HMDE) by cyclic (CV) and alternating current (AC) voltammetric methods. The studies showed the adsorptive behavior of amfepramone at the HMDE and were performed in H2SO4 0.1 mol L-1 (pH 1.0) and Ringer buffer (pH 11.0) as supporting electrolytes. The linear range for the amfepramone determination by differential pulse voltammetry (DPV) was 0.05 to 2.0 mg L-1 (r = 0.998) i...

On the use of voltammetric methods to determine electrochemical stability limits for lithium battery electrolytes

Science.gov (United States)

Georén, Peter; Lindbergh, Göran

In previous studies a novel amphiphilic co-polymer was developed for use in lithium-ion batteries. In order to evaluate the electrochemical stability of that electrolyte and compare it with others, a voltammetric method was applied on a set of electrolytes with different salts, solvents and polymers. However, initially the voltammetric methodology was studied. Platinum was found to be the most suited electrode material, experiencing no significant interfering reactions and a proper diffusion-controlled kinetic behaviour when sweep rate was varied. Furthermore, the influence on the voltammograms of adding water traces to the electrolytes was studied. It could be established that the oxidation peak around 3.8 V versus Li was related to water reactions. It was concluded that quantitative voltage values of the stability limits were difficult to assess using voltammetry. On the other hand, the method seemed well suited for comparison of electrolytes and to investigate the influences of electrolyte components on the stability. The voltammetric results varied little between the different electrolytes evaluated and the anodic and cathodic limits, as defined here, were in the range of 1 and 4.5 V vs. Li, respectively. Although the novel polymer did not affect the stability limit significantly it seemed to promote the breakdown reaction rate in all electrolytes tested. Furthermore, the use of LiTFSI salt reduced the stability window.

Electrochemistry and determination of cefdinir by voltammetric and computational approaches

Directory of Open Access Journals (Sweden)

İbrahim Hüdai Taşdemir

2014-12-01

Full Text Available The oxidation and reduction behavior of cefdinir (CEF was studied by experimental methods and computational calculations at B3LYP/6-31+G (d//AM1. Voltammetric studies were carried out based on two irreversible reduction peaks at approximately −0.5 and −1.2 V on a hanging mercury drop electrode (HMDE and on one irreversible oxidation peak at approximately 1.0 V on a glassy carbon electrode (GCE versus Ag/AgCl, KCl (3.0M in Britton–Robinson (BR buffer at pH 4.2 and 5.0, respectively. Differential pulse adsorptive stripping voltammetric methods have been developed and validated for determination of CEF in different samples. The linear range was established as 0.25–40.0 μM for HMDE and 0.40–10.0 μM for GCE. Limit of quantification was calculated to be 0.20 and 0.26 μM for HMDE and GCE, respectively. These methods were successfully applied to assay the drug in tablets and human serum with good recoveries between 92.7% and 107.3% having relative standard deviation less than 10%.

Development and characterization of a voltammetric carbon-fiber microelectrode pH sensor.

Science.gov (United States)

Makos, Monique A; Omiatek, Donna M; Ewing, Andrew G; Heien, Michael L

2010-06-15

This work describes the development and characterization of a modified carbon-fiber microelectrode sensor capable of measuring real-time physiological pH changes in biological microenvironments. The reagentless sensor was fabricated under ambient conditions from voltammetric reduction of the diazonium salt Fast Blue RR onto a carbon-fiber surface in aprotic media. Fast-scan cyclic voltammetry was used to probe redox activity of the p-quinone moiety of the surface-bound molecule as a function of pH. In vitro calibration of the sensor in solutions ranging from pH 6.5 to 8.0 resulted in a pH-dependent anodic peak potential response. Flow-injection analysis was used to characterize the modified microelectrode, revealing sensitivity to acidic and basic changes discernible to 0.005 pH units. Furthermore, the modified electrode was used to measure dynamic in vivo pH changes evoked during neurotransmitter release in the central nervous system of the microanalytical model organism Drosophila melanogaster.

The decrease in hypothalamic dopamine secretion induced by suckling: comparison of voltammetric and radioisotopic methods of measurement

International Nuclear Information System (INIS)

Plotsky, P.M.; Neill, J.D.

1982-01-01

Previous in situ voltammetric microelectrode measurements of median eminence dopamine release during mammary nerve stimulation of anesthetized lactating rats revealed a transient (1-3 min) 70% decline of dopamine concentrations. This dopamine was believed to be destined for secretion into the hypophysial portal circulation, but direct experimental support for this supposition was lacking. Thus, in the present study, [3H]dopamine release into brief sequential samples of hypophysial portal blood was compared with dopamine release in the median eminence measured by voltammetry. Lactating female rats were urethane anesthetized, and the median eminence pituitary region was exposed. [3H]Tyrosine was injected into a jugular cannula (100 microCi) followed by continuous infusion (5 microCi/min). In a preliminary experiment, this regimen produced a steady state level of [3H]dopamine in the portal blood within 45 min. In subsequent experiments, portal blood was collected as sequential 3-min samples, and electrochemical sampling from a microelectrode placed in the median eminence occurred at 1-min intervals. Electrochemical current resulting from the oxidation of dopamine in the medial median eminence was unvarying throughout the 75-min experiment in control rats (n . 4) and during the 30-min control period preceding mammary nerve stimulation in the other group (n . 4). These results were paralled by [3H] dopamine levels in portal blood during the same periods of time. All animals showed simultaneous decreases in oxidation current and [3H]dopamine levels within 1-4 min after initiation of mammary nerve stimulation. These and earlier results demonstrate that mammary nerve stimulation (and by extension, suckling) induces a momentary, but profound, decrease in hypothalamic dopamine secretion which precedes or accompanies the rise in PRL secretion evoked by the same stimulus

Development of Voltammetric Double-Polymer-Modified Electrodes for Nanomolar Ion Detection for Environmental and Biological Applications

Science.gov (United States)

Kim, Yushin

Qualitative and quantitative electrochemical methods for trace ion analysis of organic and inorganic species with environmental and biological attention have been developed and reported during past decades. The development of fast and accurate electrochemical methods is critical for field applications with various blocking contaminants. Voltammetric method is attractive not only to analyze selective ion species due to its characteristic based on ion lipophilicity, but also to lower the limit of detection by combining with stripping analysis. In my PhD work, I have developed and studied a highly selective and sensitive electrochemical method that can be used to characterize fundamental transport dynamics and to develop electrochemical sensors at liquid/liquid interfaces based on electrochemically-controlled ion transfer and recognition. The understanding of the kinetic and thermodynamic properties of the voltammetric ion transfer through polymer-modified ion-selective electrodes leads to realize the highly selective and sensitive analytical method. The ultrathin polymer membrane is used to maximize a current response by complete exhaustion of preconcentrated ions. Therefore, nanomolar detection is achieved and confirmed by a thermodynamic mechanism that controls the detection limit. It was also demonstrated experimentally and theoretically that more lipophilic ionic species gives a significantly lower detection limit. The voltammetric method was expanded into inexpensive and disposable applications based on pencil lead modified with the thin polymer membrane. In the other hand, micropipet/nanopipet voltammetry as an artificial cell membrane was used to study the interface between two immiscible solutions for environmental and biomedical applications. It is very useful to get quantitative kinetic and thermodynamic information by studying numerical simulations of ion transfer and diffusion. Molecular recognition and transport of heparin and low

Sensitive voltammetric detection of yeast RNA based on its interaction with Victoria Blue B

Directory of Open Access Journals (Sweden)

WEI SUN

2009-12-01

Full Text Available Voltammetric studies of the interaction of yeast RNA (y-RNA with Victoria Blue B (VBB are described in this paper. Furthermore, a linear sweep voltammetric method for the detection of y-RNA was established. The reaction conditions, such as acidity and amount of buffer solution, the concentration of VBB, the reaction time and temperature, etc., were carefully investigated by second order derivative linear sweep voltammetry. Under the optimal conditions, the reduction peak current of VBB at –0.75 V decreased greatly after the addition of y-RNA to the solution without any shift of the reduction peak potential. Based on the decrease of the peak current, a new quantitative method for the determination of y-RNA was developed. The effects of co-existing substances on the determination were carefully investigated and three synthetic samples were determined with satisfactory results. The stoichiometry of the VBB–y-RNA complex was calculated by linear sweep voltammetry and the interaction mechanism is discussed.

Voltammetric methods for determination and speciation of inorganic arsenic in the environment-A review

Energy Technology Data Exchange (ETDEWEB)

Mays, Douglas E. [Centre for Clean Water and Sustainable Technologies, Department of Chemistry and Biochemistry, George Mason University, Fairfax, VA 20120 (United States); Hussam, Abul, E-mail: ahussam@gmu.edu [Centre for Clean Water and Sustainable Technologies, Department of Chemistry and Biochemistry, George Mason University, Fairfax, VA 20120 (United States)

2009-07-30

The measurement of inorganic arsenic in the environment has received considerable attention over the past 40+ years due to its toxicity and prevalence in drinking water. This paper provides an overview of voltammetric techniques used since 2001. More than fifty papers from refereed analytical chemistry journals on the speciation and measurement of inorganic arsenic (As(III) and As(V)) in practical and environmental samples are included. The present review shows that stripping voltammetry is a sensitive and inexpensive technique. The new approaches include development of novel measurement protocols through media variation, development and use of new boron doped diamond electrodes modified with metals, nano Au-modified electrodes on carbon or carbon nano-tubes, novel rotating disc and vibrating electrodes to enhance mass transfer, and modified Hg(l) and thin film Bi on carbon for cathodic stripping voltammetry are discussed. Although, majority of the papers were of exploratory in nature, the trend towards developing a commercial standalone instrument for field use is still in progress.

Novel approach for the voltammetric evaluation of antioxidant activity using DPPH·-modified electrode

International Nuclear Information System (INIS)

Ziyatdinova, Guzel; Snegureva, Yulia; Budnikov, Herman

2017-01-01

Highlights: •Voltammetric characteristics of DPPH· immobilized on the electrode surface is studied. •DPPH·/CeO 2 -CPB/GCE gives reversible one electron highly sensitive radical reduction. •DPV on DPPH·/CeO 2 -CPB/GCE is developed for the antioxidants activity evaluation. •Natural phenolic antioxidants and medicinal herbs extracts are investigated. •Good agreement of DPV and standard method data is obtained. -- Abstract: The electrochemical behavior of 2,2-diphenyl-1-picrylhydrazyl (DPPH·) immobilized on the electrode surface has been studied. Bare glassy carbon electrode (GCE) and modified with dispersions of CeO 2 nanoparticles in water (CeO 2 -H 2 O/GCE) and cationic surfactant cetylpyridinium bromide medium (CeO 2 -CPB/GCE) has been investigated as a platform for the DPPH· immobilization. The best voltammetric characteristics (peak potential separation of 70 mV, system reversibility with currents ratio of 0.98 and the highest peaks currents) have been observed on CeO 2 -CPB/GCE. The effect of CeO 2 nanoparticles concentration has been evaluated. Scanning electron microscopy and electrochemical impedance spectroscopy have been applied for the electrode characterization. DPPH·/CeO 2 -CPB/GCE has been used for the estimation of the antioxidants activity of natural phenolic antioxidants (quercetin, tannin, catechin and ferulic acid) expressed as the EC 50 parameter according to differential pulse voltammetric (DPV) data. The EC 50 decreased in the following order: quercetin (29 ± 1 μM), tannin (29 ± 4 μM), catechin (117 ± 4 μM) and ferulic acid (731 ± 17 μM). These data are in a good agreement with the results of standard spectrophotometric determination. The developed approach has been successfully applied for the antioxidant activity evaluation of medicinal herbs tinctures, infusions and decoctions.

Dual Approach to Amplify Anodic Stripping Voltammetric Signals Recorded Using Screen Printed Electrodes

Directory of Open Access Journals (Sweden)

Agnieszka KRÓLICKA

2016-12-01

Full Text Available Screen printed electrodes plated with bismuth were used to record anodic stripping voltammograms of Pb(II, In(III and Cd(II. Using two bismuth precursors: Bi2O3 dispersed in the electrode body and Bi(III ions spiked into the tested solution it was possible to deposit bismuth layers, demonstrating exceptional ability to accumulate metals forming alloys with bismuth. The voltammetric signals were amplified by adjusting the electrode location with respect to rotating magnetic field. The electrode response was influenced by vertical and horizontal distance between the magnet center and the sensing area of screen printed electrode as well as the angle between the magnet surface and the electrode. When the electrode was moved away from the magnet center the recorded peaks were increasingly smaller and almost not affected by the presence of bismuth ions. It was shown that to obtain well-shaped signals a favourable morphology of bismuth deposits is of key importance. Hypotheses explaining processes responsible for the amplification of voltammetric signals were proposed.

Discrimination of Apple Liqueurs (Nalewka) Using a Voltammetric Electronic Tongue, UV-Vis and Raman Spectroscopy.

Science.gov (United States)

Śliwińska, Magdalena; Garcia-Hernandez, Celia; Kościński, Mikołaj; Dymerski, Tomasz; Wardencki, Waldemar; Namieśnik, Jacek; Śliwińska-Bartkowiak, Małgorzata; Jurga, Stefan; Garcia-Cabezon, Cristina; Rodriguez-Mendez, Maria Luz

2016-10-09

The capability of a phthalocyanine-based voltammetric electronic tongue to analyze strong alcoholic beverages has been evaluated and compared with the performance of spectroscopic techniques coupled to chemometrics. Nalewka Polish liqueurs prepared from five apple varieties have been used as a model of strong liqueurs. Principal Component Analysis has demonstrated that the best discrimination between liqueurs prepared from different apple varieties is achieved using the e-tongue and UV-Vis spectroscopy. Raman spectra coupled to chemometrics have not been efficient in discriminating liqueurs. The calculated Euclidean distances and the k-Nearest Neighbors algorithm (kNN) confirmed these results. The main advantage of the e-tongue is that, using PLS-1, good correlations have been found simultaneously with the phenolic content measured by the Folin-Ciocalteu method (R² of 0.97 in calibration and R² of 0.93 in validation) and also with the density, a marker of the alcoholic content method (R² of 0.93 in calibration and R² of 0.88 in validation). UV-Vis coupled with chemometrics has shown good correlations only with the phenolic content (R² of 0.99 in calibration and R² of 0.99 in validation) but correlations with the alcoholic content were low. Raman coupled with chemometrics has shown good correlations only with density (R² of 0.96 in calibration and R² of 0.85 in validation). In summary, from the three holistic methods evaluated to analyze strong alcoholic liqueurs, the voltammetric electronic tongue using phthalocyanines as sensing elements is superior to Raman or UV-Vis techniques because it shows an excellent discrimination capability and remarkable correlations with both antioxidant capacity and alcoholic content-the most important parameters to be measured in this type of liqueurs.

Emerging trends in biosensing using stripping voltammetric detection of metal-containing nanolabels – A review

Energy Technology Data Exchange (ETDEWEB)

Kokkinos, Christos; Economou, Anastasios, E-mail: aeconomo@chem.uoa.gr

2017-04-08

Over the last years, nanomaterials have found many applications in the development of electrochemical biosensors. Among other functions, metal nanoparticles (NPs) and quantum dots (QDs) (semiconducting nanocrystals composed of metal salts) are increasingly being used as voltammetric labels in affinity biosensing. Labeling is based on the attachment of the label(s) on the target biomolecules or on a biorecognition reporting probe. After an appropriate specific affinity interaction between the target and the reporting probe, the metallic nanolabels are converted to the respective cations which are quantified by a voltammetric technique. The very use of metal-containing nanoprobes as labels provides a first amplification step since each nanoprobe can release a very significant number of detectable cations. When anodic stripping voltammetry (ASV) (in which a preconcentration step precedes the actual voltammetric scan) is further employed as the detection format, ultra-sensitive bioassays can be developed. The present paper reviews the emerging trends in affinity biosensing using ASV detection of metal-containing nanolabels. It provides a critical discussion of recent developments in ASV transduction and electrodes, novel strategies for signal enhancement, approaches for multiplexed detection as well as fluidics, paper-based and lab-on-a-chip devices. - Highlights: • This paper reviews the use of ASV for affinity biosensing with metal-containing nanolabels. • Both metal nanoparticles and quantum dots applications are considered. • Transducers and new electrode materials are covered. • Signal enhancement and multiplexing strategies are discussed. • Sensor arrays, paper-based, fluidic and lab-on-chip applications are described.

Adsorptive stripping voltammetric determination of triprolidine hydrochloride in pharmaceutical tablets.

Science.gov (United States)

Zayed, S I M; Habib, I H I

2005-01-01

The electrochemical behavior of antihistaminic drug, viz. triprolidine hydrochloride (TripCl), at a hanging mercury drop electrode (HMDE) is investigated. Chemical and electrical parameters affecting the adsorptive voltammetric measurements are optimized. Different modes of sweep, viz. direct current DC, normal pulse NP, differential pulse DP and square wave SW modes, over the potential range from -800 to -1400 mV, are used in the presence of 0.04 M Britton-Robinson buffer pH 11, with accumulation time 30 s, scan rate 50 mV/s and pulse amplitude 50 mV. The reduction process is irreversible and involved the transfer of two electrons and two protons. Their responses are linear over the concentration range 15-157 ng/ml with average correlation coefficient 0.9998, while the detection limit is 2.64, 6.24, 8.80 and 2.12 ng/ml for DC, DP, SW and NP mode, respectively. The differential pulse method has been applied successfully for the determination of the drug in Egyptian pharmaceutical preparation with mean recovery 99.55+/-0.67%.

Classification of monofloral honeys by voltammetric electronic tongue with chemometrics method

Energy Technology Data Exchange (ETDEWEB)

Wei Zhenbo [Department of Bio-systems Engineering, Zhejiang University, 268 Kaixuan Road, Hangzhou 310029, Zhejiang (China); Wang Jun, E-mail: jwang@zju.edu.cn [Department of Bio-systems Engineering, Zhejiang University, 268 Kaixuan Road, Hangzhou 310029, Zhejiang (China)

2011-05-01

Highlights: > We self-developed a voltammetric electronic tongue based on new sensors array. > We advanced a new method to extract eigenvalues from signals obtained by VE-tongue. > We first detected the monofloral honeys of different floral origins using VE-tongue. - Abstract: A voltammetric electronic tongue (VE-tongue) based on multifrequency large amplitude pulse voltammetry (MLAPV) was developed to classify monofloral honeys of seven kinds of floral origins. The VE-tongue was composed of six working electrodes (gold, silver, platinum, palladium, tungsten, and titanium) in a standard three-electrode configuration. The applied waveform of MLAPV was composed of four individual frequencies: 1 Hz, 10 Hz, 100 Hz, and 1000 Hz. Two eigenvalues (the maximum value and the minimum value) of each cycle were extracted for building the first database (FDB); four eigenvalues (the maximum value, the minimum value, and two inflexion values) were exacted for building the second database (SDB). The two databases were analyzed by three-pattern recognition techniques: principal component analysis (PCA), discriminant function analysis (DFA) and cluster analysis (CA), respectively. It was possible to discriminate the seven kinds of honeys of different floral origins completely based on FDB and SDB by PCA, DFA and CA, and FDB was certificated as an efficient database by contrasting with the SDB. Moreover, the effective working electrodes and frequencies were picked out as the best experimental project for the further study.

Cathodic adsorptive stripping voltammetric determination of Ribavirin in pharmaceutical dosage form, urine and serum

Directory of Open Access Journals (Sweden)

Ahmed A. Abdel Gaber

2017-05-01

Full Text Available A sensitive, simple and rapid square-wave adsorptive stripping voltammetric method was developed and validated for the determination of Ribavirin in pharmaceutical formulations. The proposed method was based on the electrochemical reduction of Ribavirin at a hanging mercury drop electrode in Britton Robinson buffer at pH 10. A well-defined peak was observed at 880 mV with 30 s of accumulation time and 50 mV of accumulation potential. Under these optimized conditions, the square-wave adsorptive stripping voltammetric peak current showed a linear correlation on drug concentration over the range of 1 × 10−10–2 × 10−7 mol L−1 with a correlation coefficient of 0.9995 for the proposed method. The detection and quantitation limits for this method were 2.02 × 10−10 and 6.80 × 10−10 mol L−1, respectively. The results obtained for intra-day and inter-day precision (as RSD % were between 0.447% and 1.024%. This method was applied successfully for the determination of Ribavirin in its pharmaceutical dosage forms with mean recoveries of 99.68 ± 0.13 with RSD % of 0.81% and 99.20 ± 0.24 with RSD % of 0.49% for two concentrations 5 × 10−9 and 5 × 10−8 mol L−1, respectively for 200 mg capsules. The results obtained from the developed square-wave adsorptive stripping voltammetric method were compared with those obtained by the analytical method reported in the literature.

Voltammetric determination of copper in selected pharmaceutical preparations--validation of the method.

Science.gov (United States)

Lutka, Anna; Maruszewska, Małgorzata

2011-01-01

It were established and validated the conditions of voltammetric determination of copper in pharmaceutical preparations. The three selected preparations: Zincuprim (A), Wapń, cynk, miedź z wit. C (B), Vigor complete (V) contained different salts and different quantity of copper (II) and increasing number of accompanied ingredients. For the purpose to transfer copper into solution, the samples of powdered tablets of the first and second preparation were undergone extraction and of the third the mineralization procedures. The concentration of copper in solution was determined by differential pulse voltammetry (DP) using comparison with standard technique. In the validation process, the selectivity, accuracy, precision and linearity of DP determination of copper in three preparations were estimated. Copper was determined within the concentration range of 1-9 ppm (1-9 microg/mL): the mean recoveries approached 102% (A), 100% (B), 102% (V); the relative standard deviations of determinations (RSD) were 0.79-1.59% (A), 0.62-0.85% (B) and 1.68-2.28% (V), respectively. The mean recoveries and the RSDs of determination satisfied the requirements for the analyte concentration at the level 1-10 ppm. The statistical verification confirmed that the tested voltammetric method is suitable for determination of copper in pharmaceutical preparation.

Voltammetric Behaviour of Metronidazole at Mercury Electrodes

Directory of Open Access Journals (Sweden)

La-Scalea Mauro A.

1999-01-01

Full Text Available Metronidazole is the most important drug of the group of 5-nitroimidazoles and possesses toxicity to anaerobic micro-organisms DNA being the main target for their biological action. The mechanism of biological action of metronidazole is dependent upon the nitro group reduction process. The reduction of metronidazole is pH dependent in acid medium and four electrons are involved in the complete reduction to the hydroxylamine derivative. In aprotic medium the reduction of the metronidazole occurs in two steps, the first involving one electron to form the nitro radical and the second step involving three more electrons until the formation of the hydroxylamine derivative. In this paper the mechanism of reduction of metronidazole was studied by using the voltammetric techniques: d.c. polarography, differential pulse polarography and cyclic voltammetry using the mercury drop as the working electrode.

Voltammetric analysis of N-containing drugs using the hanging galinstan drop electrode (HGDE).

Science.gov (United States)

Channaa, H; Surmann, P

2009-03-01

The electrochemical behaviour of several N-containing voltammetric active drugs such as 1,4-benzodiazepines (chlordiazepoxide, nitrazepam and diazepam) as well as one nitro-compound (nitrofurantoin) and one azo-compound (phenazopyridine) is described using a new kind of liquid electrode, the hanging galinstan drop electrode. Concentrations of 10(-5) - 10(-8) mol L(-1) are generally measurable. Differential pulse and adsorptive stripping voltammograms are recorded in different supporting electrolytes, like 0.1 M KNO3, acetate buffer solution pH = 4.6 and phosphate buffer solution pH = 7.0. The effects of varying the starting potentials, U(start) for DPV and accumulation times, t(acc) for AdSV are considered. Briefly, it is shown that the novel galinstan electrode is suitable for reducing several functional groups in organic substances, here presented for N-oxide-, azomethine-, nitro- and azo-groups.

Adsorptive Cathodic Stripping Voltammetric Determination of Cefoperazone in Bulk Powder, Pharmaceutical Dosage Forms, and Human Urine

Directory of Open Access Journals (Sweden)

Vu Dang Hoang

2013-01-01

Full Text Available The electroreduction behaviour and determination of cefoperazone using a hanging mercury drop electrode were investigated. Cyclic voltammograms of cefoperazone recorded in universal Britton-Robinson buffers pH 3–6 exhibited a single irreversible cathodic peak. The process was adsorption-controlled. Britton-Robinson buffer 0.04 M pH 4.0 was selected as a supporting electrolyte for quantitative purposes by differential pulse and square wave adsorptive cathodic stripping voltammetry. The experimental voltammetric conditions were optimized using Central Composite Face design. A reduction wave was seen in the range from −0.7 to −0.8 V. These voltammetric techniques were successfully validated as per ICH guidelines and applied for the determination of cefoperazone in its single and sulbactam containing powders for injection and statistically comparable to USP-HPLC. They were further extended to determine cefoperazone in spiked human urine with no matrix effect.

Voltammetric Determination of Lead (II) and Cadmium (II) Using a Bismuth Film Electrode Modified with Mesoporous Silica Nanoparticles

International Nuclear Information System (INIS)

Yang, Die; Wang, Liang; Chen, Zuliang; Megharaj, Mallavarapu; Naidu, Ravi

2014-01-01

A new chemically modified glassy carbon electrode based on bismuth film coated mesoporous silica nanoparticles was developed and evaluated for reliable quantification of trace Pb 2+ and Cd 2+ by anodic stripping square wave voltammetry in natural water samples. Compared with conventional bismuth film electrodes or bismuth nanoparticles modified electrodes, this electrode exhibited significantly improved sensitivity and stability for Pb 2+ and Cd 2+ detection. The key experimental parameters related to the fabrication of the electrode and the voltammetric measurements were optimized on the basis of the stripping signals, where the peak currents increased linearly with the metal concentrations in a range of 2-150 μg L −1 with a detect limit of 0.2 μg L −1 for Pb 2+ , and 0.6 μg L −1 for Cd 2+ for 120s deposition. Good reproducibility was achieved on both single and equally prepared electrodes. In addition, scanning electron microscopy reveals that fibril-like bismuth structures were formed on silica nanoparticles, which could be responsible for the improved voltammetric performance due to the enhanced surface area. Finally, the developed electrode was applied to determine Pb 2+ and Cd 2+ in water samples, indicating that this electrode was sensitive, reliable and effective for the simultaneous determination of Pb 2+ and Cd 2+

Voltammetric method for the determination of sildenafil citrate (Viagra) in pure form and in pharmaceutical formulations.

Science.gov (United States)

Tyszczuk, Katarzyna; Korolczuk, Mieczyslaw

2010-06-01

A highly sensitive and simple voltammetric method for the determination of sildenafil citrate (SC) was developed. The method is based on the accumulation by adsorption of SC on a lead film modified glassy carbon electrode (LF/GCE) and then the reduction of SC throughout the stripping step. During the determinations of SC at the lead film electrode three adsorptive stripping voltammetric peaks at -1.2, -1.33 and -1.45V were observed. The respective response selected for identification and quantification has been evaluated with respect to the composition and pH of the supporting electrolyte, the potential and the time of the lead film formation, the potential and the time of the SC accumulation and other variables. Experimental results indicate an excellent linear correlation between the peak current and concentration in the range of 2x10(-9)-1.5x10(-7)mol/L (for peaks 1 and 2) and 1x10(-8)-1.5x10(-7)mol/L (for the peak 3). The detection limits (LOD) for SC following 30s of accumulation time were equal to 9x10(-10)mol/L (for peaks 1 and 2) and 4.5x10(-9)mol/L (for the peak 3). The method was successfully applied to the determination of SC in the tablets (Viagra 25 and Viagra 50) and average the contents were in close agreement with those quoted by the manufacturer and with those obtained by the reported spectrophotometric method and voltammetric method using a hanging mercury drop electrode. Copyright 2009 Elsevier B.V. All rights reserved.

Voltammetric technique, a panacea for analytical examination of environmental samples

International Nuclear Information System (INIS)

Zahir, E.; Mohiuddin, S.; Naqvi, I.I.

2012-01-01

Voltammetric methods for trace metal analysis in environmental samples of marine origin like mangrove, sediments and shrimps are generally recommended. Three different electro-analytical techniques i.e. polarography, anodic stripping voltammetry (ASV) and adsorptive stripping voltammetry (ADSV) have been used. Cd/sub 2/+, Pb/sub 2/+, Cu/sub 2/+ and Mn/sub 2/+ were determined through ASV, Cr/sub 6/+ was analyzed by ADSV and Fe/sub 2/+, Zn/sub 2/+, Ni/sub 2/+ and Co/sub 2/+ were determined through polarography. Out of which pairs of Fe/sub 2/+Zn/sub 2/+ and Ni/sub 2/+Co/sub 2/+ were determined in two separate runs while Cd/sub 2/+, Pb/sub 2/+, Cu/sub 2/+ were analyzed in single run of ASV. Sensitivity and speciation capabilities of voltammetric methods have been employed. Analysis conditions were optimized that includes selection of supporting electrolyte, pH, working electrodes, sweep rate etc. Stripping voltammetry was adopted for analysis at ultra trace levels. Statistical parameters for analytical method development like selectivity factor, interference, repeatability (0.0065-0.130 macro g/g), reproducibility (0.08125-1.625 macro g/g), detection limits (0.032-5.06 macro g/g), limits of quantification (0.081-12.652 macro g/g), sensitivities (5.636-2.15 nA mL macro g-1) etc. were also determined. The percentage recoveries were found in between 95-105% using certified reference materials. Real samples of complex marine environment from Karachi coastline were also analyzed. The standard addition method was employed where any matrix effect was evidenced. (author)

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

Science.gov (United States)

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.

Voltammetric determination of heparin based on its interaction with malachite green

Directory of Open Access Journals (Sweden)

Xueliang Niu

2008-08-01

Full Text Available In this paper malachite green (MG was used as a bioprobe to determine heparin concentration by linear sweep voltammetry on the dropping mercury working electrode (DME. In Britton-Robinson (B-R buffer solution of pH 1.5, MG had a well-defined second order derivative linear sweep voltammetric reductive peak at –0.618 V (vs. SCE. After the addition of heparin into the MG solution, the reductive peak current decreased apparently without the movement of peak potential. Based on the difference of the peak current, a new voltammetric method for the determination of heparin was established. The conditions for the binding reaction and the electrochemical detection were optimized. Under the selected experimental conditions the difference of peak current was directly proportional to the concentration of heparin in the range from 0.3 to 10.0 mg/L with the linear regression equation as ∆ip″ (nA = 360.19 C (mg/L + 178.88 (n = 15, γ = 0.998 and the detection limit as 0.28 mg/L (3σ. The effects of coexisting substances such as metal ions, amino acids on the determination of heparin were investigated and the results showed that this method had good selectivity. This method was further applied to determine the heparin content in heparin sodium injection samples with satisfactory results and good recovery. The stoichiometry of the biocomplex was calculated by the electrochemical method and the binding mechanism was further discussed.

Voltammetric Behaviour of Sulfamethoxazole on Electropolymerized-Molecularly Imprinted Overoxidized Polypyrrole

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Yücel Sahin

2008-12-01

Full Text Available In this work, preparation of a molecularly imprinted polymer (MIP film and its recognition properties for sulfamethoxazolewere investigated. The overoxidized polypyrrole (OPPy film was prepared by the cyclic voltammetric deposition of pyrrole (Py in the presence of supporting electrolyte (tetrabutylammonium perchlorate-TBAP with and without a template molecule (sulfamethoxazole on a pencil graphite electrode (PGE. The voltammetric behaviour of sulfamethoxazole on imprinted and non-imprinted (NIP films was investigated by differential pulse voltammetry (DPV in Britton-Robinson (BR buffer solutions prepared in different ratio of acetonitrile-water binary mixture, between the pH 1.5 and 7.0. The effect of the acetonitrile-water ratio and pH, monomer and template concentrations, electropolymerization cycles on the performance of the MIP electrode was investigated and optimized. The MIP electrode exhibited the best reproducibility and highest sensitivity. The results showed that changing acetonitrile-water ratio and pH of BR buffer solution changes the oxidation peak current values. The highest anodic signal of sulfamethoxazole was obtained in BR buffer solution prepared in 50% (v/v acetonitrile-water at pH 2.5. The calibration curve for sulfamethoxazole at MIP electrode has linear region for a concentration range of 25.10-3 to 0.75 mM (R2=0.9993. The detection limit of sulfamethoxazole was found as 3.59.10-4 mM (S/N=3. The same method was also applied to determination of sulfamethoxazole in commercial pharmaceutical samples. Method precision (RSD87% were satisfactory. The proposed method is simple and quick. The polypyrrole (PPy electrodes have low response time, good mechanical stability and are disposable simple to construct.

Electrochemical Oxidation of l-selenomethionine and Se-methylseleno-l-cysteine at a Thiol-Compound-Modified Gold Electrode: Its Application in a Flow-Through Voltammetric Sensor

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Lai-Hao Wang

2017-02-01

Full Text Available A flow-electrolytic cell that consists of a bare gold wire or of different thiol-compound-modified gold electrodes (such as 2,4-thiazolidinedione, 2-mercapto-5-thiazoline, 2-mercaptothiazoline, l-cysteine, thioglycolic acid was designed to be used in a voltammetric detector to identify l-selenomethionine and Se-methylseleno-l-cysteine using high-performance liquid chromatography. Both l-selenomethionine and Se-methylseleno-l-cysteine are more efficiently electrochemically oxidized on a thiol/gold than on a bare gold electrode. For the DC mode, and for measurements with suitable experimental parameters, a linear concentration from 10 to 1600 ng·mL−1 was found. The limits of quantification for l-selenomethionine and Se-methylseleno-l-cysteine were below 10 ng·mL−1. The method can be applied to the quantitative determination of l-selenomethionine and Se-methylseleno-l-cysteine in commercial selenium-containing supplement products. Findings using high-performance liquid chromatography with a flow-through voltammetric detector and ultraviolet detector are comparable.

Voltammetric behavior of sedative drug midazolam at glassy carbon electrode in solubilized systems

OpenAIRE

Jain, Rajeev; Yadav, Rajeev Kumar

2012-01-01

Redox behavior of midazolam was studied at a glassy carbon electrode in various buffer systems, supporting electrolytes and pH using differential pulse, square-wave and cyclic voltammetry. Based on its reduction behavior, a direct differential pulse voltammetric method has been developed and validated for the determination of midazolam in parenteral dosage. Three well-defined peaks were observed in 0.1% SLS, BrittonâRobinson (BR) buffer of pH 2.5. The effect of surfactants like sodium lauryl ...

Voltammetric behavior of sedative drug midazolam at glassy carbon electrode in solubilized systems

OpenAIRE

Jain, Rajeev; Yadav, Rajeev Kumar

2011-01-01

Redox behavior of midazolam was studied at a glassy carbon electrode in various buffer systems, supporting electrolytes and pH using differential pulse, square-wave and cyclic voltammetry. Based on its reduction behavior, a direct differential pulse voltammetric method has been developed and validated for the determination of midazolam in parenteral dosage. Three well-defined peaks were observed in 0.1% SLS, Britton–Robinson (BR) buffer of pH 2.5. The effect of surfactants like sodium lauryl ...

Electrodeposition of Isolated Platinum Atoms and Clusters on Bismuth-Characterization and Electrocatalysis.

Science.gov (United States)

Zhou, Min; Dick, Jeffrey E; Bard, Allen J

2017-12-06

We describe a method for the electrodeposition of an isolated single Pt atom or small cluster, up to 9 atoms, on a bismuth ultramicroelectrode (UME). This deposition was immediately followed by electrochemical characterization via the hydrogen evolution reaction (HER) that occurs readily on the electrodeposited Pt but not on Bi. The observed voltammetric current plateau, even for a single atom, which behaves as an electrode, allows the estimation of deposit size. Pt was plated from solutions of femtomolar PtCl 6 2- , which allowed precise control of the arrival of ions and thus the plating rate on the Bi UME, to one ion every few seconds. This allowed the atom-by-atom fabrication of isolated platinum deposits, ranging from single atoms to 9-atom clusters. The limiting currents in voltammetry gave the size and number of atoms of the clusters. Given the stochasticity of the plating process, we show that the number of atoms plated over a given time (10 and 20 s) follows a Poisson distribution. Taking the potential at a certain current density as a measure of the relative rate of the HER, we found that the potential shifted positively as the size increased, with single atoms showing the largest overpotentials compared to bulk Pt.

Vapor permeation-stepwise injection simultaneous determination of methanol and ethanol in biodiesel with voltammetric detection.

Science.gov (United States)

Shishov, Andrey; Penkova, Anastasia; Zabrodin, Andrey; Nikolaev, Konstantin; Dmitrenko, Maria; Ermakov, Sergey; Bulatov, Andrey

2016-02-01

A novel vapor permeation-stepwise injection (VP-SWI) method for the determination of methanol and ethanol in biodiesel samples is discussed. In the current study, stepwise injection analysis was successfully combined with voltammetric detection and vapor permeation. This method is based on the separation of methanol and ethanol from a sample using a vapor permeation module (VPM) with a selective polymer membrane based on poly(phenylene isophtalamide) (PA) containing high amounts of a residual solvent. After the evaporation into the headspace of the VPM, methanol and ethanol were transported, by gas bubbling, through a PA membrane to a mixing chamber equipped with a voltammetric detector. Ethanol was selectively detected at +0.19 V, and both compounds were detected at +1.20 V. Current subtractions (using a correction factor) were used for the selective determination of methanol. A linear range between 0.05 and 0.5% (m/m) was established for each analyte. The limits of detection were estimated at 0.02% (m/m) for ethanol and methanol. The sample throughput was 5 samples h(-1). The method was successfully applied to the analysis of biodiesel samples. Copyright © 2015 Elsevier B.V. All rights reserved.

Voltammetric studies on the electrochemical determination of methylmercury in chloride medium at carbon microelectrodes

Energy Technology Data Exchange (ETDEWEB)

Ribeiro, F. [Centro de Electroquimica e Cinetica da Universidade de Lisboa, Departamento de Quimica e Bioquimica, Faculdade de Ciencias, Universidade de Lisboa, Campo Grande, Ed. C8, 1749-016 Lisbon (Portugal); Neto, M.M.M. [Centro de Electroquimica e Cinetica da Universidade de Lisboa, Departamento de Quimica e Bioquimica, Faculdade de Ciencias, Universidade de Lisboa, Campo Grande, Ed. C8, 1749-016 Lisbon (Portugal) and Departamento de Quimica Agricola e Ambiental, Instituto Superior de Agronomia, Tapada da Ajuda, 1349-017 Lisbon (Portugal)]. E-mail: mm.neto@netcabo.pt; Rocha, M.M. [Centro de Electroquimica e Cinetica da Universidade de Lisboa, Departamento de Quimica e Bioquimica, Faculdade de Ciencias, Universidade de Lisboa, Campo Grande, Ed. C8, 1749-016 Lisbon (Portugal); Fonseca, I.T.E. [Centro de Electroquimica e Cinetica da Universidade de Lisboa, Departamento de Quimica e Bioquimica, Faculdade de Ciencias, Universidade de Lisboa, Campo Grande, Ed. C8, 1749-016 Lisbon (Portugal)

2006-10-10

Electroanalytical techniques have been used to determine methylmercury at low levels in environmental matrices. The electrochemical behaviour of methylmercury at carbon microelectrodes in a hydrochloric acid medium using cyclic, square wave and fast-scan linear-sweep voltammetric techniques has been investigated. The analytical utility of the methylmercury reoxidation peak has been explored, but the recorded peak currents were found to be poorly reproducible. This is ascribed to two factors: the adsorption of insoluble chloromercury compounds on the electrode surface, which appears to be an important contribution to hinder the voltammetric signal of methylmercury; and the competition between the reoxidation of the methylmercury radical and its dimerization reaction, which limits the reproducibility of the methylmercury peak. These problems were successfully overcome by adopting the appropriate experimental conditions. Fast-scan rates were employed and an efficient electrochemical regeneration procedure of the electrode surface was achieved, under potentiostatic conditions in a mercury-free solution containing potassium thiocyanate-a strong complexing agent. The influence of chloride ion concentration was analysed. Interference by metals, such as lead and cadmium, was considered. Calibration plots were obtained in the micromolar and submicromolar concentration ranges, allowing the electrochemical determination of methylmercury in trace amounts. An estuarine water sample was analysed using the new method with a glassy carbon microelectrode.

Voltammetric studies on the electrochemical determination of methylmercury in chloride medium at carbon microelectrodes

International Nuclear Information System (INIS)

Ribeiro, F.; Neto, M.M.M.; Rocha, M.M.; Fonseca, I.T.E.

2006-01-01

Electroanalytical techniques have been used to determine methylmercury at low levels in environmental matrices. The electrochemical behaviour of methylmercury at carbon microelectrodes in a hydrochloric acid medium using cyclic, square wave and fast-scan linear-sweep voltammetric techniques has been investigated. The analytical utility of the methylmercury reoxidation peak has been explored, but the recorded peak currents were found to be poorly reproducible. This is ascribed to two factors: the adsorption of insoluble chloromercury compounds on the electrode surface, which appears to be an important contribution to hinder the voltammetric signal of methylmercury; and the competition between the reoxidation of the methylmercury radical and its dimerization reaction, which limits the reproducibility of the methylmercury peak. These problems were successfully overcome by adopting the appropriate experimental conditions. Fast-scan rates were employed and an efficient electrochemical regeneration procedure of the electrode surface was achieved, under potentiostatic conditions in a mercury-free solution containing potassium thiocyanate-a strong complexing agent. The influence of chloride ion concentration was analysed. Interference by metals, such as lead and cadmium, was considered. Calibration plots were obtained in the micromolar and submicromolar concentration ranges, allowing the electrochemical determination of methylmercury in trace amounts. An estuarine water sample was analysed using the new method with a glassy carbon microelectrode

A simple, rapid and green method based on pulsed potentiostatic electrodeposition of reduced graphene oxide on glass carbon electrode for sensitive voltammetric detection of sophoridine

International Nuclear Information System (INIS)

Wang, Fei; Wu, Yanju; Lu, Kui; Gao, Lin; Ye, Baoxian

2014-01-01

Graphical abstract: A simple, rapid and green method, based on graphene nanosheets directly deposited onto a glassy carbon electrode by pulsed potentiostatic reduction of a graphene oxide colloidal solution, to build sensitive voltammetric sensor for the determination of sophoridine was presented. - Highlights: • A simple, rapid and green method to build sensitive voltammetric sensor was presented. • The proposed sensor has a high electrochemical sensitivity for determination of sophoridine. • The proposed sensor exhibited an excellent selectivity. - Abstract: A simple, rapid and green method was described for sensitive voltammetric detection of sophoridine based on graphene nanosheets directly deposited onto a glassy carbon electrode (GCE) by pulsed potentiostatic reduction of a graphene oxide (GO) colloidal solution. The resulting electrodes (PP-ERGO/GCE) were characterized by electrochemical methods and scanning electron microscopy. Moreover, the electrochemical behaviors of sophoridine at the modified electrode were investigated in detail by cyclic voltammetry (CV), chronoamperometry (CA) and chronocoulometry (CC). Compared with the bare GCE and the preparation of reduced graphene oxide (RGO) films by potentiostatic method (PM) modified GCE, PP-ERGO/GCE could intensively enhance the oxidation peak currents and decrease the overpotential of sophoridine. Under the selected conditions, the modified electrode showed a linear voltammetric response to sophoridine within the concentration range of 8.0 × 10 −7 ∼ 1.0 × 10 −4 mol L −11 , with the detection limit of 2.0 × 10 −7 mol L −1 . And, the method was also applied to detect sophoridine in spiked human urine with wonderful satisfactory

Adsorptive stripping voltammetric determination of uranium with cephradine

International Nuclear Information System (INIS)

Ali, A.M.M.; Ghandour, M.A.; Khodari, M.

1995-01-01

Uranium adsorbed with cephradine is reduced on a hanging mercury drop electrode. This property was exploited in developing a highly sensitive stripping voltammetric procedure for the determination of uranium. A detection limit 2 x 10 -9 mol I -1 (0.5 μg I -1 ) of uranium ion is obtained with an 180 s accumulation time. Cyclic voltammetry was used to characterize the interfacial and redox behaviour. The effects of various parameters are discussed. Experimental conditions include the use of 5 x 10 -6 mol I -1 cephradine in 0.05 mol I -1 sodium perchlorate (pH ''approx ='' 6.5), an accumulation potential of 0.0 V versus SCE and a direct current stripping technique. The response is linear up to 5 x 10 -6 mol I -1 uranium and the relative standard deviation at 1 x 10 -7 mol I -1 ) UO 2+ is 4.4%. The effect of other metal ions was investigated. (author)

Cyclic Voltammetric Investigation of Dopamine at Poly-(Gabapentin Modified Carbon Paste Electrode

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M. T. Shreenivas

2011-01-01

Full Text Available The poly (gabapentin film was prepared on the surface of carbon paste electrode by electrochemical method using cyclic voltammetric technique. The poly (gabapentin film-modified carbon paste electrode was calibrated with standard potassium ferrocyanide solution in 1 M KCl as a supporting electrolyte. The prepared poly (gabapentin film-coated electrode exhibits excellent electrocatalytic activity towards the detection of dopamine at physiological pH. The scan rate effect was found to be diffusion-controlled electrode process. The concentration effect of dopamine was studied, and the redox peak potentials of dopamine were dependant on pH.

Unique, Voltammetric Electrochemical Sensors for Organic Contaminants, with Excellent Discrimination, Based on Conducting Polymer-, Aptamer- and Other-Functionalized Sensing Electrodes, Phase I

Data.gov (United States)

National Aeronautics and Space Administration — In ongoing and recent prior work for the Army, this firm has developed a unique, patented technology for voltammetric electrochemical detection of toxic gases,...

Voltammetric enzyme sensor for urea using mercaptohydroquinone-modified gold electrode as the base transducer.

Science.gov (United States)

Mizutani, F; Yabuki, S; Sato, Y

1997-01-01

A voltammetric urea-sensing electrode was prepared by combining a lipid-attached urease layer with a 2,5-dihydroxythiophenol-modified gold electrode. A self-assembled monolayer of dihydroxythiophenol was prepared on the gold surface by soaking the electrode into an ethanolic solution containing the modifier. A layer of the lipid-attached enzyme and that of acetyl cellulose overcoat were successively made on the dihydroxythiophenol-modified electrode by applying a dip-coating procedure. The addition of urea in a test solution (10 mM phosphate buffer, pH 7.0) brought about an increase of pH near the urease layer. The pH shift accompanied a negative shift of the anodic peak, which corresponded to the electro-oxidation of dihydroxyphenol moiety to form quinone, on the linear sweep voltammograms for the urease/dihydroxythiophenol electrode. The concentration of urea (0.2-5 mM) could be determined by measuring the electrode current at -0.05 V versus Ag/AgCl from the voltammogram. The electrode was applied to the determination of urea in human urine; the measurement of electrode current at such a low potential provided the urea determination without any electrochemical interference from L-ascorbic acid and uric acid.

Extraction or adsorption? Voltammetric assessment of protamine transfer at ionophore-based polymeric membranes.

Science.gov (United States)

Garada, Mohammed B; Kabagambe, Benjamin; Amemiya, Shigeru

2015-01-01

Cation-exchange extraction of polypeptide protamine from water into an ionophore-based polymeric membrane has been hypothesized as the origin of a potentiometric sensor response to this important heparin antidote. Here, we apply ion-transfer voltammetry not only to confirm protamine extraction into ionophore-doped polymeric membranes but also to reveal protamine adsorption at the membrane/water interface. Protamine adsorption is thermodynamically more favorable than protamine extraction as shown by cyclic voltammetry at plasticized poly(vinyl chloride) membranes containing dinonylnaphthalenesulfonate as a protamine-selective ionophore. Reversible adsorption of protamine at low concentrations down to 0.038 μg/mL is demonstrated by stripping voltammetry. Adsorptive preconcentration of protamine at the membrane/water interface is quantitatively modeled by using the Frumkin adsorption isotherm. We apply this model to ensure that stripping voltammograms are based on desorption of all protamine molecules that are transferred across the interface during a preconcentration step. In comparison to adsorption, voltammetric extraction of protamine requires ∼0.2 V more negative potentials, where a potentiometric super-Nernstian response to protamine is also observed. This agreement confirms that the potentiometric protamine response is based on protamine extraction. The voltammetrically reversible protamine extraction results in an apparently irreversible potentiometric response to protamine because back-extraction of protamine from the membrane extremely slows down at the mixed potential based on cation-exchange extraction of protamine. Significantly, this study demonstrates the advantages of ion-transfer voltammetry over potentiometry to quantitatively and mechanistically assess protamine transfer at ionophore-based polymeric membranes as foundation for reversible, selective, and sensitive detection of protamine.

Differential pulse voltammetric determination of salbutamol sulfate in syrup pharmaceutical formulation using poly(4-amino-3-hydroxynaphthalene sulfonic acid modified glassy carbon electrode

Directory of Open Access Journals (Sweden)

Meareg Amare

2017-10-01

Full Text Available A new method for determination of salbutamol sulfate has been developed using poly(4-amino-3-hydroxynaphthalene sulfonic acid/GCE. Cyclic voltammetric investigation of the electrochemical behavior of salbutamol sulfate at the polymer modified glassy carbon unveiled electrocatalytic activity of the modifier towards irreversible oxidation of salbutamol sulfate. Dependence of peak current predominantly on scan rate than on square root of scan rate, and peak potential shift with pH demonstrated that oxidation of salbutamol sulfate at the polymer modified electrode follows adsorption reaction kinetics with proton participation.Under optimized solution and differential pulse voltammetric parameters, the oxidative peak current showed linear dependence on salbutamol sulfate concentration in the range 0.2 to 8 μM with method detection limit (3s/m and determination coefficient (R2 of 6.8 × 10−8 M and 0.99786, respectively. Low method detection limit, relatively wide linear range, and recovery results of spiked standard salbutamol sulfate in syrup samples in the range 96.7–98.9% validated the method for determination of salbutamol sulfate in pharmaceutical formulations.Differential pulse voltammetric analysis of salbutamol sulfate syrup formulation for its salbutamol sulfate content revealed 98.8 to 99.3% of the labeled value confirming the applicability of the developed method for determination of salbutamol sulfate in real samples. Keywords: Electrochemistry, Analytical chemistry

Emerging approach for analytical characterization and geographical classification of Moroccan and French honeys by means of a voltammetric electronic tongue.

Science.gov (United States)

El Alami El Hassani, Nadia; Tahri, Khalid; Llobet, Eduard; Bouchikhi, Benachir; Errachid, Abdelhamid; Zine, Nadia; El Bari, Nezha

2018-03-15

Moroccan and French honeys from different geographical areas were classified and characterized by applying a voltammetric electronic tongue (VE-tongue) coupled to analytical methods. The studied parameters include color intensity, free lactonic and total acidity, proteins, phenols, hydroxymethylfurfural content (HMF), sucrose, reducing and total sugars. The geographical classification of different honeys was developed through three-pattern recognition techniques: principal component analysis (PCA), support vector machines (SVMs) and hierarchical cluster analysis (HCA). Honey characterization was achieved by partial least squares modeling (PLS). All the PLS models developed were able to accurately estimate the correct values of the parameters analyzed using as input the voltammetric experimental data (i.e. r>0.9). This confirms the potential ability of the VE-tongue for performing a rapid characterization of honeys via PLS in which an uncomplicated, cost-effective sample preparation process that does not require the use of additional chemicals is implemented. Copyright © 2017 Elsevier Ltd. All rights reserved.

Manganese dioxide-graphene nanocomposite film modified electrode as a sensitive voltammetric sensor of indomethacin detection

Energy Technology Data Exchange (ETDEWEB)

Liu, Yuxia; Zhang, Zhenfa; Zhang, Cuizong; Huang, Wei; Liang, Caiyun; Peng, Jinyun [Guangxi Normal University for Nationalities, Chongzuo (China)

2016-08-15

Excess amount of analgesic and anti-inflammatory drug, such as indomethacin, often leads to serious gastrointestinal complications; therefore, amount of such active compound should be regulated in commercial drugs. This study proposes an efficient analytical technique to detect indomethacin selectively. We prepared and investigated electrochemical properties of a manganese dioxide-graphene nanocomposite film modified glassy carbon electrode (MnO{sub 2}-Gr/GCE). The behavior of the modified electrode as electrocatalyst towards indomethacin oxidation was also examined. The cyclic voltammetric results reveal that the electrocatalytic activity for the oxidation of indomethacin can significantly be enhanced on the MnO{sub 2}-Gr/GCE. Indomethacin exhibited a sensitive anodic peak at about 0.90 V at MnO{sub 2}-Gr/GCE. The data obtained from differential pulse voltammetry showed that the anodic peak currents were linearly dependent on the indomethacin concentrations in the range of 1.0 X 10{sup -7} to 2.5 X 10{sup -5} mol/L with a detection limit of 3.2 X 10{sup -8} mol/L (S/N = 3). Most importantly, the proposed method shows efficient and selective sensing of indomethacin in commercial harmaceutical formulations. This is the first report of a voltammetric sensor for indomethacin using MnO{sub 2}-Gr/GCE. We believe that this new method can be commercialized for routine applications in laboratories.

Direct voltammetric determination of redox-active iron in carbon nanotubes.

Science.gov (United States)

Teo, Wei Zhe; Pumera, Martin

2014-12-01

With the advances in nanotechnology over the past decade, consumer products are increasingly being incorporated with carbon nanotubes (CNTs). As the harmful effects of CNTs are suggested to be primarily due to the bioavailable amounts of metallic impurities, it is vital to detect and quantify these species using sensitive and facile methods. Therefore, in this study, we investigated the possibility of quantifying the amount of redox-available iron-containing impurities in CNTs with voltammetric techniques such as cyclic voltammetry. We examined the electrochemistry of Fe3 O4 nanoparticles in phosphate buffer solution and discovered that its electrochemical behavior could be affected by pH of the electrolyte. By utilizing the unique redox reaction between the iron and phosphate species, the redox available iron content in CNTs was determined successfully using voltammetry. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Characterization of electrochemiluminescence of tris(2,2'-bipyridine)ruthenium(II) with glyphosate as coreactant in aqueous solution

International Nuclear Information System (INIS)

Jin, Jiye; Takahashi, Fumiki; Kaneko, Tsutomu; Nakamura, Toshio

2010-01-01

Glyphosate, a phosphorus-containing amino acid type herbicide was used as a coreactant for studying of electrochemiluminescence (ECL) reaction of tris(2,2'-bipyridyl)ruthenium(II) [Ru(bpy) 3 2+ ] in an aqueous solution. In a phosphate buffer solution of pH 8, glyphosate itself was known to be electrochemically inactive at glassy carbon electrode, however, it participated in a homogeneous chemical reaction with the electrogenerated Ru(bpy) 3 3+ , and resulted in producing Ru(bpy) 3 2+ species at the electrode surface. Kinetic and mechanistic information for the catalysis of glyphosate oxidation were evaluated by the steady-state voltammetric measurement with an ultramicroelectrode. The simulated cyclic voltammogram based on this mechanism was in good agreement with that obtained experimentally. ECL reaction of Ru(bpy) 3 2+ /glyphosate system was found to be strongly dependent on the media pH. In a pH region of 5-9, an ECL wave appeared at ca. +1.1 V vs. Ag/AgCl, which was caused by the generation of *Ru(bpy) 3 2+ via a Ru(bpy) 3 3+ -mediated oxidation of glyphosate. When pH >10, a second ECL wave was observed at ca. +1.35 V vs. Ag/AgCl, which was believed to be associated with a reaction between Ru(bpy) 3 3+ and the species from direct oxidation of GLYP at a GC electrode surface.

Sulfonated Polyaniline Coated Mercury Film Electrodes for Voltammetric Analysis of Metals in Water

Directory of Open Access Journals (Sweden)

Denise Alves Fungaro

2001-11-01

Full Text Available The electrochemical polymerization of 2-aminobenzenesulfonic acid with and without aniline has been carried by cyclic potencial sweep in sulfuric acid solution at the glassy carbon electrode. The polymer and copolymer formed have been characterized voltammetrically. The sulfonated polyaniline coated mercury thin-film electrodes have been evaluated for use with anodic stripping voltammetry. The electrodes were tested and compared with a conventional thin-film mercury electrode. Calibration plots showed linearity up to 10-7 mol L-1. Detection limits for zinc, lead and cadmium test species are very similar at around 12 nmol L-1. Applications to analysis of waters samples are demonstrated.

Direct voltammetric specific recognition of dopamine using AlIII-DA complexes at the hanging mercury drop electrode.

Science.gov (United States)

Zhang, Fuping; Zhang, Min; Cheng, Jiongjia; Yang, Li; Ji, Ming; Bi, Shuping

2007-11-01

In this paper, we firstly report the direct voltammetric recognition and determination of dopamine (DA) by using Al(III)-DA complexes at the hanging mercury drop electrode (HMDE). A new sensitive cathodic peak of Al(III)-DA can be detected at -900 mV (vs. SCE) in 0.1 M NH(4)Cl-NH(3).H(2)O-0.1 M KCl buffer solution at pH 8.5. This unique -900 mV cathodic peak arises from the specific interaction between Al(III) and DA on the HMDE, whereas other substances with similar structures, such as L-dopa, epinephrine (EP), norepinephrine (NE), catechols, caffeic acid (CA), trihydric phenols and tiron, do not yield any new peak on the voltammograms in the potential range from -100 to -1200 mV when Al(III) is added. The distinct voltammetric characteristic of the recognition of DA can effectively inhibit the interferences of both ascorbic acid and uric acid in the DA determination by the direct electrochemistry, which is a major difficulty when a solid electrode is used. The proposed method can be anticipated as an effective means for the recognition of DA in the elucidation of the mechanisms of Parkinson's disease (PD) and Alzheimer's disease (AD) in the presence of Al(III).

Voltammetric sensor for tartrazine determination in soft drinks using poly (p-aminobenzenesulfonic acid/zinc oxide nanoparticles in carbon paste electrode

Directory of Open Access Journals (Sweden)

Ghasem Karim-Nezhad

2017-04-01

Full Text Available Zinc oxide nanoparticles (ZnO NPs and p-aminobenzenesulfonic acid (p-ABSA were used to fabricate a modified electrode, as a highly sensitive and selective voltammetric sensor, for the determination of tartrazine. A fast and easy method for the fabrication of poly p-ABSA (Pp-ABSA/ZnO NPs-carbon paste electrode (Pp-ABSA/ZnO NPs-CPE by cyclic voltammetry was used. By combining the benefits of Pp-ABSA, ZnO NPs, and CPE, the resulted modified electrode exhibited outstanding electrocatalytic activity in terms of tartrazine oxidation by giving much higher peak currents than those obtained for the unmodified CPE and also other constructed electrodes. The effects of various experimental parameters on the voltammetric response of tartrazine were investigated. At the optimum conditions, the sensor has a linear response in the concentration range of 0349–5.44 μM, a good detection sensitivity (2.2034 μA/μM, and a detection limit of 80 nM of tartrazine. The proposed electrode was used for the determination of tartrazine in soft drinks with satisfactory results.

The redox behaviour of diazepam (Valium®) using a disposable screen-printed sensor and its determination in drinks using a novel adsorptive stripping voltammetric assay.

Science.gov (United States)

Honeychurch, Kevin C; Crew, Adrian; Northall, Hannah; Radbourne, Stuart; Davies, Owian; Newman, Sam; Hart, John P

2013-11-15

In this study we investigated the possibility of applying disposable electrochemical screen-printed carbon sensors for the rapid identification and quantitative determination of diazepam in beverages. This was achieved utilising a previously unreported oxidation peak. The origin of this peak was investigated further by cyclic voltammetry and gas chromatography/mass spectroscopy. At pH 6 the voltammetric behaviour of this oxidation process was found to involve adsorption of the drug allowing for the development of an adsorptive stripping voltammetric assay. Experimental conditions were then optimised for the determination of diazepam in a beverage sample using a medium exchange technique. It was shown that no elaborate extraction procedures were required as the calibration plots obtained in the absence and presence of the beverage were very similar. © 2013 Elsevier B.V. All rights reserved.

Thrombin-Binding Aptamer Quadruplex Formation: AFM and Voltammetric Characterization

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Victor Constantin Diculescu

2010-01-01

Full Text Available The adsorption and the redox behaviour of thrombin-binding aptamer (TBA and extended TBA (eTBA were studied using atomic force microscopy and voltammetry at highly oriented pyrolytic graphite and glassy carbon. The different adsorption patterns and degree of surface coverage were correlated with the sequence base composition, presence/absence of K+, and voltammetric behaviour of TBA and eTBA. In the presence of K+, only a few single-stranded sequences present adsorption, while the majority of the molecules forms stable and rigid quadruplexes with no adsorption. Both TBA and eTBA are oxidized and the only anodic peak corresponds to guanine oxidation. Upon addition of K+ ions, TBA and eTBA fold into a quadruplex, causing the decrease of guanine oxidation peak and occurrence of a new peak at a higher potential due to the oxidation of G-quartets. The higher oxidation potential of G-quartets is due to the greater difficulty of electron transfer from the inside of the quadruplex to the electrode surface than electron transfer from the more flexible single strands.

Electropolymerized supramolecular tetraruthenated porphyrins applied as a voltammetric sensor

Energy Technology Data Exchange (ETDEWEB)

Silva, Monize M. da; Ribeiro, Gabriel H.; Faria, Anizio M. de; Bogado, Andre L.; Dinelli, Luis R., E-mail: dinelli@pontal.ufu.br [Universidade Federal de Uberlandia (UFU), Ituiutaba, MG (Brazil). Faculdade de Ciencias Integradas do Pontal; Batista, Alzir A. [Universidade Federal de Sao Carlos (UFSCar), SP (Brazil). Departamento de Quimica

2013-11-15

Porphyrin 5,10,15,20-Tetra(4-pyridyl)manganese(III), [Mn-TPyP(H{sub 2}O){sub 2}]PF{sub 6}, and electropolymerized supramolecular porphyrins (ESP), {l_brace}Mn-TPyP(H{sub 2}O){sub 2}[RuCl{sub 3}(dppb)]{sub 4}{r_brace}PF{sub 6} (dppb = 1,4-bis(diphenylphosphine)butane), were synthesized and characterized. A thin solid film of ESP was obtained on a glass carbon electrode surface by a cyclic voltammetry method. The peak current increased with the number of voltammetric cycles, which shows a typical behavior of the species being adsorbed on the surface of the electrode. Cyclic voltammetry was also employed for acetaminophen quantification using an ESP modified electrode. The modified electrode shows a linear relationship between the anodic peak current and the concentration of acetaminophen (in the rage 0.05 to 0.7 mmol L{sup -1}. The performance of the modified electrode was verified by the determination of acetaminophen in a commercial pharmaceutical product and the results were in good agreement with those obtained by a control HPLC method. (author)

Voltammetric behavior of sedative drug midazolam at glassy carbon electrode in solubilized systems.

Science.gov (United States)

Jain, Rajeev; Yadav, Rajeev Kumar

2012-04-01

Redox behavior of midazolam was studied at a glassy carbon electrode in various buffer systems, supporting electrolytes and pH using differential pulse, square-wave and cyclic voltammetry. Based on its reduction behavior, a direct differential pulse voltammetric method has been developed and validated for the determination of midazolam in parenteral dosage. Three well-defined peaks were observed in 0.1% SLS, Britton-Robinson (BR) buffer of pH 2.5. The effect of surfactants like sodium lauryl sulfate (SLS), cetyl trimethyl ammonium bromide (CTAB) and Tween 20 was studied. Among these surfactants SLS showed significant enhancement in reduction peak. The cathodic peak currents were directly proportional to the concentration of midazolam with correlation coefficient of 0.99.

Voltammetric investigation of avidin-biotin complex formation using an electroactive bisbiotinyl compound

International Nuclear Information System (INIS)

Sugawara, Kazuharu; Shirotori, Tatsuya; Hirabayashi, George; Kamiya, Naoto; Kuramitz, Hideki; Tanaka, Shunitz

2004-01-01

Formation of avidin-biotin complex was investigated using bisbiotinyl thionine (BBT) by means of voltammetric techniques. Thionine is an electroactive compound and has two amino groups that are necessary for the reaction with a biotinylation reagent. The biotinylation of thionine produces a new reagent with two biotin moieties at each end of thionine. Three BBTs of different lengths of the spacer that connects the biotin moiety to the thionine moiety were prepared. The avidin-biotin binding assay was achieved by measuring the electrode response of the thionine moiety in BBT. The binding affinity and the conformation of complex, which depended on the length of spacer, are discussed. BBT in which the spacer is shortest (BBT-S, distance between carbonyl group of the two biotin moieties: 11 A) binds with only one avidin molecule. BBT with medium length of spacer (BBT-M, 28.8 A) forms the complex with two avidin molecules. BBT with the longest spacer (BBT-L, 46.6 A) allows binding with two avidin molecules as well as intramolecular binding within one avidin molecule. The affinity constants of BBT-S, BBT-M and BBT-L for avidin were estimated to be 7.0 x 10 12 M -1 , 3.2 x 10 12 M -1 and 4.0 x 10 12 M -1 , respectively

Voltammetric sensor for tartrazine determination in soft drinks using poly (p-aminobenzenesulfonic acid)/zinc oxide nanoparticles in carbon paste electrode.

Science.gov (United States)

Karim-Nezhad, Ghasem; Khorablou, Zeynab; Zamani, Maryam; Seyed Dorraji, Parisa; Alamgholiloo, Mahdieh

2017-04-01

Zinc oxide nanoparticles (ZnO NPs) and p-aminobenzenesulfonic acid (p-ABSA) were used to fabricate a modified electrode, as a highly sensitive and selective voltammetric sensor, for the determination of tartrazine. A fast and easy method for the fabrication of poly p-ABSA (Pp-ABSA)/ZnO NPs-carbon paste electrode (Pp-ABSA/ZnO NPs-CPE) by cyclic voltammetry was used. By combining the benefits of Pp-ABSA, ZnO NPs, and CPE, the resulted modified electrode exhibited outstanding electrocatalytic activity in terms of tartrazine oxidation by giving much higher peak currents than those obtained for the unmodified CPE and also other constructed electrodes. The effects of various experimental parameters on the voltammetric response of tartrazine were investigated. At the optimum conditions, the sensor has a linear response in the concentration range of 0349-5.44 μM, a good detection sensitivity (2.2034 μA/μM), and a detection limit of 80 nM of tartrazine. The proposed electrode was used for the determination of tartrazine in soft drinks with satisfactory results. Copyright © 2016. Published by Elsevier B.V.

Voltammetric behavior, biocidal effect and synthesis of some new nanomeric fused cyclic thiosemicarbazones and their mercuric(II salts

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M.S.T. Makki

2014-11-01

Full Text Available New nanomeric 3-thioxo-5-methoxy-4,5-dihydro-6-methyl-9-unsubstituted/substituted-1,2,4-triazino[5,6-b]indoles (2a–c and 3-thioxo-5-methoxy-4,5-dihydro-6,7-dihydroxy-1,2,4-triaino[5,6]-cyclobut-6-ene (3 were prepared via reaction of thiosemicarbazide with 5-unsubstitutedand/substituted-indol-2,3-diones and/or 3,4-dihydroxycyclobutane-1,2-dione in methanol–concentrated HCl at room temperature. A series of mercury(II–ligand salts e.g. compound 4b and Hg(II complexes 5a,b and 6 of cyclic Schiff base were prepared. Structures of these compounds were established by elemental analysis and spectral measurements. The redox characteristics of selected compounds were studied for use as chelating agents for stripping voltammetric determination of mercuric(II ions in aqueous media. The compounds were also screened for their use as molluscicidal agents against Biomophalaria Alexandrina Snails responsible for Bilhariziasis.

Voltammetric sensing of bisphenol A based on a single-walled carbon nanotubes/poly{3-butyl-1-[3-(N-pyrrolyl)propyl] imidazolium ionic liquid} composite film modified electrode

International Nuclear Information System (INIS)

Chen, Xuemin; Ren, Tongqing; Ma, Ming; Wang, Zhengguo; Zhan, Guoqing; Li, Chunya

2013-01-01

Highlights: • Single-walled carbon nanotubes (SWCNTs)-ionic liquid (IL) nanocomposite fabrication. • SWCNTs-Poly-IL film modified electrode was prepared and characterized. • Voltammetric behaviors of bisphenol A were investigated thoroughly. • Sensitive voltammetric method for bisphenol A determination was developed. -- Abstract: Using carboxylic acid-functionalized single walled carbon nanotubes (SWCNTs-COO − ) as an anion and 3-butyl-1-[3-(N-pyrrolyl)propyl]imidazolium as a cation, a novel SWCNTs-COO-ionic liquid (SWCNTs-COO-IL) nanocomposite was fabricated successfully. The as-prepared SWCNTs-COO-IL nanocomposite was confirmed with transmission electron microscopy, X-ray photoelectron spectroscopy, UV–vis, FTIR and Raman spectroscopy. The SWCNTs-COO-IL nanocomposite was coated onto a glassy carbon electrode surface followed by cyclic voltammetric scanning to fabricate a SWCNTs/poly{3-butyl-1-[3-(N-pyrrolyl)propyl] imidazolium ionic liquid} composite film modified electrode (SWCNTs/Poly-IL/GCE). Scanning electron microscope and electrochemical impedance spectroscopy were used to characterize SWCNTs/Poly-IL/GCE. Electrochemical behaviors of bisphenol A (BPA) at the SWCNTs/Poly-IL/GCE were investigated thoroughly. It was found that an obvious oxidation peak appeared without reduction peak in the reverse scanning, indicating an irreversible electrochemical process. The oxidation peak currents of BPA were linearly related to scan rate in the range of 20–300 mV s −1 , suggesting an adsorption controlled process rather than a diffusion controlled process. Differential pulse voltammetry was employed for the voltammetric sensing of BPA. Experimental conditions such as film thickness, pH value, accumulation potential and time that influence the analytical performance of the SWCNTs/Poly-IL/GCE were optimized. Under optimal conditions, the oxidation peak current was linearly related to BPA concentration in the range of 5.0 × 10 −9 to 3.0 × 10 −5 mol L

Characterization of electrochemiluminescence of tris(2,2'-bipyridine)ruthenium(II) with glyphosate as coreactant in aqueous solution

Energy Technology Data Exchange (ETDEWEB)

Jin, Jiye, E-mail: jin@shinshu-u.ac.j [Department of Chemistry, Faculty of Science, Shinshu University, 3-1-1 Asahi, Matsumoto, Nagano 390-8621 (Japan); Takahashi, Fumiki; Kaneko, Tsutomu; Nakamura, Toshio [Department of Chemistry, Faculty of Science, Shinshu University, 3-1-1 Asahi, Matsumoto, Nagano 390-8621 (Japan)

2010-08-01

Glyphosate, a phosphorus-containing amino acid type herbicide was used as a coreactant for studying of electrochemiluminescence (ECL) reaction of tris(2,2'-bipyridyl)ruthenium(II) [Ru(bpy){sub 3}{sup 2+}] in an aqueous solution. In a phosphate buffer solution of pH 8, glyphosate itself was known to be electrochemically inactive at glassy carbon electrode, however, it participated in a homogeneous chemical reaction with the electrogenerated Ru(bpy){sub 3}{sup 3+}, and resulted in producing Ru(bpy){sub 3}{sup 2+} species at the electrode surface. Kinetic and mechanistic information for the catalysis of glyphosate oxidation were evaluated by the steady-state voltammetric measurement with an ultramicroelectrode. The simulated cyclic voltammogram based on this mechanism was in good agreement with that obtained experimentally. ECL reaction of Ru(bpy){sub 3}{sup 2+}/glyphosate system was found to be strongly dependent on the media pH. In a pH region of 5-9, an ECL wave appeared at ca. +1.1 V vs. Ag/AgCl, which was caused by the generation of *Ru(bpy){sub 3}{sup 2+} via a Ru(bpy){sub 3}{sup 3+}-mediated oxidation of glyphosate. When pH >10, a second ECL wave was observed at ca. +1.35 V vs. Ag/AgCl, which was believed to be associated with a reaction between Ru(bpy){sub 3}{sup 3+} and the species from direct oxidation of GLYP at a GC electrode surface.

Penicillamine-modified sensor for the voltammetric determination of Cd(II) and Pb(II) ions in natural samples.

Science.gov (United States)

Pérez-Ràfols, Clara; Serrano, Núria; Díaz-Cruz, José Manuel; Ariño, Cristina; Esteban, Miquel

2015-11-01

A new penicillamine-GCE was developed based on the immobilization of d-penicillamine on aryl diazonium salt monolayers anchored to the glassy carbon electrode (GCE) surface and it was applied for the first time to the simultaneous determination of Cd(II) and Pb(II) ions by stripping voltammetric techniques. The detection and quantification limits at levels of µg L(-1) suggest that the penicillamine-GCE could be fully suitable for the determination of the considered ions in natural samples. Copyright © 2015 Elsevier B.V. All rights reserved.

Voltammetric behavior of sedative drug midazolam at glassy carbon electrode in solubilized systems

Directory of Open Access Journals (Sweden)

Rajeev Jain

2012-04-01

Full Text Available Redox behavior of midazolam was studied at a glassy carbon electrode in various buffer systems, supporting electrolytes and pH using differential pulse, square-wave and cyclic voltammetry. Based on its reduction behavior, a direct differential pulse voltammetric method has been developed and validated for the determination of midazolam in parenteral dosage. Three well-defined peaks were observed in 0.1% SLS, Britton–Robinson (BR buffer of pH 2.5. The effect of surfactants like sodium lauryl sulfate (SLS, cetyl trimethyl ammonium bromide (CTAB and Tween 20 was studied. Among these surfactants SLS showed significant enhancement in reduction peak. The cathodic peak currents were directly proportional to the concentration of midazolam with correlation coefficient of 0.99. Keywords: Midazolam, Voltammetry, Surfactant, Glassy carbon electrode, Parenteral dosage form

Adsorptive stripping voltammetric methods for determination of aripiprazole

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Derya Aşangil

2012-06-01

Full Text Available Anodic behavior of aripiprazole (ARP was studied using electrochemical methods. Charge transfer, diffusion and surface coverage coefficients of adsorbed molecules and the number of electrons transferred in electrode mechanisms were calculated for quasi-reversible and adsorption-controlled electrochemical oxidation of ARP at 1.15 V versus Ag/AgCl at pH 4.0 in Britton–Robinson buffer (BR on glassy carbon electrode. Voltammetric methods for direct determination of ARP in pharmaceutical dosage forms and biological samples were developed. Linearity range is found as from 11.4 μM (5.11 mg/L to 157 μM (70.41 mg/L without stripping mode and it is found as from 0.221 μM (0.10 mg/L to 13.6 μM (6.10 mg/L with stripping mode. Limit of detection (LOD was found to be 0.11 μM (0.05 mg/L in stripping voltammetry. Methods were successfully applied to assay the drug in tablets, human serum and human urine with good recoveries between 95.0% and 104.6% with relative standard deviation less than 10%. Keywords: Adsorptive stripping voltammetry, Aripiprazole, Electrochemical behavior, Human serum and urine, Pharmaceuticals

Rapid screening and guided extraction of antioxidants from microalgae using voltammetric methods.

Science.gov (United States)

Goiris, Koen; De Vreese, Peter; De Cooman, Luc; Muylaert, Koenraad

2012-08-01

Currently, microalgae draw much attention as a promising source of natural antioxidants to replace synthetic antioxidants for food applications. In this paper, the use of voltammetric techniques as a fast alternative for chemical assays to determine the antioxidant power of microalgal biomass is discussed. It was found that antioxidant activities determined by square wave voltammetry correlate well with the results from other established antioxidant assays, such as Trolox equivalent antioxidant capacity (R(2) = 0.737), ferric reducing antioxidant potential (R(2) = 0.729), and AAPH-induced oxidation of linoleic acid (R(2) = 0.566). Besides yielding quantitative data on the antioxidant activity, square wave voltammetry provides additional information on the antioxidant profile of microalgal biomass as the peak potentials of antioxidant components are determined. Consequently, square wave voltammetry can be used as a tool for optimizing the extraction processes to recover antioxidant components from microalgae.

Optimisation of the conditions for stripping voltammetric analysis at liquid-liquid interfaces supported at micropore arrays: a computational simulation.

Science.gov (United States)

Strutwolf, Jörg; Arrigan, Damien W M

2010-10-01

Micropore membranes have been used to form arrays of microinterfaces between immiscible electrolyte solutions (µITIES) as a basis for the sensing of non-redox-active ions. Implementation of stripping voltammetry as a sensing method at these arrays of µITIES was applied recently to detect drugs and biomolecules at low concentrations. The present study uses computational simulation to investigate the optimum conditions for stripping voltammetric sensing at the µITIES array. In this scenario, the diffusion of ions in both the aqueous and the organic phases contributes to the sensing response. The influence of the preconcentration time, the micropore aspect ratio, the location of the microinterface within the pore, the ratio of the diffusion coefficients of the analyte ion in the organic and aqueous phases, and the pore wall angle were investigated. The simulations reveal that the accessibility of the microinterfaces during the preconcentration period should not be hampered by a recessed interface and that diffusional transport in the phase where the analyte ions are preconcentrated should be minimized. This will ensure that the ions are accumulated within the micropores close to the interface and thus be readily available for back transfer during the stripping process. On the basis of the results, an optimal combination of the examined parameters is proposed, which together improve the stripping voltammetric signal and provide an improvement in the detection limit.

Influence of the acidity level change in aprotic media on the voltammetric behavior of nitrogabacinamamides

International Nuclear Information System (INIS)

Bautista-Martinez, J.A.; Gonzalez, I.; Aguilar-Martinez, M.

2004-01-01

This work presents a comparative voltammetric study of o-, m- and p-nitrogabacinamamides (N-[3(X-nitrophenyl)-(2E)-propenyl]-4-aminobutanoic acids), NG, in acetonitrile. These compounds, a HDR-NO 2 nitro compounds type, display three reduction waves, two of them are waves similar to those appearing in the reduction of the nitro compounds lacking a proton donor group and one new wave at less negative potentials, associated with the nitro-to-hydroxylamine reduction through a self-protonation reaction. Experiments were carried out in the presence of different chemical species giving an acidity level control by homogeneous buffer systems. The presence of tetraethylammonium phenolate achieves complete inhibition of self-protonation reactions, thus recovering the behavior established by ( - DR-NO 2 / - DR-NO 2 · - ) system. When the conjugated acid of the above mentioned base is added to the acetonitrile solution, where the acidity level was controlled by the phenol/phenolate system (acidity level buffer), only the second electroreduction wave ( - DR-NO 2 · - /HDR-NHOH) shows to be affected by the presence of phenol in the electrolytic medium and displaces towards less negative potential values. On the other hand, in the benzoic acid (HBz)/benzoate (Bz - ) medium, the electrochemical behavior of these nitro compounds changes completely passing from ( - DR-NO 2 / - DR-NO 2 · - ) system to (HDR-NO 2 + 4HBz/HDR-NHOH + 4Bz - ) type system, in which both the stoichiometry of the electroreduction process and the energetic requirement for its realization are changed. The comparison of the different voltammetric behavior in the presence of the different acidic and basic additives allowed constructing an acidity level scale where the different acid base couples of the intermediaries of the NG electroreduction were placed. This kind of scale allows choosing the chemical conditions necessaries to drive the pathway of the electrochemical transformation of nitro compounds

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

Energy Technology Data Exchange (ETDEWEB)

Dorraji, Parisa S.; Jalali, Fahimeh, E-mail: fjalali@razi.ac.ir

2016-04-01

An electrochemical sensor for the sensitive detection of acyclovir was developed by the electropolymerization of Eriochrome black T at a pretreated glassy carbon electrode. The surface morphology of the modified electrode was characterized by field emission scanning electron microscopy. Under the optimized conditions, a significant electrochemical improvement was observed toward the electrooxidation of acyclovir on the modified electrode surface relative to the unmodified electrode. The detection limit of 12 nM and two linear calibration ranges of 0.03–0.3 μM and 0.3–1.5 μM were obtained for acyclovir determination using a differential pulse voltammetric method in acetate buffer (0.1 M, pH 4.0). Real sample studies were carried out in human blood serum and pharmaceutical formulations, which offered good recovery (98–102%). The electrode showed excellent reproducibility, selectivity and antifouling effects. - Graphical abstract: Eriochrome black T (EBT) was electropolymerized at the surface of a pretreated glassy carbon electrode. The modified electrode enhanced the oxidation current of acyclovir, significantly. The sensor was used in the determination of acyclovir in human blood serum samples and pharmaceutical dosages. - Highlights: • Construction of a voltammetric sensor for acyclovir is described. • Eriochrome black T was electropolymerized at the electrode surface. • The sensor improved the sensitivity of the electrode for monitoring acyclovir. • The recoveries and standard deviations were acceptable in spiked human blood serum. • The proposed sensor had good lifetime to be used in biological matrices.

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

International Nuclear Information System (INIS)

Dorraji, Parisa S.; Jalali, Fahimeh

2016-01-01

An electrochemical sensor for the sensitive detection of acyclovir was developed by the electropolymerization of Eriochrome black T at a pretreated glassy carbon electrode. The surface morphology of the modified electrode was characterized by field emission scanning electron microscopy. Under the optimized conditions, a significant electrochemical improvement was observed toward the electrooxidation of acyclovir on the modified electrode surface relative to the unmodified electrode. The detection limit of 12 nM and two linear calibration ranges of 0.03–0.3 μM and 0.3–1.5 μM were obtained for acyclovir determination using a differential pulse voltammetric method in acetate buffer (0.1 M, pH 4.0). Real sample studies were carried out in human blood serum and pharmaceutical formulations, which offered good recovery (98–102%). The electrode showed excellent reproducibility, selectivity and antifouling effects. - Graphical abstract: Eriochrome black T (EBT) was electropolymerized at the surface of a pretreated glassy carbon electrode. The modified electrode enhanced the oxidation current of acyclovir, significantly. The sensor was used in the determination of acyclovir in human blood serum samples and pharmaceutical dosages. - Highlights: • Construction of a voltammetric sensor for acyclovir is described. • Eriochrome black T was electropolymerized at the electrode surface. • The sensor improved the sensitivity of the electrode for monitoring acyclovir. • The recoveries and standard deviations were acceptable in spiked human blood serum. • The proposed sensor had good lifetime to be used in biological matrices.

Study and Elimination of the Interference of Aluminium on the Voltammetric Determination of Uranium with Chloranilic Acid. Application to the Determination of Uranium in Waters and Geological Samples

International Nuclear Information System (INIS)

Fernandez, C.; Sanchez, M.; Ballesteros, O.; Fernandez, M.; Clavero, M. A.; Gonzalez, A. M.

2000-01-01

The interference of aluminium during the voltammetric determination of uranium with 2,5-dichloro-3,6-dihydroxy-1,4-benzoquinone (chloranilic acid) has been investigated. The presence of aluminium originates a voltammetric signal due to its chloranilic acid complex at the same potential range as the uranium analytical signal appears. The interference of aluminium can be overcome by addition of an appropriate amount of sodium fluoride as complexing reagent. The determination of uranium by adsorptive stripping voltammetry (AdSV) can be carried out at concentration levels as low as 1 μg/L in the presence of 100 μg/L aluminium after the addition of 100μL of 0.1 mol/L NaF. The method can be applied to the determination of uranium in aluminium-containing waters and geological samples containing high aluminium levels. (Author) 19 refs

Voltammetric sensor for caffeine based on a glassy carbon electrode modified with Nafion and graphene oxide

International Nuclear Information System (INIS)

Zhao, F.; Wang, F.; Zhao, W.; Zhou, J.; Liu, Y.; Zou, L.; Ye, B.

2011-01-01

We report on a voltammetric sensor for caffeine that is based on a glassy carbon electrode modified with Nafion and graphene oxide (GO). It exhibits a good affinity for caffeine (resulting from the presence of Nafion), and excellent electrochemical response (resulting from the pressence of GO) for the oxidation of caffeine. The electrode enables the determination of caffeine in the range from 4.0 x 10 -7 to 8.0 x 10 -5 mol L -1 , with a detection limit of 2.0 x 10 -7 mol L -1 . The sensor displays good stability, reproducibility, and high sensitivity. It was successfully applied to the quantitative determination of caffeine in beverages. (author)

Square Wave Voltammetric Determination of 2-Thiouracil in Pharmaceuticals and Real Samples Using Glassy Carbon Electrode

OpenAIRE

Naveen M. Gokavi; Vijay P. Pattar; Atmanand M. Bagoji; Sharanappa T. Nandibewoor

2013-01-01

A simple and rapid method was developed using cyclic and square wave voltammetric techniques for the determination of trace-level sulfur containing compound, 2-thiouracil, at a glassy carbon electrode. 2-thiouracil produced two anodic peaks at 0.334 V and 1.421 V and a cathodic peak at −0.534 V. The square wave voltammetry of 2-thiouracil gave a good linear response in the range of 1–20 μM with a detection limit of 0.16 μM and quantification limit of 0.53 μM (0.0679 μg/g), which is in good ag...

Electrochemical behavior and voltammetric determination of vanillin based on an acetylene black paste electrode modified with graphene-polyvinylpyrrolidone composite film.

Science.gov (United States)

Deng, Peihong; Xu, Zhifeng; Zeng, Rongying; Ding, Chunxia

2015-08-01

The graphene-polyvinylpyrrolidone composite film modified acetylene black paste electrode (GR-PVP/ABPE) was fabricated and used to determine vanillin. In 0.1M H3PO4 solution, the oxidation peak current of vanillin increased significantly at GR-PVP/ABPE compared with bare ABPE, PVP/ABPE and GR/ABPE. The oxidation mechanism was discussed. The experimental conditions that exert influence on the voltammetric determination of vanillin, such as supporting electrolytes, pH values, accumulation potential and accumulation time, were optimized. Besides, the interference, repeatability, reproducibility and stability measurements were also evaluated. Under the optimal experimental conditions, the oxidation peak current was proportional to vanillin concentration in the range of 0.02-2.0 μM, 2.0-40 μM and 40-100 μM. The detection limit was 10nM. This sensor was used successfully for vanillin determination in various food samples. Copyright © 2015 Elsevier Ltd. All rights reserved.

Online Monitoring of Copper Damascene Electroplating Bath by Voltammetry: Selection of Variables for Multiblock and Hierarchical Chemometric Analysis of Voltammetric Data

Directory of Open Access Journals (Sweden)

Aleksander Jaworski

2017-01-01

Full Text Available The Real Time Analyzer (RTA utilizing DC- and AC-voltammetric techniques is an in situ, online monitoring system that provides a complete chemical analysis of different electrochemical deposition solutions. The RTA employs multivariate calibration when predicting concentration parameters from a multivariate data set. Although the hierarchical and multiblock Principal Component Regression- (PCR- and Partial Least Squares- (PLS- based methods can handle data sets even when the number of variables significantly exceeds the number of samples, it can be advantageous to reduce the number of variables to obtain improvement of the model predictions and better interpretation. This presentation focuses on the introduction of a multistep, rigorous method of data-selection-based Least Squares Regression, Simple Modeling of Class Analogy modeling power, and, as a novel application in electroanalysis, Uninformative Variable Elimination by PLS and by PCR, Variable Importance in the Projection coupled with PLS, Interval PLS, Interval PCR, and Moving Window PLS. Selection criteria of the optimum decomposition technique for the specific data are also demonstrated. The chief goal of this paper is to introduce to the community of electroanalytical chemists numerous variable selection methods which are well established in spectroscopy and can be successfully applied to voltammetric data analysis.

Nafion Coated Electrodes as Voltammetric Sensors for Iron Analysis in Sediments and Pore Waters: an Example from the Lagoon of Venice

Directory of Open Access Journals (Sweden)

Emanuele Argese

2001-09-01

Full Text Available Glassy carbon electrodes coated with Nafion are used for the ion-exchange voltammetric (IEV determination of Fe(II in the pore-waters and acidic extracts of sediments of the lagoon of Venice (Italy. The coated electrodes give reversible voltammetric signals, well resolved from background currents, which can be used for quantitative determinations. The yield of iron extracted by HCl from the sediment depends on the experimental conditions, in particular on the concentration of hydrochloric acid. By combining IEV on the acid extract with trapping and analysis of gaseous H2S evolved it is possible to obtain quantitative information both on the total content of iron dissolved by the acid attack and on the fraction of iron present in the form of acid volatile sulphides (AVS. As far as pore-waters are concerned, in this kind of samples the IEV determination of iron can be performed simply after dilution with HCl. The pore-waters here examined were sampled without alteration of their equilibrium conditions by using a suitable “in situ” sampler. IEV data obtained in samples from the lagoon of Venice (Italy show satisfactory correlation with previous results obtained using different analytical techniques.

Electrochemistry of cefditoren pivoxil and its voltammetric determination

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İbrahim Hüdai Taşdemir

2016-01-01

Full Text Available Electrochemical behavior of cefditoren pivoxil (CTP was studied via experimental electrochemical methods and theoretical calculations performed at B3LYP/6-31+G(d//AM1 level. Experimental studies were carried out based on an irreversible 4e−/4H+ reduction peak at ca. −0.8 V on hanging mercury drop electrode (HMDE and irreversible 1e−/1H+ oxidation of CTP at ca. 0.8 V on glassy carbon electrode (GCE versus Ag/AgCl, KCl (3.0 M in Britton–Robinson buffer at pH 6.0 and 4.0, respectively. Tentative reduction and oxidation mechanisms were proposed based on computational and experimental results. Square-wave adsorptive stripping voltammetric methods have been developed and validated for quantification of CTP in different samples. Linear working range was established as 0.15–15.0 μM for HMDE and 1.0–50.0 μM for GCE. Limit of quantification (S/N = 10 was calculated to be (0.10 ± 0.02 μM and (0.80 ± 0.03 μM for HMDE and GCE, respectively. Methods were successfully applied to assay the drug in tablets and human serum with good recoveries between (99.2 ± 11.6 % and (102.5 ± 9.5 % having relative standard deviation less than 10%.

Modification of glassy carbon electrode with poly(hydroxynaphthol blue)/multi-walled carbon nanotubes composite and construction a new voltammetric sensor for the simultaneous determination of hydroquinone, catechol, and resorcinol

Science.gov (United States)

Daneshinejad, Hassan; Arab Chamjangali, Mansour; Goudarzi, Nasser; Hossain Amin, Amir

2018-03-01

A novel voltammetric sensor is developed based on a poly(hydroxynaphthol blue)/multi-walled carbon nanotubes-modified glassy carbon electrode for the simultaneous determination of the dihydroxybenzene isomers hydroquinone (HQ), catechol (CC), and resorcinol (RS). The preparation and basic electrochemical performance of the sensor are investigated in details. The electrochemical behavior of the dihydroxybenzene isomers at the sensor is studied by the cyclic and differential pulse voltammetric techniques. The results obtained show that this new electrochemical sensor exhibits an excellent electro-catalytic activity towards oxidation of the three isomers. The mechanism of this electro-catalytic activity is discussed. Using the optimum parameters, limit of detection obtained 0.24, 0.24, and 0.26 μmol L-1 for HQ, CC, and RS, respectively. The modified electrode is also successfully applied to the simultaneous determination of dihydroxybenzene in water samples.

Cyclic Voltammetric Study of Complexes of Fe (III) with Saponins Isolated from Cicer aritinum and Glycyrrhizin

International Nuclear Information System (INIS)

Khan, S.S.; Kazmi, S.A.; Anwar, H

2013-01-01

Cyclic voltammetric study was used to analyze three new saponins (isolated from the seeds of Cicer aritinum) along with a known saponin soyasaponin I and beta sitosterol glycoside isolated saponins as well as glycyrrhizin. These studies were carried out in aqueous medium at Glassy carbon (GCE) electrode vs. AgCl reference electrode. Results revealed that the voltammograms of Fe(III) with isolated saponins are irreversible while that of Fe(III)-glycyrrhizin complex is reversible. Even though precise Eo values of their Fe(III) complex could not be determined, it is clearly indicated that Fe(III) forms complexes with these saponins. The ability to form strong complexes with Fe(III) therefore reduces the availability of Fe(III) by saponins. (author)

Determinação voltamétrica do herbicida glifosato em águas naturais utilizando eletrodo de cobre Voltammetric determination of glyphosate in natural waters with a copper electrode

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Andresa Fabiana Garcia

2007-01-01

Full Text Available The aim of this work was to investigate the copper electrode behavior in the voltammetric determination of glyphosate. The best conditions for this determination are phosphate buffer 0.05 mol L-1 and pH 7.3, and the peak potential is observed at 187 mV. LD and LQ values are 59 µg L-1 e 196 µg L-1, respectively. A water sample was analysed for glyphosate and identical results were obtained by using the analytical curve and the standard addition method. The comparison with a voltammetric method with Hg electrode, after a reaction with nitrite, showed quite concordant results for the analysis of the surface water sample. Therefore, the proposed method can be applied to direct determinations of the herbicide in waters, decreasing the time of analysis; besides, the method is in agreement with the "green chemistry" concept.

Electrochemistry of Pt (100) in alkaline media: A voltammetric study

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van der Vliet, Dennis F.; Koper, Marc T. M.

2010-10-01

Pt (100) is one of the fcc metal surface planes that reconstruct upon annealing at high temperatures. The state of the surface is important in electrochemistry, in order to correlate catalytic behavior with surface structure. Therefore, the behavior of single crystalline Pt (100) in alkaline media was investigated, with particular attention paid to surface long-range order. It was found that, in line with previous results, the manner of cooling the crystal after annealing influenced the state of surface significantly, with a profound effect on blank cyclic voltammetry as well as on carbon monoxide oxidation. Different ratios of inert and reductive gases were used to see if an optimal mixture could be obtained. Using air, argon, hydrogen, CO, and combinations of these gases gave rise to different states of the surface, with clear observable differences in blank voltammetric behavior and CO stripping. Also, the effect of alkali-metal cations and bromide on the blank and CO stripping voltammetry was investigated. Our main conclusion is that cooling in a carbon monoxide containing gas gives a clean, almost defect-free surface with long-range 1 × 1 symmetry. A similar surface can also be prepared with a hydrogen-containing cooling gas, but the content of hydrogen in that stream is critical.

Simultaneous square-wave voltammetric determination of aspartame and cyclamate using a boron-doped diamond electrode.

Science.gov (United States)

Medeiros, Roberta Antigo; de Carvalho, Adriana Evaristo; Rocha-Filho, Romeu C; Fatibello-Filho, Orlando

2008-07-30

A simple and highly selective electrochemical method was developed for the simultaneous determination of aspartame and cyclamate in dietary products at a boron-doped diamond (BDD) electrode. In square-wave voltammetric (SWV) measurements, the BDD electrode was able to separate the oxidation peak potentials of aspartame and cyclamate present in binary mixtures by about 400 mV. The detection limit for aspartame in the presence of 3.0x10(-4) mol L(-1) cyclamate was 4.7x10(-7) mol L(-1), and the detection limit for cyclamate in the presence of 1.0x10(-4) mol L(-1) aspartame was 4.2x10(-6) mol L(-1). When simultaneously changing the concentration of both aspartame and cyclamate in a 0.5 mol L(-1) sulfuric acid solution, the corresponding detection limits were 3.5x10(-7) and 4.5x10(-6) mol L(-1), respectively. The relative standard deviation (R.S.D.) obtained was 1.3% for the 1.0x10(-4) mol L(-1) aspartame solution (n=5) and 1.1% for the 3.0x10(-3) mol L(-1) cyclamate solution. The proposed method was successfully applied in the determination of aspartame in several dietary products with results similar to those obtained using an HPLC method at 95% confidence level.

ENHANCEMENT OF THE SENSITIVITY AND SELECTIVITY OF THE VOLTAMMETRIC SENSOR FOR URIC ACID USING MOLECULARLY IMPRINTED POLYMER

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Miratul Khasanah

2010-12-01

Full Text Available The sensitivity and selectivity of voltammetric sensor for uric acid can be improved by modifying the working electrode using a polymer with a molecular template (molecularly imprinted polymer, MIP. Polymer and MIP was synthesized from methacrylic acid (MAA as monomer, ethylene glycol dimethacrylic acid (EGDMA as cross-linker, uric acid (UA as template and the results were characterized by various methods. The poly-MAA formation was identified by a decrease in the intensity of infrared (IR spectra at ~1540 cm-1 (C=C and an increase at ~1700 cm-1 (C=O compared to the IR spectra of the MAA and EGDMA. The SEM analysis showed that the cavity of polymer is small enough (~ 0.1 µm and homogeneous. Establishment of MIP was carried out by extracting of the uric acid from the polymer network. The IR spectra of MIP exhibited the decrease in intensity at ~1700 cm-1 (C=O compared to the non imprinted polymer (NIP. The data of BET analysis showed that polymer pore size increase slightly from 37.71 Å to 38.02 Å after the extraction process of uric acid from the polymer network. Its may be due to incomplete extraction of uric acid from the polymer network. Modifications of hanging mercury drop electrode using MIP made from MAA, EGDMA, and UA with a mole ratio of 1:3:1 produced a sensitive and selective voltammetric sensor for uric acid. The sensitivity obtained was 16.405 nA L/µg. The presence of ascorbic acid in equal concentration with uric acid decreased the current response of only 0.08%. Compared to HMDE electrode, the sensitivity and selectivity of the HMDE-MIP sensor enhanced about 100 and 700 times, respectively. The detection limit was found to be 5.94 x10-10 M.

Voltammetric behavior and determination of the macrolide antibiotics azithromycin, clarithromycin and roxithromycin at a renewable silver – amalgam film electrode

International Nuclear Information System (INIS)

Vajdle, Olga; Guzsvány, Valéria; Škorić, Dušan; Csanádi, János; Petković, Miloš; Avramov-Ivić, Milka; Kónya, Zoltán; Petrović, Slobodan

2017-01-01

Highlights: • Voltammetric characterization of AZI, CLA and ROX at Hg(Ag)FE was performed. • AZI, CLA and ROX were determined via optimized SWV and SW-AdSV procedures. • Protonated forms of AZI, CLA and ROX favored their adsorption on Hg(Ag)FE. • 1 H NMR chemical shift dependence of N-methyl proton signals from pH. • Optimized SW-AdSV procedure was applied to determine ROX in Runac ® tablet. - Abstract: The renewable silver-amalgam film electrode (Hg(Ag)FE) was applied for voltammetric characterization and determination of semi-synthetic macrolide antibiotics azithromycin (AZI), clarithromycin (CLA) and roxithromycin (ROX) in the Britton-Robinson buffer as supporting electrolyte ranging the pH from 4.0 to 11.9. All three macrolides showed reduction signals in fairly negative potential range. During direct cathodic square wave voltammetric (SWV) investigations conducted over the potential range from −0.75 V to −2.00 V vs SCE, either one or two reduction peaks were obtained in the potential range from −1.5 to −1.9 V. The shapes and intensities of the signals depend on the applied pH values in wider pH ranges. For analytical purposes concerning the development of direct cathodic SWV and adsorptive stripping SWV (SW-AdSV) methods the neutral and slightly alkaline media were suitable as pH 7.2, pH 7.4 and pH 7.0 for AZI, CLA and ROX, respectively. Based on the cyclic voltammograms recorded at these pH values, adsorption-controlled electrode kinetics process can be proposed for all three macrolides. Furthermore, the water suppressed 1 H NMR measurements in the pH range between 6.0 and 10.5 indicated that the macrolide molecules at the optimal analytical conditions are predominantly in protonated form via their tertiary amino groups which supported in all three cases their adsorption on the appropriately polarized Hg(Ag)FE electrode. The optimized direct cathodic SWV methods showed good linearity in concentration ranges 4.81–23.3 μg mL −1 , 1.96�

Voltammetric Determination of Ivabradine Hydrochloride Using Multiwalled Carbon Nanotubes Modified Electrode in Presence of Sodium Dodecyl Sulfate.

Science.gov (United States)

Attia, Ali Kamal; Abo-Talib, Nisreen Farouk; Tammam, Marwa Hosny

2017-04-01

Purpose: A new sensitive sensor was fabricated for the determination of ivabradine hydrochloride (IH) based on modification with multiwalled carbon nanotubes using sodium dodecyl sulfate as micellar medium to increase the sensitivity. Methods: The electrochemical behavior of IH was studied in Britton-Robinson buffer (pH: 2.0-11.0) using cyclic and differential pulse voltammetry. Results: The voltammetric response was linear over the range of 3.984 x 10 -6 -3.475 x 10 -5 mol L -1 . The limits of detection and quantification were found to be 5.160 x 10 -7 and 1.720 x 10-6 mol L -1 , respectively. Conclusion: This method is suitable for determination of IH in tablets and plasma.

Voltammetric Response of Alizarin Red S-Confined Film-Coated Electrodes to Diol and Polyol Compounds: Use of Phenylboronic Acid-Modified Poly(ethyleneimine) as Film Component.

Science.gov (United States)

Takahashi, Shigehiro; Suzuki, Iwao; Ojima, Takuto; Minaki, Daichi; Anzai, Jun-Ichi

2018-01-22

Alizarin red S (ARS) was confined in layer-by-layer (LbL) films composed of phenylboronic acid-modified poly(ethyleneimine) (PBA-PEI) and carboxymethylcellulose (CMC) to study the voltammetric response to diol and polyol compounds. The LbL film-coated gold (Au) electrode and quartz slide were immersed in an ARS solution to uptake ARS into the film. UV-visible absorption spectra of ARS-confined LbL film suggested that ARS formed boronate ester (ARS-PBS) in the film. The cyclic voltammetry of the ARS-confined LbL film-coated electrodes exhibited oxidation peaks at -0.50 and -0.62 V, which were ascribed to the oxidation reactions of ARS-PBS and free ARS, respectively, in the LbL film. The peak current at -0.62 V increased upon the addition of diol or polyol compounds such as L-dopa, glucose, and sorbitol into the solution, depending on the concentration, whereas the peak current at -0.50 V decreased. The results suggest a possible use of ARS-confined PBA-PEI/CMC LbL film-coated Au electrodes for the construction of voltammetric sensors for diol and polyol compounds.

Indirect Voltammetric Sensing Platforms For Fluoride Detection on Boron-Doped Diamond Electrode Mediated via [FeF6]3− and [CeF6]2− Complexes Formation

International Nuclear Information System (INIS)

Culková, Eva; Tomčík, Peter; Švorc, Ľubomír; Cinková, Kristína; Chomisteková, Zuzana; Durdiak, Jaroslav; Rievaj, Miroslav; Bustin, Dušan

2014-01-01

Very simple and sensitive electroanalytical technique based on synergistic combination of reaction electrochemistry (specificity) and bare boron-doped diamond electrode (sensitivity) for the detection of fluorides in drinking water was developed as variant based on dynamic electrochemistry to ISE analysis. It is based on the formation of electroinactive fluoride complexes with Fe(III) and Ce(IV) ions decreasing such diffusion current of free metal on boron-doped diamond electrode. Due to low background signal of boron-doped diamond electrode reasonably low detection limits of the order of 10 −6 mol L −1 for linear sweep voltammetric method using formation of [FeF 6 ] 3− and 10 −7 mol L −1 in a square-wave variant of this technique have been achieved. This is approximately 1–2 orders lower than in the case of platinum comb-shaped interdigitated microelectrode array. Linear sweep voltammetric method based on [CeF 6 ] 2− complex formation has lower sensitivity and may be suitable for samples with higher content of fluoride and not to analysis of drinking water

Voltammetric Studies on Vitamins D2 and D3 in Organic Solvents

International Nuclear Information System (INIS)

Chan, Ya Yun; Yue, Yanni; Webster, Richard D.

2014-01-01

Highlights: • Vitamins D 2 and D 3 undergo a chemically irreversible oxidation process. • The electrochemical oxidation occurs via one-electron on short (CV) time-scales. • On long time scales (electrolysis) the oxidation occurs via two-electrons. • Chemical oxidation was performed using two molar equivalents of NO + . • Oxidation occurs at the triene moiety. - Abstract: The electrochemical behavior of vitamins D 2 and D 3 were examined by performing cyclic voltammetry (CV), rotating disk electrode voltammetry, controlled potential electrolysis and chemical oxidation in aprotic organic solvents. Both vitamins were electrochemically oxidized in dichloromethane and acetonitrile (E p ox ∼ +0.8 vs. (Fc/Fc + )/V, where E p ox is the anodic peak potential and Fc = ferrocene) via a one-electron chemically irreversible process on the short voltammetric time scale (≤ seconds). Varying the scan rate (0.1 V s −1 to 20 V s −1 ) and temperature (233 K to 293 K) did not strongly affect the voltammetric response recorded on platinum and glassy carbon electrode surfaces with the oxidation process remaining chemically irreversible over the range of scan rates and temperatures tested, indicating that the initially formed cation radical was not long-lived. Repetitive CV experiments indicated that the oxidized product partially adsorbed onto the electrode surface, resulting in diminishing peak currents with multiple scans. Bulk controlled potential electrolysis of the vitamin D compounds performed by alternating several cycles of oxidative electrolysis and reductive pulsed stripping proved to be effective in stripping the adsorbed species off the electrode surfaces. Longer time scale bulk electrolysis experiments led to the detection of a new oxidation peak appearing at less positive potentials as the electrolysis progressed, suggesting that the compounds underwent oxidation on long time scales (minutes to hours) via a two electron process. The vitamins were most

Facile stripping voltammetric determination of haloperidol using a high performance magnetite/carbon nanotube paste electrode in pharmaceutical and biological samples

International Nuclear Information System (INIS)

Bagheri, Hasan; Afkhami, Abbas; Panahi, Yunes; Khoshsafar, Hosein; Shirzadmehr, Ali

2014-01-01

Multi-walled carbon nanotubes decorated with Fe 3 O 4 nanoparticles were prepared to construct a novel sensor for the determination of haloperidol (Hp) by voltammetric methods. The morphology and properties of electrode surface were characterized by scanning electron microscopy (SEM) and electrochemical impedance spectroscopy. This modified sensor was used as a selective electrochemical sensor for the determination of trace amounts of Hp. The peak currents of differential pulse and square wave voltammograms of Hp increased linearly with its concentration in the ranges of 1.2 × 10 −3 –0.52 and 6.5 × 10 −4 –0.52 μmol L −1 , respectively. The detection limits for Hp were 7.02 × 10 −4 and 1.33 × 10 −4 μmol L −1 for differential pulse and square wave voltammetric methods, respectively. The results show that the combination of multi-walled carbon nanotubes and Fe 3 O 4 nanoparticles causes a dramatic enhancement in the sensitivity of Hp quantification. This sensor was successfully applied to determine Hp in pharmaceutical samples and biological fluids. The fabricated electrode showed excellent reproducibility, repeatability and stability. - Highlights: • A sensitive paste using Fe 3 O 4 /multi-walled carbon nanotubes was fabricated. • Haloperidol determination is based on its adsorption on the surface of Fe 3 O 4 /MWCNTs. • Different electrochemical methods and impedance spectroscopy were used for this study. • Haloperidol was determined in pharmaceutical and biological samples. • In comparison to other conventional methods, this method is simple, rapid, selective and cost-effective

Voltammetric study of chromium(VI)-ammonia/ammonium chloride solutions in the presence of dimethylglyoxime

International Nuclear Information System (INIS)

Ginzburg, V.G.; Salikhdzhanova, R.M.F.

1987-01-01

The authors believed complexation to be possible in the system Cr(VI)-dimethylglyoxime (DMG, H 2 D) by reduction of Cr(VI) to Cr(III) on a mercury electrode. The DMG can be used in chromium voltammetry and is promising for a number of reasons: The Cr(III) has an affinity for donor nitrogen atoms in the DMG molecule. Insertion of the H 2 D into the inner sphere of the complex is expected to weaken the bond between the Cr(III) and the hydroxyl group, slow down formation of the insoluble hydroxide Cr(OH) 3 , and lower the rate of the electrode reaction Cr(III) → Cr(II). Molecules of H 2 D adsorb on a mercury electrode. It is therefore possible to accelerate the electrode process by including adsorptive preconcentration of the chromium and thus lowering its detection limit. This paper reports the voltammetric behavior of the system Cr(VI)-DMG-NH 4 + (proton donor) for the purpose of lowering the chromium detection limit

Voltammetric Determination of Ivabradine Hydrochloride Using Multiwalled Carbon Nanotubes Modified Electrode in Presence of Sodium Dodecyl Sulfate

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Ali Kamal Attia

2017-04-01

Full Text Available Purpose: A new sensitive sensor was fabricated for the determination of ivabradine hydrochloride (IH based on modification with multiwalled carbon nanotubes using sodium dodecyl sulfate as micellar medium to increase the sensitivity. Methods: The electrochemical behavior of IH was studied in Britton-Robinson buffer (pH: 2.0-11.0 using cyclic and differential pulse voltammetry. Results: The voltammetric response was linear over the range of 3.984 x 10-6-3.475 x 10-5 mol L-1. The limits of detection and quantification were found to be 5.160 x 10-7 and 1.720 x 10-6 mol L-1, respectively. Conclusion: This method is suitable for determination of IH in tablets and plasma.

A voltammetric electronic tongue as tool for water quality monitoring in wastewater treatment plants.

Science.gov (United States)

Campos, Inmaculada; Alcañiz, Miguel; Aguado, Daniel; Barat, Ramón; Ferrer, José; Gil, Luis; Marrakchi, Mouna; Martínez-Mañez, Ramón; Soto, Juan; Vivancos, José-Luis

2012-05-15

The use of a voltammetric electronic tongue as tool for the prediction of concentration levels of certain water quality parameters from influent and effluent wastewater from a Submerged Anaerobic Membrane Bioreactor pilot plant applied to domestic wastewater treatment is proposed here. The electronic tongue consists of a set of noble (Au, Pt, Rh, Ir, and Ag) and non-noble (Ni, Co and Cu) electrodes that were housed inside a stainless steel cylinder which was used as the body of the electronic tongue system. As a previous step an electrochemical study of the response of the ions sulphate, orthophosphate, acetate, bicarbonate and ammonium was carried out in water using the electrodes contained in the electronic tongue. The second part of the work was devoted to the application of the electronic tongue to the characterization of the influent and effluent waters from the wastewater treatment plant. Partial Least Squares analysis was used to obtain a correlation between the data from the tongue and the pollution parameters measured in the laboratory such as soluble chemical oxygen demand (CODs), soluble biological oxygen demand (BODs), ammonia (NH(4)-N), orthophosphate (PO(4)-P), Sulphate (SO(4)-S), acetic acid (HAC) and alkalinity (Alk). A total of 28 and 11 samples were used in the training and the validation steps, respectively, for both influent and effluent water samples. The electronic tongue showed relatively good predictive power for the determination of BOD, COD, NH(4)-N, PO(4)-P, SO(4)-S, and Alk. Copyright © 2012 Elsevier Ltd. All rights reserved.

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

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Anamaria Baciu

2015-06-01

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

Adsorptive Stripping Voltammetric Determination of Hydroquinone using an Electrochemically Pretreated Glassy Carbon Electrode

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Abdul Niaz1,

2008-12-01

Full Text Available A simple and efficient adsorptive stripping voltammetric (AdSV method was developed for the determination of hydroquinone at an electrochemically pretreated glassy carbon (GC electrode in waste water. Various parameters such as solvent system, accumulation potential, accumulation time and scan rate were optimized. The electrochemically pretreated GC electrode showed good response towards hydroquinone determination by using AdSV. Under the optimized conditions the peak current showed good linear relationship with the hydroquinone concentration in the range of 0.5-4.0mg L-1 and 5-30mg L-1. The 60/40 methanol/water composition was found to be the best solvent system and 0.05mol L-1 H2SO4 was found as useful supporting electrolyte concentration. The accumulation time was 60 s and the detection limit was 50µg L-1. The developed method was successfully applied for the determination of hydroquinone in polymeric industrial discharge samples waste photographic developer solution and cream sample without any significant effect of surface fouling.

Facile stripping voltammetric determination of haloperidol using a high performance magnetite/carbon nanotube paste electrode in pharmaceutical and biological samples

Energy Technology Data Exchange (ETDEWEB)

Bagheri, Hasan, E-mail: h.bagheri@srbiau.ac.ir [Chemical Injuries Research Center, Baqiyatallah University of Medical Sciences, Tehran (Iran, Islamic Republic of); Afkhami, Abbas [Faculty of Chemistry, Bu-Ali Sina University, Hamedan (Iran, Islamic Republic of); Panahi, Yunes [Chemical Injuries Research Center, Baqiyatallah University of Medical Sciences, Tehran (Iran, Islamic Republic of); Khoshsafar, Hosein; Shirzadmehr, Ali [Faculty of Chemistry, Bu-Ali Sina University, Hamedan (Iran, Islamic Republic of)

2014-04-01

Multi-walled carbon nanotubes decorated with Fe{sub 3}O{sub 4} nanoparticles were prepared to construct a novel sensor for the determination of haloperidol (Hp) by voltammetric methods. The morphology and properties of electrode surface were characterized by scanning electron microscopy (SEM) and electrochemical impedance spectroscopy. This modified sensor was used as a selective electrochemical sensor for the determination of trace amounts of Hp. The peak currents of differential pulse and square wave voltammograms of Hp increased linearly with its concentration in the ranges of 1.2 × 10{sup −3}–0.52 and 6.5 × 10{sup −4}–0.52 μmol L{sup −1}, respectively. The detection limits for Hp were 7.02 × 10{sup −4} and 1.33 × 10{sup −4} μmol L{sup −1} for differential pulse and square wave voltammetric methods, respectively. The results show that the combination of multi-walled carbon nanotubes and Fe{sub 3}O{sub 4} nanoparticles causes a dramatic enhancement in the sensitivity of Hp quantification. This sensor was successfully applied to determine Hp in pharmaceutical samples and biological fluids. The fabricated electrode showed excellent reproducibility, repeatability and stability. - Highlights: • A sensitive paste using Fe{sub 3}O{sub 4}/multi-walled carbon nanotubes was fabricated. • Haloperidol determination is based on its adsorption on the surface of Fe{sub 3}O{sub 4}/MWCNTs. • Different electrochemical methods and impedance spectroscopy were used for this study. • Haloperidol was determined in pharmaceutical and biological samples. • In comparison to other conventional methods, this method is simple, rapid, selective and cost-effective.

Determination of lead element trace in some Syrian cigarettes and Its mixtures using voltammetric method on HMDE

International Nuclear Information System (INIS)

Nasser, H.; Kabass, H.

2010-01-01

This study aims for estimating of trace for these elements in various brands of Syrian Cigarettes and its mixtures, by using voltammetric method (HMDE) hanging mercury drop elec trod. This method is first used to determined Syrian Cigarettes brand and its mixtures, during this study it was found that we can use it easily with low commission, high sensitivity and accurate results comparing with others studies. We prepare the samples by using reference methods. The samples were collected during two times in one year from the same kinds of samples. We noticed that the high concentrations was (3.795μg/g) in Gitanes samples, and the low concentrations in shame samples was (0.37 μg/g). This study refers that there is different concentrations of lead element in this samples.(author)

Estudo voltamétrico do complexo de cobre(II com o ligante vermelho de alizarina S, adsorvido na superfície do eletrodo de grafite pirolítico Voltammetric study of complex of copper (II with alizarin red S ligand, absorbed on surface of pyrolytic graphite electrode

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Victor E. Mouchrek Filho

1999-06-01

Full Text Available The alizarin red S (ARS has been used as a spectrophotometric reagent of several metals for a long time. Now this alizarin has been used as modifier agent of electrodes, for voltammetric analyses. In this work cyclic voltammetry experiments was accomplished on closed circuit, with the objective of studying the voltammetric behavior of alizarin red S adsorbed and of its copper complex, on the surface of the pyrolytic graphite electrode. These studies showed that ARS strongly adsorbs on the surface of this electrode. This adsorption was used to immobilize ions copper(II from the solution.

Electrochemical Investigation of Catechol at Poly(niacinamide Modified Carbon Paste Electrode: A Voltammetric Study

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A. B. Teradale

2016-01-01

Full Text Available A polymeric thin film modified electrode, that is, poly(niacinamide modified carbon paste electrode (MCPE, was developed for the electrochemical determination of catechol (CC by using cyclic voltammetric technique. Compared to bare carbon paste electrode (BCPE, the poly(niacinamide MCPE shows good electrocatalytic activity towards the oxidation of catechol in phosphate buffer solution (PBS of physiological pH 7.4. All experimental parameters were optimized. Poly(niacinamide modified carbon paste electrode gave a linear response between concentration of CC and its anodic peak current in the range within 20.6–229.0 μM. The limit of detection (3S/M and limit of quantification (10S/M were 1.497 μM and 4.99 μM, respectively. From the study of scan rate variation, the electrode process was found to be adsorption-controlled. The involvement of protons and electrons in the oxidation of CC was found to be equal. The probable electropolymerisation mechanism of niacinamide was proposed. Finally, this method can be used in development of a sensor for sensitive determination of CC.

Inappropriate use of the quasi-reversible electrode kinetic model in simulation-experiment comparisons of voltammetric processes that approach the reversible limit.

Science.gov (United States)

Simonov, Alexandr N; Morris, Graham P; Mashkina, Elena A; Bethwaite, Blair; Gillow, Kathryn; Baker, Ruth E; Gavaghan, David J; Bond, Alan M

2014-08-19

Many electrode processes that approach the "reversible" (infinitely fast) limit under voltammetric conditions have been inappropriately analyzed by comparison of experimental data and theory derived from the "quasi-reversible" model. Simulations based on "reversible" and "quasi-reversible" models have been fitted to an extensive series of a.c. voltammetric experiments undertaken at macrodisk glassy carbon (GC) electrodes for oxidation of ferrocene (Fc(0/+)) in CH3CN (0.10 M (n-Bu)4NPF6) and reduction of [Ru(NH3)6](3+) and [Fe(CN)6](3-) in 1 M KCl aqueous electrolyte. The confidence with which parameters such as standard formal potential (E(0)), heterogeneous electron transfer rate constant at E(0) (k(0)), charge transfer coefficient (α), uncompensated resistance (Ru), and double layer capacitance (CDL) can be reported using the "quasi-reversible" model has been assessed using bootstrapping and parameter sweep (contour plot) techniques. Underparameterization, such as that which occurs when modeling CDL with a potential independent value, results in a less than optimal level of experiment-theory agreement. Overparameterization may improve the agreement but easily results in generation of physically meaningful but incorrect values of the recovered parameters, as is the case with the very fast Fc(0/+) and [Ru(NH3)6](3+/2+) processes. In summary, for fast electrode kinetics approaching the "reversible" limit, it is recommended that the "reversible" model be used for theory-experiment comparisons with only E(0), Ru, and CDL being quantified and a lower limit of k(0) being reported; e.g., k(0) ≥ 9 cm s(-1) for the Fc(0/+) process.

Inappropriate Use of the Quasi-Reversible Electrode Kinetic Model in Simulation-Experiment Comparisons of Voltammetric Processes That Approach the Reversible Limit

KAUST Repository

Simonov, Alexandr N.

2014-08-19

Many electrode processes that approach the "reversible" (infinitely fast) limit under voltammetric conditions have been inappropriately analyzed by comparison of experimental data and theory derived from the "quasi-reversible" model. Simulations based on "reversible" and "quasi-reversible" models have been fitted to an extensive series of a.c. voltammetric experiments undertaken at macrodisk glassy carbon (GC) electrodes for oxidation of ferrocene (Fc0/+) in CH3CN (0.10 M (n-Bu)4NPF6) and reduction of [Ru(NH 3)6]3+ and [Fe(CN)6]3- in 1 M KCl aqueous electrolyte. The confidence with which parameters such as standard formal potential (E0), heterogeneous electron transfer rate constant at E0 (k0), charge transfer coefficient (α), uncompensated resistance (Ru), and double layer capacitance (CDL) can be reported using the "quasi- reversible" model has been assessed using bootstrapping and parameter sweep (contour plot) techniques. Underparameterization, such as that which occurs when modeling CDL with a potential independent value, results in a less than optimal level of experiment-theory agreement. Overparameterization may improve the agreement but easily results in generation of physically meaningful but incorrect values of the recovered parameters, as is the case with the very fast Fc0/+ and [Ru(NH3)6]3+/2+ processes. In summary, for fast electrode kinetics approaching the "reversible" limit, it is recommended that the "reversible" model be used for theory-experiment comparisons with only E0, R u, and CDL being quantified and a lower limit of k 0 being reported; e.g., k0 ≥ 9 cm s-1 for the Fc0/+ process. © 2014 American Chemical Society.

Inappropriate Use of the Quasi-Reversible Electrode Kinetic Model in Simulation-Experiment Comparisons of Voltammetric Processes That Approach the Reversible Limit

KAUST Repository

Simonov, Alexandr N.; Morris, Graham P.; Mashkina, Elena A.; Bethwaite, Blair; Gillow, Kathryn; Baker, Ruth E.; Gavaghan, David J.; Bond, Alan M.

2014-01-01

Many electrode processes that approach the "reversible" (infinitely fast) limit under voltammetric conditions have been inappropriately analyzed by comparison of experimental data and theory derived from the "quasi-reversible" model. Simulations based on "reversible" and "quasi-reversible" models have been fitted to an extensive series of a.c. voltammetric experiments undertaken at macrodisk glassy carbon (GC) electrodes for oxidation of ferrocene (Fc0/+) in CH3CN (0.10 M (n-Bu)4NPF6) and reduction of [Ru(NH 3)6]3+ and [Fe(CN)6]3- in 1 M KCl aqueous electrolyte. The confidence with which parameters such as standard formal potential (E0), heterogeneous electron transfer rate constant at E0 (k0), charge transfer coefficient (α), uncompensated resistance (Ru), and double layer capacitance (CDL) can be reported using the "quasi- reversible" model has been assessed using bootstrapping and parameter sweep (contour plot) techniques. Underparameterization, such as that which occurs when modeling CDL with a potential independent value, results in a less than optimal level of experiment-theory agreement. Overparameterization may improve the agreement but easily results in generation of physically meaningful but incorrect values of the recovered parameters, as is the case with the very fast Fc0/+ and [Ru(NH3)6]3+/2+ processes. In summary, for fast electrode kinetics approaching the "reversible" limit, it is recommended that the "reversible" model be used for theory-experiment comparisons with only E0, R u, and CDL being quantified and a lower limit of k 0 being reported; e.g., k0 ≥ 9 cm s-1 for the Fc0/+ process. © 2014 American Chemical Society.

Solar UV-treatment of water samples for stripping-voltammetric determination of trace heavy metals in Awash river, Ethiopia

Directory of Open Access Journals (Sweden)

Gelaneh Woldemichael

2016-03-01

Full Text Available We report about testing a new mobile and sustainable water sample digestion method in a preliminary field trial in Ethiopia. In order to determine heavy metals at the ultra-trace level by stripping voltammetric techniques in water samples from Awash River, we applied our new method of solar UV-assisted sample pretreatment to destroy the relevant interfering dissolved organic matter. The field tests revealed that 24 h of solar UV irradiation were sufficient to achieve the same sample pretreatment results as with classic digestion method based on intense and hard UV. Analytical results of this study suggest that both a hydroelectric power station and agrichemical applications at Koka Lake have increased the levels of the investigated metals zinc, cadmium, lead, copper, cobalt, nickel, and uranium.

Evaluation of red wines antioxidant capacity by means of a voltammetric e-tongue with an optimized sensor array

International Nuclear Information System (INIS)

Cetó, Xavi; Apetrei, Constantin; Valle, Manel del; Rodríguez-Méndez, Maria Luz

2014-01-01

In this work, two sets of voltammetric sensors -prepared using different strategies- have been combined in an electronic tongue to evaluate the complete antioxidant profile of red wines. To this aim, wine samples were analyzed with the whole set of sensors. In order to reduce the large dimensionality of the data set while keeping the relevant information provided by the sensors, two different methods of feature selection and data compression were used (the kernels method and Discrete Wavelet Transform feature extraction method). Then, the coefficients obtained were used as the input variables of Principal Component Analysis (to evaluate the capability of discrimination. Partial-least squares regression (PLS) and artificial neural networks (ANNs) were performer to build the quantitative prediction models that allowed the quantification of the antioxidant capacity of the tested wines

Differential pulse polarography of cadmium-and lead-urate and adsorptive stripping voltammetric determination of uric acid.

Science.gov (United States)

Gandour, M A; Ensaf-Aboul-Kasim; Amrallah, A H; Farghaly, O A

1994-03-01

The complex formation between uric acid and zinc, cadmium and lead ions has been investigated using differential pulse polarography in 0.01M NaNO(3). It is found that the complexes formed by Cd(II) and Pb(II) ions with uric acid have the stoichiometry of 1:2 and the logarithmic values of the apparent stability constant are 9.47 and 11.7, respectively. On the other hand, zinc(II) ions do not give any indication of complexation with uric acid. A sensitive voltammetric method is developed for the quantitative determination of uric acid. This method is based on controlled adsorptive preconcentration of uric acid on the hanging mercury drop electrode (HMDE), followed by tracing the voltammogram in the cathodic going potential scan. The modes used are direct current stripping voltammetry (DCSV) and differential pulse stripping voltammetry (DPSV). The detection limits found were 8 x 10(-9)M (quiescent period 15 sec) by DPSV and 1.6 x 10(-8)M by DCSV.

Anodic stripping voltammetric determination of silver ion at a carbon paste electrode modified with carbon nanotubes

International Nuclear Information System (INIS)

Tashkhourian, J.; Javadi, S.; Ana, F.N.

2011-01-01

A carbon paste electrode (CPE) was modified with multi-wall carbon nanotubes and successfully applied to the determination of silver ion by differential pulse anodic stripping voltammetry. Compared to a conventional CPE, a remarkably improved peak current response and sensitivity is observed. The analytical procedure consisted of an open circuit accumulation step for 2 min in -0.4 V, this followed by an anodic potential scan between +0.2 and + 0.6 V to obtain the voltammetric peak. The oxidation peak current is proportional to the concentration of silver ion in the range from 1.0 x 10 -8 to 1.0 x 10 -5 mol L -1 , with a detection limit of 1.8 x 10 -9 mol L -1 after an accumulation time of 120 s. The relative standard deviation for 7 successive determinations of Ag(I) at 0.1 μM concentration is 1.99%. The procedure was validated by determining Ag(I) in natural waters. (author)

Square Wave Voltammetric Determination of 2-Thiouracil in Pharmaceuticals and Real Samples Using Glassy Carbon Electrode

Directory of Open Access Journals (Sweden)

Naveen M. Gokavi

2013-01-01

Full Text Available A simple and rapid method was developed using cyclic and square wave voltammetric techniques for the determination of trace-level sulfur containing compound, 2-thiouracil, at a glassy carbon electrode. 2-thiouracil produced two anodic peaks at 0.334 V and 1.421 V and a cathodic peak at −0.534 V. The square wave voltammetry of 2-thiouracil gave a good linear response in the range of 1–20 μM with a detection limit of 0.16 μM and quantification limit of 0.53 μM (0.0679 μg/g, which is in good agreement as per IUPAC definition of trace component analysis (100 μg/g. The obtained recoveries range from 98.10% to 102.1%. The proposed method was used successfully for its quantitative determination in pharmaceutical formulations and urine as real samples.

Monitoring of quality and storage time of unsealed pasteurized milk by voltammetric electronic tongue

International Nuclear Information System (INIS)

Wei, Zhenbo; Wang, Jun; Zhang, Xi

2013-01-01

A voltammetric electronic tongue (VE-tongue) was self-developed and applied to monitor the quality and storage time of unsealed pasteurized milk. The VE-tongue comprised four working electrodes: gold, silver, platinum, and palladium electrode. Two potential waveforms: Multi-frequency rectangle pulse voltammetry (MRPV) and multi-frequency staircase pulse voltammetry (MSPV) were applied to working electrodes in the study, and both of MRPV and MSPV consisted of three frequency segments: 1 Hz, 10 Hz, and 100 Hz. The total areas under the corresponding curves obtained by VE-tongue in the three frequencies were applied as characteristic data, which were evaluated by the principal component analysis (PCA) and cluster analysis (CA). The results of PCA and CA indicate that the milk samples of different storage time could be successfully classified by the VE-tongue based on MRPV and MSPV, respectively. Combining the areas obtained by the VE-tongue based on MRPV and MSPV, the classification results of PCA and CA were improved evidently. The total bacterial count, acidity and viscosity of the milk samples were also measured during the storage, and those physicochemical characteristics showed regular configuration in PCA and CA plots. Furthermore, the total bacterial count and viscosity properties were predicted by partial least squares regression (PLSR) and least squares-support vector machines (LS-SVM), and the combination of the areas obtained by the VE-tongue based on the MRPV and MSPV were applied as the input data of PLSR and LS-SVM. Both the prediction techniques performed well in predicting viscosity and total bacterial count, and the prediction results of LS-SVM were better than that of PLSR. Those results demonstrate that the VE-tongue could be applied to monitor the quality storage time of unsealed pasteurized milk

Application of graphene for preconcentration and highly sensitive stripping voltammetric analysis of organophosphate pesticide

Energy Technology Data Exchange (ETDEWEB)

Wu Shuo, E-mail: wushuo@dlut.edu.cn [School of Chemistry, Dalian University of Technology, Dalian 116023 (China); Lan Xiaoqin; Cui Lijun; Zhang Lihui; Tao Shengyang; Wang Hainan; Han Mei; Liu Zhiguang; Meng Changgong [School of Chemistry, Dalian University of Technology, Dalian 116023 (China)

2011-08-12

Highlights: {yields} An electrochemical sensor is fabricated based on {beta}-CD dispersed graphene. {yields} The sensor could selectively detect organophosphate pesticide with high sensitivity. {yields} The {beta}-CD dispersed graphene owns large adsorption capacity for MP and superconductivity. {yields} The {beta}-CD dispersed graphene is superior to most of the porous sorbents ever known. - Abstract: Electrochemical reduced {beta}-cyclodextrin dispersed graphene ({beta}-CD-graphene) was developed as a sorbent for the preconcentration and electrochemical sensing of methyl parathion (MP), a representative nitroaromatic organophosphate pesticide with good redox activity. Benefited from the ultra-large surface area, large delocalized {pi}-electron system and the superconductivity of {beta}-CD-graphene, large amount of MP could be extracted on {beta}-CD-graphene modified electrode via strong {pi}-{pi} interaction and exhibited fast accumulation and electron transfer rate. Combined with differential pulse voltammetric analysis, the sensor shows ultra-high sensitivity, good selectivity and fast response. The limit of detection of 0.05 ppb is more than 10 times lower than those obtained from other sorbent based sensors. The method may open up a new possibility for the widespread use of electrochemical sensors for monitoring of ultra-trace OPs.

Studies on voltammetric determination of cadmium in samples containing native and digested proteins

Energy Technology Data Exchange (ETDEWEB)

Drozd, Marcin; Pietrzak, Mariusz, E-mail: mariusz@ch.pw.edu.pl; Malinowska, Elżbieta

2014-03-01

Highlights: • Proteins exhibit diverse impact on the DPASV cadmium signals. • Proteins subjected to HNO{sub 3} introduce less interference, than the native ones. • Optimal amount of SDS depends on the kind of protein. • Presence of thiolated coating agents of QDs do not influence the analysis. - Abstract: This work focuses on determination of cadmium ions using anodic stripping voltammetry (ASV) on thin film mercury electrode in conditions corresponding to those obtained after digestion of cadmium-based quantum dots and their conjugates. It presents the impact of selected proteins, including potential receptors and surface blocking agents on the voltammetric determination of cadmium. Experiments regarding elimination of interferences related to proteins presence using sodium dodecyl sulfate (SDS) are also shown. Effect of SDS on selected analytical parameters and simplicity of analyses carried out was investigated in the framework of current studies. The significant differences of influence among tested proteins on ASV cadmium determination, as well as the variability in SDS effectiveness as the antifouling agent were observed and explained. This work is especially important for those, who design new bioassays and biosensors with a use of quantum dots as electrochemical labels, as it shows what problems may arise from presence of native and digested proteins in tested samples.

Voltammetric and Mathematical Evidence for Dual Transport Mediation of Serotonin Clearance In Vivo

Science.gov (United States)

Wood, Kevin M.; Zeqja, Anisa; Nijhout, H. Frederik; Reed, Michael C.; Best, Janet; Hashemi, Parastoo

2014-01-01

The neurotransmitter serotonin underlies many of the brain’s functions. Understanding serotonin neurochemistry is important for improving treatments for neuropsychiatric disorders such as depression. Antidepressants commonly target serotonin clearance via serotonin transporters (SERTs) and have variable clinical effects. Adjunctive therapies, targeting other systems including serotonin autoreceptors, also vary clinically and carry adverse consequences. Fast scan cyclic voltammetry (FSCV) is particularly well suited for studying antidepressant effects on serotonin clearance and autoreceptors by providing real-time chemical information on serotonin kinetics in vivo. However, the complex nature of in vivo serotonin responses makes it difficult to interpret experimental data with established kinetic models. Here, we electrically stimulated the mouse medial forebrain bundle (MFB) to provoke and detect terminal serotonin in the substantia nigra reticulata (SNr). In response to MFB stimulation we found three dynamically distinct serotonin signals. To interpret these signals we developed a computational model that supports two independent serotonin reuptake mechanisms (high affinity, low efficiency reuptake mechanism and low affinity, high efficiency reuptake system) and bolsters an important inhibitory role for the serotonin autoreceptors. Our data and analysis, afforded by the powerful combination of voltammetric and theoretical methods, gives new understanding of the chemical heterogeneity of serotonin dynamics in the brain. This diverse serotonergic matrix likely contributes to clinical variability of antidepressants. PMID:24702305

Honey adulteration detection: voltammetric e-tongue versus official methods for physicochemical parameter determination.

Science.gov (United States)

Oroian, Mircea; Paduret, Sergiu; Ropciuc, Sorina

2018-02-10

The aim of this study was to evaluate the usefulness of a voltammetric e-tongue (three electrodes: reference electrode (Ag/AgCl), counter electrode (glassy carbon electrode rod) and working electrode (Au, Ag, Pt and glass electrode)) for honey adulteration detection. For this purpose, 55 samples of authentic honey (acacia, honeydew, sunflower, Tilia and polyfloral) and 150 adulterated ones were analyzed. The adulteration was made using fructose, glucose, inverted sugar, hydrolyzed inulin syrup and malt wort at different percentages: 5%, 10%, 20%, 30%, 40% and 50%, respectively. The e-tongue has been compared with the physicochemical parameters (pH, free acidity, electrical conductivity (EC) and CIEL*a*b* parameters (L*, a* and b*)) in order to achieve a suitable method for the classification of authentic and adulterated honeys. The e-tongue and physicochemical parameters reached a 97.50% correct classification of the authentic and adulterated honeys. In the case of the adulterated honey samples, the e-tongue achieved 83.33% correct classifications whereas the physicochemical parameters only achieved 73.33%. The e-tongue is a fast, easy and accurate method for honey adulteration detection which can be used in situ by beekeepers and provide useful information on EC and free acidity. © 2018 Society of Chemical Industry. © 2018 Society of Chemical Industry.

Anodic stripping voltammetric determination of traces of Pb(II) and Cd(II) using a glassy carbon electrode modified with bismuth nanoparticles

International Nuclear Information System (INIS)

Yang, Die; Wang, Liang; Chen, Zuliang; Megharaj, Mallavarapu; Naidu, Ravi

2014-01-01

We report on a glassy carbon electrode modified with bismuth nanoparticles (NanoBiE) for the simultaneous determination Pb 2+ and Cd 2+ by anodic stripping voltammetry. Operational parameters such as bismuth nanoparticles labelling amount, deposition potential, deposition time and stripping parameters were optimized with respect to the determination of Pb 2+ and Cd 2+ in 0.1 M acetate buffer solution (pH 4.5). The NanoBiE gives well-defined, reproducible and sharp stripping peaks. The peak current response increases linearly with the metal concentration in a range of 5.0–60.0 μg L −1 , with a detection limit of 0.8 and 0.4 μg L −1 for Pb 2+ and Cd 2+ , respectively. The morphology and composition of the modified electrode before and after voltammetric measurements were analysed by scanning electron microscopy and energy dispersive X-ray analysis. The NanoBiE was successfully applied to analysis of Pb 2+ and Cd 2+ in real water samples and the method was validated by ICP-MS technique, suggesting that the electrode can be considered as an interesting alternative to the bismuth film electrode for possible use in electrochemical studies and electro analysis. (author)

Voltammetric and impedance study of the influence of the anode composition on the electrochemical ferrate(VI) production in molten NaOH

International Nuclear Information System (INIS)

Hrnčiariková, Lucia; Gál, Miroslav; Kerekeš, Kamil; Híveš, Ján

2013-01-01

Three typical anode materials: pure iron (Fe), silicon-rich steel (FeSi) and white cast iron (FeC) electrodes were used in the process of electrochemical ferrate(VI) synthesis in the molten sodium hydroxide. The voltammetric peak current densities corresponding to the first and second step of the anode dissolution in the case of FeC as well as FeSi electrode are higher compared to the pure iron electrode. After passivity region subsequently the transpassive iron dissolution, including ferrate(VI) formation together with an oxygen evolution occurs and the current shoulder is visible for all electrodes used. Measured electrochemical impedance spectra confirm the physical model of the polarized surface based on the concept of two macrohomogeneous surface layers. In all cases the resistance of both inner and outer layer decrease with increasing applied potential. With increasing temperature the resistance of inner and outer layer decreases. The capacity of inner and outer layer increases with increasing potential. This is in agreement with decrease of the resistances of both layers: layers are getting thinner or more disintegrated by oxygen evolution or strong anodic dissolution. The number of exchanged electrons calculated from a static polarization curve at the potentials in ferrate(VI) formation region is z = 3 for all electrode materials used

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

Science.gov (United States)

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 attomolar levels of a sequence derived from the genom of hepatitis B virus by using molecular beacon mediated circular strand displacement and rolling circle amplification.

Science.gov (United States)

Huang, Shan; Feng, Mengmeng; Li, Jiawen; Liu, Yi; Xiao, Qi

2018-03-03

The authors describe an electrochemical method for the determination of the single-stranded DNA (ssDNA) oligonucleotide with a sequence derived from the genom of hepatitis B virus (HBV). It is making use of circular strand displacement (CSD) and rolling circle amplification (RCA) strategies mediated by a molecular beacon (MB). This ssDNA hybridizes with the loop portion of the MB immobilized on the surface of a gold electrode, while primer DNA also hybridizes with the rest of partial DNA sequences of MB. This triggers the MB-mediated CSD. The RCA is then initiated to produce a long DNA strand with multiple tandem-repeat sequences, and this results in a significant increase of the differential pulse voltammetric response of the electrochemical probe Methylene Blue at a rather low working potential of -0.24 V (vs. Ag/AgCl). Under optimal experimental conditions, the assay displays an ultrahigh sensitivity (with a 2.6 aM detection limit) and excellent selectivity. Response is linear in the 10 to 700 aM DNA concentration range. Graphical abstract Schematic of a voltammetric method for the determination of attomolar levels of target DNA. It is based on molecular beacon mediated circular strand displacement and rolling circle amplification strategies. Under optimal experimental conditions, the assay displays an ultrahigh sensitivity with a 2.6 aM detection limit and excellent selectivity.

Imprinted polymer-modified hanging mercury drop electrode for differential pulse cathodic stripping voltammetric analysis of creatine.

Science.gov (United States)

Lakshmi, Dhana; Sharma, Piyush S; Prasad, Bhim B

2007-06-15

The molecularly imprinted polymer [poly(p-aminobenzoicacid-co-1,2-dichloroethane)] film casting was made on the surface of a hanging mercury drop electrode by drop-coating method for the selective and sensitive evaluation of creatine in water, blood serum and pharmaceutical samples. The molecular recognition of creatine by the imprinted polymer was found to be specific via non-covalent (electrostatic) imprinting. The creatine binding could easily be detected by differential pulse, cathodic stripping voltammetric signal at optimised operational conditions: accumulation potential -0.01 V (versus Ag/AgCl), polymer deposition time 15s, template accumulation time 60s, pH 7.1 (supporting electrolyte< or =5 x 10(-4)M NaOH), scan rate 10 mV s(-1), pulse amplitude 25 mV. The modified sensor in the present study was found to be highly reproducible and selective with detection limit 0.11 ng mL(-1) of creatine. Cross-reactivity studies revealed no response to the addition of urea, creatinine and phenylalanine; however, some insignificant magnitude of current was observed for tryptophan and histidine in the test samples.

Highly sensitive detection of urinary cadmium to assess personal exposure

Energy Technology Data Exchange (ETDEWEB)

Argun, Avni A.; Banks, Ashley M.; Merlen, Gwendolynne; Tempelman, Linda A. [Giner, Inc., 89 Rumford Ave., Newton 02466, MA United States (United States); Becker, Michael F.; Schuelke, Thomas [Fraunhofer USA – CCL, 1449 Engineering Research Ct., East Lansing 48824, MI (United States); Dweik, Badawi M., E-mail: bdweik@ginerinc.com [Giner, Inc., 89 Rumford Ave., Newton 02466, MA United States (United States)

2013-04-22

Highlights: ► An electrochemical sensor capable of detecting cadmium at parts-per-billion levels in urine. ► A novel fabrication method for Boron-Doped Diamond (BDD) ultramicroelectrode (UME) arrays. ► Unique combination of BDD UME arrays and a differential pulse voltammetry algorithm. ► High sensitivity, high reproducibility, and very low noise levels. ► Opportunity for portable operation to assess on-site personal exposure. -- Abstract: A series of Boron-Doped Diamond (BDD) ultramicroelectrode arrays were fabricated and investigated for their performance as electrochemical sensors to detect trace level metals such as cadmium. The steady-state diffusion behavior of these sensors was validated using cyclic voltammetry followed by electrochemical detection of cadmium in water and in human urine to demonstrate high sensitivity (>200 μA ppb{sup −1} cm{sup −2}) and low background current (<4 nA). When an array of ultramicroelectrodes was positioned with optimal spacing, these BDD sensors showed a sigmoidal diffusion behavior. They also demonstrated high accuracy with linear dose dependence for quantification of cadmium in a certified reference river water sample from the U.S. National Institute of Standards and Technology (NIST) as well as in a human urine sample spiked with 0.25–1 ppb cadmium.

Voltammetric Perspectives on the Acidity Scale and H+/H2 Process in Ionic Liquid Media.

Science.gov (United States)

Bentley, Cameron L; Bond, Alan M; Zhang, Jie

2018-03-19

Nonhaloaluminate ionic liquids (ILs) have received considerable attention as alternatives to molecular solvents in diverse applications spanning the fields of physical, chemical, and biological science. One important and often overlooked aspect of the implementation of these designer solvents is how the properties of the IL formulation affect (electro)chemical reactivity. This aspect is emphasized herein, where recent (voltammetric) studies on the energetics of proton (H + ) transfer and electrode reaction mechanisms of the H + H 2 process in IL media are highlighted and discussed. The energetics of proton transfer, quantified using the pK 3 a (minus logarithm of acidity equilibrium constant, K a ) formalism, is strongly governed by the constituent IL anion, and to a lesser extent, the IL cation. The H + /H 2 process, a model inner-sphere reaction, also displays electrochemical characteristics that are strongly IL-dependent. Overall, these studies highlight the need to carry out systematic investigations to resolve IL structure and function relationships in order to realize the potential of these diverse and versatile solvents. Expected final online publication date for the Annual Review of Analytical Chemistry Volume 11 is June 12, 2018. Please see http://www.annualreviews.org/page/journal/pubdates for revised estimates.

Multi-spectroscopic and voltammetric evidences for binding, conformational changes of bovine serum albumin with thiamine.

Science.gov (United States)

Bagoji, Atmanand M; Gowda, Jayant I; Gokavi, Naveen M; Nandibewoor, Sharanappa T

2017-08-01

The interaction between thiamine hydrochloride (TA) and bovine serum albumin (BSA) was investigated by fluorescence, FTIR, UV-vis spectroscopic and cyclic voltammetric techniques under optimised physiological condition. The fluorescence intensity of BSA is gradually decreased upon addition of TA due to the formation of a BSA-TA complex. The binding parameters were evaluated and their behaviour at different temperatures was analysed. The quenching constants (K sv ) obtained were 2.6 × 10 4 , 2.2 × 10 4 and 2.0 × 10 4  L mol -1 at 288, 298 and 308 K, respectively. The binding mechanism was static-type quenching. The values of ΔH° and ΔS° were found to be 26.87 kJ mol -1 and 21.3 J K -1  mol -1 , and indicated that electrostatic interaction was the principal intermolecular force. The changes in the secondary structure of BSA upon interaction with TA were confirmed by synchronous and 3-D spectral results. Site probe studies reveal that TA is located in site I of BSA. The effects of some common metal ions on binding of BSA-TA complex were also investigated.

A novel voltammetric sensor based on carbon nanotubes and nanoparticles of antimony tin oxide for the determination of ractopamine

Energy Technology Data Exchange (ETDEWEB)

Baytak, Aysegul Kutluay; Teker, Tugce; Duzmen, Sehriban; Aslanoglu, Mehmet, E-mail: maslanoglu@harran.edu.tr

2016-02-01

An electrochemical sensor was prepared by the modification of a glassy carbon electrode (GCE) with carbon nanotubes (CNTs) and nanoparticles of antimony tin oxide (ATO). The surface layer was characterized by scanning electron microscopy (SEM), energy dispersive X-ray diffraction method (EDX) and ATR FT-IR spectroscopy. The proposed electrode was assessed in respect to the electro-oxidation of ractopamine. Compared with a bare GCE and a GCE electrode modified with CNTs, the ATONPs/CNTs/GCE exhibited a great catalytic activity towards the oxidation of ractopamine with a well-defined anodic peak at 600 mV. The current response was linear with the concentration of ractopamine over the range from 10 to 240 nM with a detection limit of 3.3 nM. The proposed electrode enabled the selective determination of ractopamine in the presence of high concentrations of ascorbic acid (AA), dopamine (DA) and uric acid (UA). The proposed electrode was successfully applied for the determination of ractopamine in feed and urine samples. The sensitive and selective determination of ractopamine makes the developed method of great interest for monitoring its therapeutic use and doping control purposes. - Highlights: • A novel voltammetric sensor was prepared using nanoparticles of ATO and CNTs. • The ATONPs/CNTs/GCE has greatly improved the voltammetry of ractopamine. • The proposed electrode enabled a detection limit of 3.3 nM. • AA, DA and UA did not interfere with the selective detection of ractopamine. • Measurements were precise and accurate.

A novel voltammetric sensor based on carbon nanotubes and nanoparticles of antimony tin oxide for the determination of ractopamine

International Nuclear Information System (INIS)

Baytak, Aysegul Kutluay; Teker, Tugce; Duzmen, Sehriban; Aslanoglu, Mehmet

2016-01-01

An electrochemical sensor was prepared by the modification of a glassy carbon electrode (GCE) with carbon nanotubes (CNTs) and nanoparticles of antimony tin oxide (ATO). The surface layer was characterized by scanning electron microscopy (SEM), energy dispersive X-ray diffraction method (EDX) and ATR FT-IR spectroscopy. The proposed electrode was assessed in respect to the electro-oxidation of ractopamine. Compared with a bare GCE and a GCE electrode modified with CNTs, the ATONPs/CNTs/GCE exhibited a great catalytic activity towards the oxidation of ractopamine with a well-defined anodic peak at 600 mV. The current response was linear with the concentration of ractopamine over the range from 10 to 240 nM with a detection limit of 3.3 nM. The proposed electrode enabled the selective determination of ractopamine in the presence of high concentrations of ascorbic acid (AA), dopamine (DA) and uric acid (UA). The proposed electrode was successfully applied for the determination of ractopamine in feed and urine samples. The sensitive and selective determination of ractopamine makes the developed method of great interest for monitoring its therapeutic use and doping control purposes. - Highlights: • A novel voltammetric sensor was prepared using nanoparticles of ATO and CNTs. • The ATONPs/CNTs/GCE has greatly improved the voltammetry of ractopamine. • The proposed electrode enabled a detection limit of 3.3 nM. • AA, DA and UA did not interfere with the selective detection of ractopamine. • Measurements were precise and accurate.

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

Science.gov (United States)

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.

Voltammetric electronic tongue and support vector machines for identification of selected features in Mexican coffee.

Science.gov (United States)

Domínguez, Rocio Berenice; Moreno-Barón, Laura; Muñoz, Roberto; Gutiérrez, Juan Manuel

2014-09-24

This paper describes a new method based on a voltammetric electronic tongue (ET) for the recognition of distinctive features in coffee samples. An ET was directly applied to different samples from the main Mexican coffee regions without any pretreatment before the analysis. The resulting electrochemical information was modeled with two different mathematical tools, namely Linear Discriminant Analysis (LDA) and Support Vector Machines (SVM). Growing conditions (i.e., organic or non-organic practices and altitude of crops) were considered for a first classification. LDA results showed an average discrimination rate of 88% ± 6.53% while SVM successfully accomplished an overall accuracy of 96.4% ± 3.50% for the same task. A second classification based on geographical origin of samples was carried out. Results showed an overall accuracy of 87.5% ± 7.79% for LDA and a superior performance of 97.5% ± 3.22% for SVM. Given the complexity of coffee samples, the high accuracy percentages achieved by ET coupled with SVM in both classification problems suggested a potential applicability of ET in the assessment of selected coffee features with a simpler and faster methodology along with a null sample pretreatment. In addition, the proposed method can be applied to authentication assessment while improving cost, time and accuracy of the general procedure.

Voltammetric determination of Zn(II in Zn-Fe alloy electroplating baths using square-wave voltammetry

Directory of Open Access Journals (Sweden)

Favaron Regiane

2001-01-01

Full Text Available A routine analytical method for zinc (II determination in Zn-Fe alloy galvanic baths was developed employing square-wave voltammetry with the static mercury drop electrode (SMDE as working electrode. Real alloy bath samples were analyzed by the standard addition method and recovery tests were undertaken. The supporting electrolytes used in the analyses were 1.0 mol L-1 NH3 / 0.2 mol L-1 NH4Cl or 0.1 mol L-1 citric acid (pH=3, presenting peak potentials for zinc (II, respectively, at -1.30 V and -0.99 V vs. Ag|AgCl (saturated KCl. The proposed voltammetric method showed a linear response range at 25 °C between 1.0 x 10-5 and 2.2 x 10-4 mol L-1 for zinc (II, in both electrolytes studied. The interference levels for some metals, such as Cu (II, Pb (II, Cr (III and Mn (II, which could prejudice Zn-Fe alloy deposition, were evaluated. These ions did not present significant degrees of interference in the zinc (II determination. The zinc (II recovery tests for the proposed method exhibited a good agreement with the reference method, showing relative errors lower than 3.0%.

A graphene-based label-free voltammetric immunosensor for sensitive detection of the egg allergen ovalbumin.

Science.gov (United States)

Eissa, Shimaa; L'Hocine, Lamia; Siaj, Mohamed; Zourob, Mohammed

2013-08-07

A graphene-based label-free voltammetric immunosensor for the sensitive detection of the egg white allergen ovalbumin has been developed. Graphene-modified screen printed carbon electrodes have been covalently functionalized using electrochemical reduction of in situ generated aryl diazonium salt forming a carboxyphenyl film on the graphene surface. The blocking property of the carboxyphenyl film grafted on to the graphene electrodes using different cyclic voltammetry cycles has been characterized using differential pulse voltammetry in [Fe(CN)6](3-/4-) solution. Then, the terminal carboxylic groups on the graphene surface were activated using EDC/NHS and used to immobilize the ovalbumin antibody and construct the immunosensor. The fabrication steps of the immunosensor have also been characterized using differential pulse voltammetry. The decrease in the [Fe(CN)6](3-/4-) reduction peak current after the immunochemical reaction with ovalbumin has been used for the ovalbumin detection. The developed immunosensor has been used for ovalbumin detection in the concentration range of 1 pg mL(-1) to 0.5 μg mL(-1) with a detection limit of 0.83 pg mL(-1) in PBS buffer. The food matrix effect studied with ovalbumin spiked cake extract showed a good percentage of recovery, indicating the possible applicability of the developed immunosensor in real food samples.

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

Directory of Open Access Journals (Sweden)

Fathali Gholami-Orimi

2012-01-01

Full Text Available 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.

Polyaniline Langmuir-Blodgett film modified glassy carbon electrode as a voltammetric sensor for determination of Ag+ ions

International Nuclear Information System (INIS)

Liu Qiongyan; Wang Fei; Qiao Yonghui; Zhang Shusheng; Ye Baoxian

2010-01-01

A highly sensitive electrochemical sensor made of a glassy carbon electrode (GCE) coated with a Langmuir-Blodgett film (LB) containing polyaniline (PAn) doped with p-toluenesulfonic acid (PTSA) (LB/PAn-PTSA/GCE) has been used for the detection of trace concentrations of Ag + . UV-vis absorption spectra indicated that the PAn was doped by PTSA. The surface morphology of the PAn LB film was characterized by atomic force microscopy (AFM). The electrochemical properties of this LB/PAn-PTSA/GCE were studied using electrochemical impedance spectroscopy (EIS) and cyclic voltammetry. The LB/PAn-PTSA/GCE was used as a voltammetric sensor for determination of trace Ag + at pH 5.0 using linear scanning stripping voltammetry. Under the optimal experimental conditions, the stripping current was proportional to the Ag + concentration over the range from 6.0 x 10 -10 mol L -1 to 1.0 x 10 -6 mol L -1 , with a detection limit of 4.0 x 10 -10 mol L -1 . The high sensitivity, selectivity, and stability of this LB/PAn-PTSA/GCE also demonstrated its practical utility for simple, rapid and economical determination of Ag + in water samples.

Molecular modeling of the voltammetric oxidation at a glassy carbon electrode of the antimalarial drug primaquine and its prodrugs succinylprimaquine and maleylprimaquine

Energy Technology Data Exchange (ETDEWEB)

La-Scalea, Mauro A [Lapen, Laboratorio de Planejamento e Sintese de Quimioterapicos Potencialmente Ativos Contra Endemias Tropicais, Departamento de Farmacia, Faculdade de Ciencias Farmaceuticas, Universidade de Sao Paulo, Av. Prof. Lineu Prestes, 580 Bl. 13 sup., 05508-900 Sao Paulo (Brazil); Menezes, Carla M.S. [Lapen, Laboratorio de Planejamento e Sintese de Quimioterapicos Potencialmente Ativos Contra Endemias Tropicais, Departamento de Farmacia, Faculdade de Ciencias Farmaceuticas, Universidade de Sao Paulo, Av. Prof. Lineu Prestes, 580 Bl. 13 sup., 05508-900 Sao Paulo (Brazil); Matsutami, Guilherme C [Lapen, Laboratorio de Planejamento e Sintese de Quimioterapicos Potencialmente Ativos Contra Endemias Tropicais, Departamento de Farmacia, Faculdade de Ciencias Farmaceuticas, Universidade de Sao Paulo, Av. Prof. Lineu Prestes, 580 Bl. 13 sup., 05508-900 Sao Paulo (Brazil); Polli, Michelle C [Lapen, Laboratorio de Planejamento e Sintese de Quimioterapicos Potencialmente Ativos Contra Endemias Tropicais, Departamento de Farmacia, Faculdade de Ciencias Farmaceuticas, Universidade de Sao Paulo, Av. Prof. Lineu Prestes, 580 Bl. 13 sup., 05508-900 Sao Paulo (Brazil); Serrano, Silvia H.P. [Departamento de Quimica Fundamental, Instituto de Quimica, Universidade de Sao Paulo, Av. Prof. Lineu Prestes, 748 Bl. 2 sup., 05508-90 Sao Paulo (Brazil); Ferreira, Elizabeth I [Lapen, Laboratorio de Planejamento e Sintese de Quimioterapicos Potencialmente Ativos Contra Endemias Tropicais, Departamento de Farmacia, Faculdade de Ciencias Farmaceuticas, Universidade de Sao Paulo, Av. Prof. Lineu Prestes, 580 Bl. 13 sup., 05508-900 Sao Paulo (Brazil)

2006-07-15

The 8-aminoquinoline primaquine (PQ) is the only antimalarial drug used as tissue schizonticide and relapsing malaria. Antichagasic activity was also reported. Nevertheless, as it also shows serious side effects, prodrugs such as succinyl and maleyl derivatives have been proposed to decrease its toxicity. Although PQ mechanism of action has not been completely elucidated, the promotion of oxidative stress is an advanced hypothesis that could explain its activity in both plasmodia and trypanosome parasites. The oxidation of PQ and its prodrugs, maleylprimaquine (MPQ) and succinylprimaquine (SPQ), was studied by cyclic voltammetry using glassy carbon electrode. All compounds were oxidized in aqueous medium, with the charge transfer process being pH-dependent in acidic medium and pH-independent in a weak basic medium, being the neutral form more easily oxidized. This indicated that the protonation of the nitrogen atoms displays a determinant role in the voltammetric oxidation, being both prodrugs more easily oxidized than PQ protonated forms, in the order: SPQ < MPQ < PQ. For a better understanding of this behavior, a molecular modeling study was performed using the AM1 semi-empirical method from Spartan 04 for Linux (v.119, Wavefunction Inc.). The medium pH showed to be fundamental not only to the electronic density of the quinoline ring but also to the rearrangement of the nitrogen side chain. The electronic density of primaquine non-protonated quinoline ring is higher than that in its protonated and diprotonated species. Also, the use of prodrugs and the degree of saturation of the carriers (maleic or succinic acid) interfere with this feature. SPQ and MPQ have a slight increase in the quinoline electronic density in comparison to PQ. Nevertheless, the carrier in the side chain of SPQ is closer to the quinoline ring than it is in MPQ, which accounts for the higher electronic density in the former. The most significant effect occurs in the correspondent protonated

Molecular modeling of the voltammetric oxidation at a glassy carbon electrode of the antimalarial drug primaquine and its prodrugs succinylprimaquine and maleylprimaquine

International Nuclear Information System (INIS)

La-Scalea, Mauro A.; Menezes, Carla M.S.; Matsutami, Guilherme C.; Polli, Michelle C.; Serrano, Silvia H.P.; Ferreira, Elizabeth I.

2006-01-01

The 8-aminoquinoline primaquine (PQ) is the only antimalarial drug used as tissue schizonticide and relapsing malaria. Antichagasic activity was also reported. Nevertheless, as it also shows serious side effects, prodrugs such as succinyl and maleyl derivatives have been proposed to decrease its toxicity. Although PQ mechanism of action has not been completely elucidated, the promotion of oxidative stress is an advanced hypothesis that could explain its activity in both plasmodia and trypanosome parasites. The oxidation of PQ and its prodrugs, maleylprimaquine (MPQ) and succinylprimaquine (SPQ), was studied by cyclic voltammetry using glassy carbon electrode. All compounds were oxidized in aqueous medium, with the charge transfer process being pH-dependent in acidic medium and pH-independent in a weak basic medium, being the neutral form more easily oxidized. This indicated that the protonation of the nitrogen atoms displays a determinant role in the voltammetric oxidation, being both prodrugs more easily oxidized than PQ protonated forms, in the order: SPQ < MPQ < PQ. For a better understanding of this behavior, a molecular modeling study was performed using the AM1 semi-empirical method from Spartan 04 for Linux (v.119, Wavefunction Inc.). The medium pH showed to be fundamental not only to the electronic density of the quinoline ring but also to the rearrangement of the nitrogen side chain. The electronic density of primaquine non-protonated quinoline ring is higher than that in its protonated and diprotonated species. Also, the use of prodrugs and the degree of saturation of the carriers (maleic or succinic acid) interfere with this feature. SPQ and MPQ have a slight increase in the quinoline electronic density in comparison to PQ. Nevertheless, the carrier in the side chain of SPQ is closer to the quinoline ring than it is in MPQ, which accounts for the higher electronic density in the former. The most significant effect occurs in the correspondent protonated

Voltammetric sensing of paracetamole, dopamine and 4-aminophenol at a glassy carbon electrode coated with gold nanoparticles and an organophillic layered double hydroxide

International Nuclear Information System (INIS)

Yin, H.; Shang, K.; Meng, X.; Ai, S.

2011-01-01

A differential pulse voltammetric method was developed for the simultaneous determination of paracetamole, 4-aminophenol and dopamine at pH 7.0 using a glassy carbon electrode (GCE) coated with gold nanoparticles (AuNPs) and a layered double hydroxide sodium modified with dodecyl sulfate (SDS-LDH). The modified electrode displays excellent redox activity towards paracetamole, and the redox current is increased (and the corresponding over-potential decreased) compared to those of the bare GCE, the AuNPs-modified GCE, and the SDS-LDH-modified GCE. The modified electrode enables the determination of paracetamole in the concentration range from 0.5 to 400 μM, with a detection limit of 0.13 μM (at an S/N of 3). The sensor was successfully applied to the simultaneous determination of paracetamole and dopamine, and of paracetamole and 4-aminophenol, respectively, in pharmaceutical tablets and in spiked human serum samples. (author)

Sensors properties of an alkylamine-intercalated kaolinite material towards the voltammetric preconcentration of [Ru(CN)6]4- at a clay-modified electrode

Energy Technology Data Exchange (ETDEWEB)

Tonle, I.K. [Ottawa Univ., ON (Canada). Dept. of Chemistry, Center for Catalysis Research and Innovation; Yanoude Univ. (Cameroon). Laboratoire de Chimie Analytique, Faculte des Sciences; Dschang Univ. (Cameroon). Dept. de Chimie; Bouwe, B.; Rose, G.; Ngameni, E. [Yanoude Univ. (Cameroon). Laboratoire de Chimie Analytique, Faculte des Sciences; Detellier, C. [Yanoude Univ. (Cameroon). Laboratoire de Chimie Analytique, Faculte des Sciences

2008-07-01

This study discussed the sensor properties of a kaolinite material in relation to the voltammetric preconcentration of ruthenium (Ru) anions in a clay-modified electrode. An organoclay was intercalated at room temperature with a layer of hexylamine. Dimethylsulfoxide (DMSO) was intercalated between the clay layers and displaced in wet conditions by the akylamine. The modified clay was then characterized using X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR). The analyses confirmed the incorporation of the hexylamine between the kaolinite platelets. The organokaolinite was then studied for use as a preconcentration agent when coated on the active surface of a glassy carbon electrode for the accumulation of [Ru(CN)6]4- anions in a hydrochloric acid medium. Factors that influenced the conductivity of the film and the diffusion of the electroactive species within the film included the concentration of the electrolyte, and the redox probe. The study showed that kaolinite can be used as a material in electrochemical sensors.

Electrochemical maps and movies of the hydrogen evolution reaction on natural crystals of molybdenite (MoS2): basal vs. edge plane activity† †Electronic supplementary information (ESI) available: Movies S1 to S4: spatially resolved LSV-SECCM movies obtained from the electrocatalytic HER on the surface of bulk MoS2. Fig. S1 to S14: XRD, XPS, Raman, SEM and OM characterization of MoS2; SEM images of the nanopipets; WCA measurements; LSVs and Tafel plots obtained from the HER on MoS2. See DOI: 10.1039/c7sc02545a Click here for additional data file. Click here for additional data file. Click here for additional data file. Click here for additional data file. Click here for additional data file.

Science.gov (United States)

Kang, Minkyung; Maddar, Faduma M.; Li, Fengwang; Walker, Marc; Zhang, Jie

2017-01-01

Two dimensional (2D) semiconductor materials, such as molybdenum disulfide (MoS2) have attracted considerable interest in a range of chemical and electrochemical applications, for example, as an abundant and low-cost alternative electrocatalyst to platinum for the hydrogen evolution reaction (HER). While it has been proposed that the edge plane of MoS2 possesses high catalytic activity for the HER relative to the “catalytically inert” basal plane, this conclusion has been drawn mainly from macroscale electrochemical (voltammetric) measurements, which reflect the “average” electrocatalytic behavior of complex electrode ensembles. In this work, we report the first spatially-resolved measurements of HER activity on natural crystals of molybdenite, achieved using voltammetric scanning electrochemical cell microscopy (SECCM), whereby pixel-resolved linear-sweep voltammogram (LSV) measurements have allowed the HER to be visualized at multiple different potentials to construct electrochemical flux movies with nanoscale resolution. Key features of the SECCM technique are that characteristic surface sites can be targeted and analyzed in detail and, further, that the electrocatalyst area is known with good precision (in contrast to many macroscale measurements on supported catalysts). Through correlation of the local voltammetric response with information from scanning electron microscopy (SEM) and atomic force microscopy (AFM) in a multi-microscopy approach, it is demonstrated unequivocally that while the basal plane of bulk MoS2 (2H crystal phase) possesses significant activity, the HER is greatly facilitated at the edge plane (e.g., surface defects such as steps, edges or crevices). Semi-quantitative treatment of the voltammetric data reveals that the HER at the basal plane of MoS2 has a Tafel slope and exchange current density (J 0) of ∼120 mV per decade and 2.5 × 10–6 A cm–2 (comparable to polycrystalline Co, Ni, Cu and Au), respectively, while the edge

Redox cycling with facing interdigitated array electrodes as a method for selective detection of redox species

NARCIS (Netherlands)

Dam, T.V.A.; Olthuis, Wouter; van den Berg, Albert

2007-01-01

A pair of interdigitated ultramicroelectrodes (UMEs) is used to electrochemically detect a weak reductor ( dopamine) in the presence of a stronger one (K-4[ Fe(CN)(6)]). In the mixture of both reductors, one of the two interdigitated electrodes ( the generator electrode) is used to oxidize both

Elucidation of the Mechanism of Redox Grafting of Diazotated Anthraquinone

DEFF Research Database (Denmark)

Chernyy, Sergey; Bousquet, Antoine; Torbensen, Kristian

2012-01-01

. Scanning electrochemical microscopy was used to study the relationship between the conductivity of thefilm and the charging level of the AQ redox units in the grafted film. For that purpose, approach curves were recorded at a platinum ultramicroelectrode for AQ-containing films on gold and glassy carbon...

A novel label-free voltammetric immunosensor for the detection of {alpha}-fetoprotein using functional titanium dioxide nanoparticles

Energy Technology Data Exchange (ETDEWEB)

Liang Wenbin [Chongqing Key Laboratory of Analytical Chemistry, College of Chemistry and Chemical Engineering, Southwest University, Chongqing 400715 (China); Yuan Ruo [Chongqing Key Laboratory of Analytical Chemistry, College of Chemistry and Chemical Engineering, Southwest University, Chongqing 400715 (China)], E-mail: yuanruo@swu.edu.cn; Chai Yaqin; Li Yan; Zhuo Ying [Chongqing Key Laboratory of Analytical Chemistry, College of Chemistry and Chemical Engineering, Southwest University, Chongqing 400715 (China)

2008-01-01

A highly sensitive label-free voltammetric immunosensor was developed based on the functional titanium dioxide nanoparticles (PV-NTiP), which was prepared by capping 1,1'-bis-(2-phosphonoethyl)-4,4'-bipyridinium dibromide (PV) on the surface of the titanium dioxide nanoparticles (NTiP) with covalent attachment. The PV-NTiP has prominent biocompatibility, good electron transfer ability, primarily excellent adsorption, large specific surface area and positively charged environment. As a result, the negatively charged gold nanoparticles (NGP) could be adsorbed on the PV-NTiP modified electrode surface by electrostatic adsorption, and then to immobilize {alpha}-1-fetoprotein antibody (anti-AFP) for the assay of {alpha}-1-fetoprotein (AFP). The fabricated procedures and electrochemical behaviors of the immunosensor were characterized by electrochemical impedance spectroscopy (EIS), scanning electron microscopy (SEM) and cyclic voltammetry (CV). The anti-AFP/NGP/PV-NTiP modified electrode was sensitive to AFP in linear relation between 1.25 and 200 ng/mL with the correlation coefficient of 0.9982, and the detection limit (S/N = 3) is 0.6 ng/mL under the optimal conditions. In addition, the proposed immunosensor exhibits good sensitivity, selectivity, stability and long-term maintenance of bioactivity and it may be used to immobilize other biomoleculars to develop biosensor for the detection of other antigens or biocompounds.

Redox cycling with facing interdigitated array electrodes as a method for selective detection of redox species

NARCIS (Netherlands)

Dam, V.A.T.; Olthuis, W.; Berg, van den A.

2007-01-01

A pair of interdigitated ultramicroelectrodes (UMEs) is used to electrochemically detect a weak reductor (dopamine) in the presence of a stronger one (K4[Fe(CN)6]). In the mixture of both reductors, one of the two interdigitated electrodes (the generator electrode) is used to oxidize both species at

Electrodeposition of uranium and transuranic metals (Pu) on solid cathode

International Nuclear Information System (INIS)

Laplace, A. F.; Lacquement, J.; Willitt, J. L.; Finch, R. A.; Fletcher, G. A.; Williamson, M. A.

2008-01-01

The results from a study of U and Pu metal electrodeposition from molten eutectic LiCl-KCl on a solid inert cathode are presented. This study has been conducted using ∼ to 50 g of U-Pu together with rare earths (mostly Nd) and 1.5 kg of salt. The introduction of a three-electrode probe with an Ag/AgCl reference electrode has allowed voltammetric measurement during electrolysis and control of the cathode potential versus the reference. Cyclic and square-wave voltammetric measurements proved to be very useful tools for monitoring the electrolysis as well as selecting the cathode versus reference potential to maximize the separation between actinides and rare earths. The voltammetric data also highlighted the occurrence of back reactions between the cathode deposit and oxidizing equivalents formed at the anode that remained in the molten salt electrolyte. Any further electrolysis test needs to be conducted continuously and followed by immediate removal of the cathode to minimize those back reactions. (authors)

Simultaneous voltammetric determination of 2-nitrophenol and 4-nitrophenol based on an acetylene black paste electrode modified with a graphene-chitosan composite

International Nuclear Information System (INIS)

Deng, Peihong; Xu, Zhifeng; Li, Junhua

2014-01-01

We describe a simple and sensitive voltammetric method for the simultaneous determination of 2-nitrophenol and 4-nitrophenol. It is based on the use of an acetylene black paste electrode modified with a graphene-chitosan composite film (denoted as Gr-Chit/ABPE). The reduction peak currents of 2-nitrophenol (at −252 mV) and of 4-nitrophenol (at −340 mV) in pH 1.0 solution increase significantly at the Gr-Chit/ABPE in comparison to a bare ABPE. Factors affecting sensitivity were optimized and a linear relationship is found between peak current and the concentrations of 2-nitrophenol (in the 0.4 μM to 80 μM range) and for 4-nitrophenol (in the 0.1 μM to 80 μM range). The detection limits (at an SNR of 3 and after a 30-s accumulation time) are 200 nM for 2-nitrophenol and 80 nM for 4-nitrophenol, respectively. The modified electrode was successfully applied to the direct and parallel determination of 2-nitrophenol and 4-nitrophenol in spiked water samples. (author)

A novel nanostructured composite formed by interaction of copper octa(3-aminopropyl)octasilsesquioxane with azide ligands: Preparation, characterization and a voltammetric application

International Nuclear Information System (INIS)

Ribeiro do Carmo, Devaney; Paim, Leonardo Lataro; Metzker, Gustavo; Dias Filho, Newton Luiz; Stradiotto, Nelson Ramos

2010-01-01

This study presents the preparation, characterization and application of copper octa(3-aminopropyl)octasilsesquioxane following its subsequent reaction with azide ions (ASCA). The precursor (AC) and the novel compound (ASCA) were characterized by Fourier transform infrared spectra (FTIR), nuclear magnetic resonance (NMR), electron paramagnetic resonance (EPR), scanning electronic microscopy (SEM), X-ray diffraction (XRD), Thermogravimetric analyses and voltammetric technique. The cyclic voltammogram of the modified graphite paste electrode with ASCA (GPE-ASCA), showed one redox couple with formal potential (E 1/2 ox ) = 0.30 V and an irreversible process at 1.1 V (vs. Ag/AgCl; NaCl 1.0 M; v=20mVs -1 ). The material is very sensitive to nitrite concentrations. The modified graphite paste electrode (GPE-ASCA) gives a linear range from 1.0 x 10 -4 to 4.0 x 10 -3 mol L -1 for the determination of nitrite, with a detection limit of 2.1 x 10 -4 mol L -1 and the amperometric sensitivity of 8.04 mA/mol L -1 .

Aging time and brand determination of pasteurized milk using a multisensor e-nose combined with a voltammetric e-tongue.

Science.gov (United States)

Bougrini, Madiha; Tahri, Khalid; Haddi, Zouhair; El Bari, Nezha; Llobet, Eduard; Jaffrezic-Renault, Nicole; Bouchikhi, Benachir

2014-12-01

A combined approach based on a multisensor system to get additional chemical information from liquid samples through the analysis of the solution and its headspace is illustrated and commented. In the present work, innovative analytical techniques, such as a hybrid e-nose and a voltammetric e-tongue were elaborated to differentiate between different pasteurized milk brands and for the exact recognition of their storage days through the data fusion technique of the combined system. The Principal Component Analysis (PCA) has shown an acceptable discrimination of the pasteurized milk brands on the first day of storage, when the two instruments were used independently. Contrariwise, PCA indicated that no clear storage day's discrimination can be drawn when the two instruments are applied separately. Mid-level of abstraction data fusion approach has demonstrated that results obtained by the data fusion approach outperformed the classification results of the e-nose and e-tongue taken individually. Furthermore, the Support Vector Machine (SVM) supervised method was applied to the new subset and confirmed that all storage days were correctly identified. This study can be generalized to several beverage and food products where their quality is based on the perception of odor and flavor. Copyright © 2014 Elsevier B.V. All rights reserved.

Studies on sorption of cadmium (II) ions onto Haro river sand from aqueous media using radiotracer and voltammetric techniques

International Nuclear Information System (INIS)

Ahmed, R.; Hasany, S.M.; Yamin, T.; Ansari, M.S.

2006-01-01

Sorption of Cd(II) ions on Haro river sand has been studied using radiotracer technique. The effects of pH and acid concentrations on the sorption were studied. The sorption increases with pH. reaches a maximum at pH 7 and decreases at higher pH values. With acids, it was found that sorption decreases with increasing acid concentration, and for more oxidizing acids sorption was less. Kinetic studies indicate that mostly intra particle diffusion occurs with first order rate constant of 18.45 x 10 -2 min -1 . The sorption data follow the Freundlich and Dubinin-Radushkevich (D-R) isotherms. In addition to the radiotracer method, voltammetric technique was applied and the results by the two techniques are in good agreement. The sorption free energy value indicates that adsorption process is chemisorption. The effect of temperature was studied and values of ΔH, ΔS and ΔG for Cd(II) have been calculated which are 20.15 kJ mol -1 , 74.04 J mol -1 K -1 and -1.754 kJ mol -1 . Adsorption of Cd(II) on Haro river sand is endothermic, spontaneous and entropy driven. The effect of different anions and cations at different concentrations was studied. Levels of cadmium have been monitored in water and sediments. (orig.)

Uniform deposition of water-soluble CdS quantum dots on TiO2 nanotube arrays by cyclic voltammetric electrodeposition: Effectively prevent aggregation and enhance visible-light photocatalytic activity

International Nuclear Information System (INIS)

Zhang, Xiaojiao; Lin, Shiwei; Liao, Jianjun; Pan, Nengqian; Li, Danhong; Cao, Xiankun; Li, Jianbao

2013-01-01

Highlights: • Water-soluble CdS QDs were deposited on the TNTAs by DC electrodeposition, CV electrodeposition, and SILAR. • The CV method could effectively prevent the aggregation and uniformly deposit CdS QDs onto the TNTAs. • The CTAB/CdS/TNTAs prepared by the CV method exhibited superior photoelectrical properties and photocatalytic activity. -- Abstract: Water-soluble CdS quantum dots (QDs) covered with cationic surfactant-cetyltrimethylammonium bromide (CTAB) were deposited on the highly ordered TiO 2 nanotube arrays (TNTAs) by various methods, such as direct current (DC) electrodeposition, cyclic voltammetric (CV) electrodeposition, and successive ionic layer adsorption reaction (SILAR). The morphology measurements show that CTAB capping could well control the QD size and the CV method could effectively prevent the nanoparticle aggregation and uniformly deposit QDs onto TNTAs. Among all the deposition methods studied, the sample prepared by the CV method possesses superior photoelectrical properties and photocatalytic activity. A maximum photoconversion efficiency of 2.81% is achieved for the CdS/TNTAs prepared by CV electrodeposition, which exhibits about 17 times enhancement over the efficiency of the sample prepared by DC electrodeposition. And the photocatalytic degradation of methyl orange under visible-light irradiation demonstrates that the rate constant of the sample prepared by the CV method is almost seven times of that of the untreated TNTAs. Moreover, the underlying mechanism for the improving properties has been discussed

Cyclic voltammetric study of electro-oxidation of methanol on platinum electrode in acidic and neutral media

International Nuclear Information System (INIS)

Khan, A.S.A.; Ahmed, R.; Mirza, M.L.

2007-01-01

The electro-oxidation of methanol on electrochemically treated platinum foil was investigated in acidic and neutral media for comparison of cyclic voltammetric characteristics and elucidation of mechanism of electro-oxidation of methanol. The surface area and roughness factor of platinum electrode was calculated. The electro-oxidation of mathanol is an irreversible process giving. anodic peaks in both anodic and cathodic sweep. The characteristic peaks of electrooxidation of methanol appeared at almost the same potential region in both acidic and neutral media. In neutral medium, certain additional cathodic/anodic peaks appeared which were confirmed to arise by the reduction/oxidation of hydrogen ions. The exchange current density and heterogeneous electron transfer rate constant was higher in neutral medium as. compared with acidic medium. The thermodynamic parameters delta H, delta S, and delta G/sub 298/ were calculated. The values of delta H and delta G/sub 298/were positive which indicated that the process of electro-oxidation of methanol is an endothermic and nonspontaneous. The mechanism of electro-oxidation of methanol was same in both acidic and neutral media involving the formation of various adsorbed intermediate species through dissociative adsorption steps leading to the formation of Co adsorbed radicals, which are removed. during interaction with adsorbed hydrous oxides provided by the oxidation of adsorbed water molecules. The higher rate of electro-oxidation of methanol in neutral medium was interpreted in the tight of electrochemical mechanism and was attributed to the presence of comparatively small amount of hydrogen ions only along the surface of working electrode, which are produced during electro-oxidation of methanol. (author)

Adsorptive stripping voltammetric determination of nitroimidazole derivative on multiwalled carbon nanotube modified electrodes: influence of size and functionalization of nanotubes

Energy Technology Data Exchange (ETDEWEB)

Jara-Ulloa, Paola; Canete-Rosales, Paulina; Nunez-Vergara, Luis J; Squella, Juan A., E-mail: asquella@ciq.uchile.c [University of Chile, Santiago (Chile). Chemical and Pharmaceutical Sciences Faculty. Bioelectrochemistry Lab.

2011-07-01

1-Methyl-4-nitro-2-bromine methylimidazole (4-NimMeBr), was electrochemically reduced on mercury, glassy carbon and multiwalled carbon nanotubes (MWCNT) modified electrodes. 4-NimMeBr was adsorbed on the MWCNT modified electrode thus permitting the implementation of an adsorptive stripping voltammetric (ASV) method. We have used 4-NimMeBr as a prototype electroactive nitro compound to study the effect of both the size of the nanotubes and its functionalization by oxidation. The oxidized MWCNT forms better dispersions than the non-oxidized, producing electrode surface with higher density of MWCNT as was determined by electrochemical mapping using scanning electrochemical microscopy (SECM). Under the optimized conditions, the peak current was proportional to the concentration of 4-NimMeBr in the range of 10{sup -6} mol L{sup -1} to 10{sup -4} mol L{sup -1} with detection and quantification limits of 4.41 x 10{sup -6} mol L{sup -1} and 6.21 x 10{sup -6} mol L{sup -1}, respectively. The sensibility of bare electrode was 0.01 {mu}A per mmol L{sup -1}, which was lower than the value of 5.34 and 6.97 mA per mmol L{sup -1} obtained using short and large oxidized MWCNT, respectively. (author)

Layer-by-Layer-Assembled AuNPs-Decorated First-Generation Poly(amidoamine) Dendrimer with Reduced Graphene Oxide Core as Highly Sensitive Biosensing Platform with Controllable 3D Nanoarchitecture for Rapid Voltammetric Analysis of Ultratrace DNA Hybridization.

Science.gov (United States)

Jayakumar, Kumarasamy; Camarada, María Belén; Dharuman, Venkataraman; Rajesh, Rajendiran; Venkatesan, Rengarajan; Ju, Huangxian; Maniraj, Mahalingam; Rai, Abhishek; Barman, Sudipta Roy; Wen, Yangping

2018-06-12

The structure and electrochemical properties of layer-by-layer-assembled gold nanoparticles (AuNPs)-decorated first-generation (G1) poly(amidoamine) dendrimer (PD) with reduced graphene oxide (rGO) core as a highly sensitive and label-free biosensing platform with a controllable three-dimensional (3D) nanoarchitecture for the rapid voltammetric analysis of DNA hybridization at ultratrace levels were characterized. Mercaptopropinoic acid (MPA) was self-assembled onto Au substrate, then GG1PD formed by the covalent functionalization between the amino terminals of G1PD and carboxyl terminals of rGO was covalently linked onto MPA, and finally AuNPs were decorated onto GG1PD by strong physicochemical interaction between AuNPs and -OH of rGO in GG1PD, which was characterized through different techniques and confirmed by computational calculation. This 3D controllable thin-film electrode was optimized and evaluated using [Fe(CN) 6 ] 3-/4- as the redox probe and employed to covalently immobilize thiol-functionalized single-stranded DNA as biorecognition element to form the DNA nanobiosensor, which achieved fast, ultrasensitive, and high-selective differential pulse voltammetric analysis of DNA hybridization in a linear range from 1 × 10 -6 to 1 × 10 -13 g m -1 with a low detection limit of 9.07 × 10 -14 g m -1 . This work will open a new pathway for the controllable 3D nanoarchitecture of the layer-by-layer-assembled metal nanoparticles-functionalized lower-generation PD with two-dimensional layered nanomaterials as cores that can be employed as ultrasensitive and label-free nanobiodevices for the fast diagnosis of specific genome diseases in the field of biomedicine.

Development of a Nafion/MWCNT-SPCE-Based Portable Sensor for the Voltammetric Analysis of the Anti-Tuberculosis Drug Ethambutol

Directory of Open Access Journals (Sweden)

Rosa A. S. Couto

2016-06-01

Full Text Available Herein we describe the development, characterization and application of an electrochemical sensor based on the use of Nafion/MWCNT-modified screen-printed carbon electrodes (SPCEs for the voltammetric detection of the anti-tuberculosis (anti-TB drug ethambutol (ETB. The electrochemical behaviour of the drug at the surface of the developed Nafion/MWCNT-SPCEs was studied through cyclic voltammetry (CV and square wave voltammetry (SWV techniques. Electrochemical impedance spectroscopy (EIS and scanning electron microscopy (SEM were employed to characterize the modified surface of the electrodes. Results showed that, compared to both unmodified and MWCNTs-modified SPCEs, negatively charged Nafion/MWCNT-SPCEs remarkably enhanced the electrochemical sensitivity and selectivity for ETB due to the synergistic effect of the electrostatic interaction between cationic ETB molecules and negatively charged Nafion polymer and the inherent electrocatalytic properties of both MWCNTs and Nafion. Nafion/MWCNT-SPCEs provided excellent biocompatibility, good electrical conductivity, low electrochemical interferences and a high signal-to-noise ratio, providing excellent performance towards ETB quantification in microvolumes of human urine and human blood serum samples. The outcomes of this paper confirm that the Nafion/MWCNT-SPCE-based device could be a potential candidate for the development of a low-cost, yet reliable and efficient electrochemical portable sensor for the low-level detection of this antimycobacterial drug in biological samples.

A square-wave adsorptive stripping voltammetric method for the determination of Amaranth, a food additive dye.

Science.gov (United States)

Alghamdi, Ahmad H

2005-01-01

Square-wave adsorptive stripping voltammetric (AdSV) determinations of trace concentrations of the azo coloring agent Amaranth are described. The analytical methodology used was based on the adsorptive preconcentration of the dye on the hanging mercury drop electrode, followed by initiation of a negative sweep. In a pH 10 carbonate supporting electrolyte, Amaranth gave a well-defined and sensitive AdSV peak at -518 mV. The electroanalytical determination of this azo dye was found to be optimal in carbonate buffer (pH 10) under the following experimental conditions: accumulation time, 120 s; accumulation potential, 0.0 V; scan rate, 600 mV/s; pulse amplitude, 90 mV; and frequency, 50 Hz. Under these optimized conditions the AdSV peak current was proportional over the concentration range 1 x 10(-8)-1.1 x 10(-7) mol/L (r = 0.999) with a detection limit of 1.7 x 10(-9) mol/L (1.03 ppb). This analytical approach possessed enhanced sensitivity, compared with conventional liquid chromatography or spectrophotometry and it was simple and fast. The precision of the method, expressed as the relative standard deviation, was 0.23%, whereas the accuracy, expressed as the mean recovery, was 104%. Possible interferences by several substances usually present as food additive azo dyes (E110, E102), gelatin, natural and artificial sweeteners, preservatives, and antioxidants were also investigated. The developed electroanalyticals method was applied to the determination of Amaranth in soft drink samples, and the results were compared with those obtained by a reference spectrophotometric method. Statistical analysis (paired t-test) of these data showed that the results of the 2 methods compared favorably.

A Fast Strategy for Determination of Vitamin B9 in Food and Pharmaceutical Samples Using an Ionic Liquid-Modified Nanostructure Voltammetric Sensor

Directory of Open Access Journals (Sweden)

Fatemeh Khaleghi

2016-05-01

Full Text Available Vitamin B9 or folic acid is an important food supplement with wide clinical applications. Due to its importance and its side effects in pregnant women, fast determination of this vitamin is very important. In this study we present a new fast and sensitive voltammetric sensor for the analysis of trace levels of vitamin B9 using a carbon paste electrode (CPE modified with 1,3-dipropylimidazolium bromide (1,3-DIBr as a binder and ZnO/CNTs nanocomposite as a mediator. The electro-oxidation signal of vitamin B9 at the surface of the 1,3-DIBr/ZnO/CNTs/CPE electrode appeared at 800 mV, which was about 95 mV less positive compared to the corresponding unmodified CPE. The oxidation current of vitamin B9 by square wave voltammetry (SWV increased linearly with its concentration in the range of 0.08–650 μM. The detection limit for vitamin B9 was 0.05 μM. Finally, the utility of the new 1,3-DIBr/ZnO/CNTs/CPE electrode was tested in the determination of vitamin B9 in food and pharmaceutical samples.

Rapid Voltammetric Measurements at Conducting Polymer Microelectrodes Using Ultralow-Capacitance Poly(3,4-ethylenedioxythiophene):Tosylate

DEFF Research Database (Denmark)

Meier, Adam R.; Matteucci, Marco; Vreeland, Richard F.

2016-01-01

. The adsorption characteristics of dopamine at the polymer electrode were fit to a Langmuir isotherm. The low apparent capacitance and the microlithographic processes for electrode design make PEDOT:tosylate an attractive material for future applications as an implantable biosens9r for FSCV measurements...

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

Science.gov (United States)

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

2014-12-01

Poly(4-aminobenzoic acid)/electrochemically reduced graphene oxide composite film modified glassy carbon electrodes (4-ABA/ERGO/GCEs) were fabricated by a two-step electrochemical method. The electrochemical behavior of acetaminophen at the modified electrode was investigated by means of cyclic voltammetry. The results indicated that 4-ABA/ERGO composite films possessed excellent electrocatalytic activity towards the oxidation of acetaminophen. The electrochemical reaction of acetaminophen at 4-ABA/ERGO/GCE is proved to be a surface-controlled process involving the same number of protons and electrons. The voltammetric determination of acetaminophen performed with the 4-ABA/ERGO modified electrode presents a good linearity in the range of 0.1-65 μM with a low detection limit of 0.01 μM (S/N=3). In the case of using the 4-ABA/ERGO/GCE, acetaminophen and dopamine can be simultaneously determined without mutual interference. Furthermore, the 4-ABA/ERGO/GCE has good reproducibility and stability, and can be used to determine acetaminophen in tablets. Copyright © 2014 Elsevier B.V. All rights reserved.

Simultaneous voltammetric determination of tramadol and acetaminophen using carbon nanoparticles modified glassy carbon electrode

International Nuclear Information System (INIS)

Ghorbani-Bidkorbeh, Fatemeh; Shahrokhian, Saeed; Mohammadi, Ali; Dinarvand, Rassoul

2010-01-01

A sensitive and selective electrochemical sensor was fabricated via the drop-casting of carbon nanoparticles (CNPs) suspension onto a glassy carbon electrode (GCE). The application of this sensor was investigated in simultaneous determination of acetaminophen (ACE) and tramadol (TRA) drugs in pharmaceutical dosage form and ACE determination in human plasma. In order to study the electrochemical behaviors of the drugs, cyclic and differential pulse voltammetric studies of ACE and TRA were carried out at the surfaces of the modified GCE (MGCE) and the bare GCE. The dependence of peak currents and potentials on pH, concentration and the potential scan rate were investigated for these compounds at the surface of MGCE. Atomic force microscopy (AFM) was used for the characterization of the film modifier and its morphology on the surface of GCE. The results of the electrochemical investigations showed that CNPs, via a thin layer model based on the diffusion within a porous layer, enhanced the electroactive surface area and caused a remarkable increase in the peak currents. The thin layer of the modifier showed a catalytic effect and accelerated the rate of the electron transfer process. Application of the MGCE resulted in a sensitivity enhancement and a considerable decrease in the anodic overpotential, leading to negative shifts in peak potentials. An optimum electrochemical response was obtained for the sensor in the buffered solution of pH 7.0 and using 2 μL CNPs suspension cast on the surface of GCE. Using differential pulse voltammetry, the prepared sensor showed good sensitivity and selectivity for the determination of ACE and TRA in wide linear ranges of 0.1-100 and 10-1000 μM, respectively. The resulted detection limits for ACE and TRA was 0.05 and 1 μM, respectively. The CNPs modified GCE was successfully applied for ACE and TRA determinations in pharmaceutical dosage forms and also for the determination of ACE in human plasma.

Silver ion imprinted polymer nanobeads based on a aza-thioether crown containing a 1,10-phenanthroline subunit for solid phase extraction and for voltammetric and potentiometric silver sensors

Energy Technology Data Exchange (ETDEWEB)

Shamsipur, Mojtaba, E-mail: mshamsipur@yahoo.com [Department of Chemistry, Razi University, Kermanshah (Iran, Islamic Republic of); Hashemi, Beshare; Dehdashtian, Sara; Mohammadi, Moslem; Gholivand, Mohammad Bagher [Department of Chemistry, Razi University, Kermanshah (Iran, Islamic Republic of); Garau, Alessandra; Lippolis, Vito [Dipartimento di Scienze Chimiche e Geologiche, Universita' degli Studi di Cagliari, S.S. 554 Bivio per Sestu, 09042 Monserrato, CA (Italy)

2014-12-10

Highlights: • Preparation of Ag{sup +} imprinted polymeric nanobeads via precipitation polymerization. • Use of a mixed aza-thioether crown containing a 1,10-phenanthroline subunit a selective host for Ag{sup +} ion. • Highly selective, sensitive and fast recognition of traces of Ag{sup +} ions. • Use of the prepared Ag{sup +}-IIP for preparation of an Ag{sup +}-voltammetric sensor with LOD of 9.0 × 10{sup −10} M. • Use of the prepared Ag{sup +}-IIP for preparation of Ag{sup +}-ISEs with LOD of 1.2 × 10{sup −9} M 9.0 × 10{sup −10} M. - Abstract: A new nano-sized silver(I) ion-imprinted polymer (IIP) was prepared via precipitation copolymerization using ethyleneglycol dimethacrylate, as a cross-linking agent in the presence of Ag{sup +} and an aza-thioether crown containing a 1,10-phenanthroline subunit as a highly selective complexing agent. The imprint silver(I) ion was removed from the polymeric matrix using a 1.0 M HNO{sub 3} solution. The resulting powder material was characterized using IR spectroscopy and scanning electron microscopy. The SEM micrographs showed colloidal nanoparticles of about 52 nm and 75 nm in diameter and slightly irregular in shape for leached and unleached IIPs, respectively. The optimal pH for quantitative enrichment was 6.0 and maximum sorbent capacity of the prepared IIP for Ag{sup +} was 18.08 μmol g{sup −1}. The relative standard deviation and limit of detection (LOD = 3S{sub b}/m) for flame atomic absorption spectrometric determination of silver(I) ion, after its selective extraction by the prepared IIP nanobeads, were evaluated as 2.42% and 2.2 × 10{sup −8} M, respectively. The new Ag{sup +}-IIP was also applied as a suitable sensing element to the preparation of highly selective and sensitive voltammetric and potentiometric sensors for ultra trace detection of silver(I) ion in water samples, with limits of detection of 9.0 × 10{sup −10} and 1.2 × 10{sup −9} M, respectively.

Zanamivir immobilized magnetic beads for voltammetric measurement of neuraminidase at gold-modified boron doped diamond electrode

Energy Technology Data Exchange (ETDEWEB)

Wahyuni, Wulan Tri, E-mail: wulantriws@gmail.com [Department of Chemistry, Faculty of Mathematics and Natural Sciences, Bogor Agricultural University, Kampus IPB Darmaga, Bogor 16680 (Indonesia); Department of Chemistry, FMIPA, Universitas Indonesia, Kampus UI Depok (Indonesia); Ivandini, Tribidasari A.; Saepudin, Endang [Department of Chemistry, FMIPA, Universitas Indonesia, Kampus UI Depok (Indonesia); Einaga, Yasuaki [Department of Chemistry, Faculty of Science and Technology, Keio University, Hiyoshi 3-14-1, Yokohama 223-8522 (Japan); CREST, JST, 3-14-1 Hiyoshi, Yokohama 223-8522 (Japan)

2016-04-19

Biomolecule modified magnetic beads has been widely used in separation and sensing process. This study used streptavidin modified magnetic beads to immobilize biotin modified zanamivir. Biotin-streptavidin affinity facilitates immobilization of zanamivir on magnetic beads. Then interaction of zanamivir and neuraminidase was adopted as basic for enzyme detection. Detection of neuraminidase was performed at gold modified BDD using cyclic voltammetry technique. The measurement was carried out based on alteration of electrochemical signals of working electrode as neuraminidase response. The result showed that zanamivir was successfully immobilized on magnetic beads. The optimum amount of magnetic beads for zanamivir immobilization was 120 ug. Linear responses of neuraminidase were detected in concentration range of 0-15 mU. Detection limit (LOD) of measurement was 2.32 mU (R2 = 0.959) with precision as % RSD of 1.41%. Measurement of neuraminidase on magnetic beads could be also performed in the presence of mucin matrix. The linearity range was 0-8 mU with LOD of 0.64 mU (R2 = 0.950) and % RSD of 7.25%.

Electroanalysis of cardioselective beta-adrenoreceptor blocking agent acebutolol by disposable graphite pencil electrodes with detailed redox mechanism

OpenAIRE

Atmanand M. Bagoji; Shreekant M. Patil; Sharanappa T. Nandibewoor

2016-01-01

A simple economic graphite pencil electrode (GPE) was used for analysis of cardioselective, hydrophilic-adrenoreceptor blocking agent, acebutolol (ACBT) using the cyclic voltammetric, linear sweep voltammetric, differential pulse voltammetric (DPV), and square-wave voltammetric (SWV) techniques. The dependence of the current on pH, concentration, and scan rate was investigated to optimize the experimental condition for determination of ACBT. The electrochemical behavior of the ACBT at GPE was...

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.

Science.gov (United States)

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.

Monolayer-protected clusters of gold nanoparticles: impacts of stabilizing ligands on the heterogeneous electron transfer dynamics and voltammetric detection.

Science.gov (United States)

Pillay, Jeseelan; Ozoemena, Kenneth I; Tshikhudo, Robert T; Moutloali, Richard M

2010-06-01

Surface electrochemistry of novel monolayer-protected gold nanoparticles (MPCAuNPs) is described. Protecting ligands, (1-sulfanylundec-11-yl)tetraethylene glycol (PEG-OH) and (1-sulfanylundec-11-yl)poly(ethylene glycol)ic acid (PEG-COOH), of three different percent ratios (PEG-COOH:PEG-OH), 1:99 (MPCAuNP-COOH(1%)), 50:50 (MPCAuNP-COOH(50%)), and 99:1 (MPCAuNP-COOH(99%)), were studied. The electron transfer rate constants (k(et)/s(-1)) in organic medium decreased as the concentration of the surface-exposed -COOH group in the protecting monolayer ligand is increased: MPCAuNP-COOH(1%) (approximately 5 s(-1)) > MPCAuNP-COOH(50%) (approximately 4 s(-1)) > MPCAuNP-COOH(99%) (approximately 0.5 s(-1)). In aqueous medium, the trend is reversed. The surface pK(a) was estimated as approximately 8.2 for the MPCAuNP-COOH(1%), while both MPCAuNP-COOH(50%) and MPCAuNP-COOH(99%) showed two pK(a) values of about 5.0 and approximately 8.0. These results have been interpreted in terms of the quasi-solidity and quasi-liquidity of the terminal -OH and -COOH head groups, respectively. MPCAuNP-COOH(99%) excellently suppressed the voltammetric response of the ascorbic acid but enhanced the electrocatalytic detection of epinephrine compared to the other MPCAuNPs studied. This study reveals important factors that should be considered when designing electrode devices that employ monolayer-protected gold nanoparticles and possibly for some other redox-active metal nanoparticles.

Development of a poly(alizarin red S)/ionic liquid film modified electrode for voltammetric determination of catechol

International Nuclear Information System (INIS)

Zhang, Qing; Pan, Dawei; Zhang, Haiyun; Han, Haitao; Kang, Qi

2014-01-01

Highlights: • This study is the first to conduct electroploymerization of ARS in RTILs. • BMIMBF 4 was successfully mixed in polymeric ARS film. • PARS/BMIMBF 4 film was tighter, smoother and better electrochemical property. • PARS/BMIMBF 4 /GCE showed superior performance for catechol determination. - Abstract: A novel modified electrode for voltammetric catechol determination was fabricated by electroploymerization of alizarin red S (ARS) onto a glassy carbon electrode (GCE) in one kind of room-temperature ionic liquid (1-butyl-3-methylimidazolium tetrafluoroborate, BMIMBF 4 ). The polymeric ARS/ionic liquid (PARS/BMIMBF 4 ) film modified electrode was characterized by using scanning electron microscope (SEM), energy dispersive X-ray spectroscopy (EDX), X-ray photoelectron spectroscopy (XPS), Fourier transform infrared spectroscopy (FTIR) and electrochemical methods. The EDX, XPS and FTIR results indicated that PARS/BMIMBF 4 film was successfully obtained. Compared with the GCE modified by electroploymerization of ARS in aqueous solution, the GCE modified by electroploymerization of ARS in BMIMBF 4 showed smoother and more compact morphology for coating and better electroanalytical properties. Given the combined electrochemical activity of PARS and excellent conductivity of BMIMBF 4 , the PARS/BMIMBF 4 /GCE has been successfully used for catechol determination by differential pulse voltammetry (DPV) with a linear range of 0.10 to 500 μM. The sensitivity and detection limit are 42 nA/μM and 0.026 μM, respectively. The PARS/BMIMBF 4 modified electrode was successfully applied to the determination of catechol in real water samples and may serve as a simple but high-performance sensor for the determination of some environmental pollutants

Combination of the optical waveguide lightmode spectroscopy method with electrochemical measurements

Energy Technology Data Exchange (ETDEWEB)

Szendro, I.; Erdelyi, K.; Fabian, M. [MicroVacuum Ltd., Kerekgyarto u.: 10, H-1147 Budapest (Hungary); Puskas, Zs. [Minvasive Ltd., Goldmann Gy. ter 3., H-1111 Budapest (Hungary); Adanyi, N. [Central Food Research Institute, H-1537 Budapest, P.O.B. 393 (Hungary); Somogyi, K. [MicroVacuum Ltd., Kerekgyarto u.: 10, H-1147 Budapest (Hungary)], E-mail: karoly.somogyi@microvacuum.com

2008-09-30

Optical waveguides are normally sensitive to the surrounding media and also to the surface contaminations. The effective refractive index changes at the surface. Various sensor systems were developed based on this effect. One of the most sensitive and effective methods is the optical waveguide lightmode spectroscopy (OWLS). At the same time, electrochemical methods are widely used both in inorganic and organic chemistry, and also advantages in microbiology were demonstrated. In this work, efforts are made and results are presented for the combination of these two methods for simultaneous measurement of refractive index and electrical current changes caused by the presence of cells/molecules/ions to be investigated. An electrically conductive indium tin oxide (ITO) nanolayer is deposited and activated on the top of the OWLS planar waveguide oxide layer. ITO layers serve as working electrodes in the electrochemical measurements. The basic setup and an integrated system are demonstrated here. Measurements using H{sub 2}O{sub 2}, toluidine blue solutions, and KCl and TRIS solutions as buffer and transport media are represented. Measurements show both the changes detected by the sensor layer and the effect of the applied potential in cyclic and chrono voltammetric measurements. Results demonstrate an effective combination of optical and electrochemical methods.

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

Energy Technology Data Exchange (ETDEWEB)

Shoja, Yalda; Rafati, Amir Abbas, E-mail: aa_rafati@basu.ac.ir; Ghodsi, Javad

2016-01-01

A novel and selective enzymatic biosensor was designed and constructed for voltammetric determination of levodopa (L-Dopa) in aqueous media (phosphate buffer solution, pH = 7). Biosensor development was on the basis of to physically immobilizing of horse radish peroxidase (HRP) as electrochemical catalyst by sol–gel on glassy carbon electrode modified with organic nucleophilic carbon nanotube composite which in this composite p-phenylenediamine (pPDA) as organic nucleophile chemically bonded with functionalized MWCNT (MWCNT-COOH). The results of this study suggest that prepared bioorganic nucleophilic carbon nanotube composite (HRP/MWCNT-pPDA) shows fast electron transfer rate for electro oxidation of L-Dopa because of its high electrochemical catalytic activity toward the oxidation of L-Dopa, more −NH{sub 2} reactive sites and large effective surface area. Also in this work we measured L-Dopa in the presence of folic acid and uric acid as interferences. The proposed biosensor was characterized by scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDX), FT-IR spectroscopy and cyclic voltammetry (CV). The differential pulse voltammetry (DPV) was used for determination of L-Dopa from 0.1 μM to 1.9 μM with a low detection limit of 40 nM (for S/N = 3) and sensitivity was about 35.5 μA/μM. Also this biosensor has several advantages such as rapid response, high stability and reproducibility. - Highlights: • Glassy carbon electrode modified by a novel composite in which pPDA as nucleophile is chemically attached to MWCNTs. • The developed biosensor exhibited excellent electrocatalytic activity in electrochemically determination of L-Dopa. • The biosensor showed acceptable sensitivity, reproducibility, detection limit, selectivity and stability. • MWCNT-pPDA provides a good electrical conductivity and large effective surface area for enzyme immobilization.

Integrated Microanalytical System for Simultaneous Voltammetric Measurements of Free Metal Ion Concentrations in Natural Waters

OpenAIRE

Noël, Stéphane; Tercier-Waeber, Mary-Lou; Lin, Lin; Buffle, Jacques; Guenat, Olivier; Koudelka-Hep, Milena

2007-01-01

A complexing gel integrated microelectrode (CGIME) for direct measurements of free metal ion concentrations in natural waters has been developed. It is prepared by the successive deposition of microlayers of a chelating resin, an antifouling agarose gel and Hg on a 100-interconnected Ir-based microelectrode array. The trace metals of interest are in a first step accumulated on the chelating resin in proportion to their free ion concentration in solution, then released in acidic solution and d...

An Electrochemical Quartz Crystal Microbalance Multisensor System Based on Phthalocyanine Nanostructured Films: Discrimination of Musts

Directory of Open Access Journals (Sweden)

Celia Garcia-Hernandez

2015-11-01

Full Text Available An array of electrochemical quartz crystal electrodes (EQCM modified with nanostructured films based on phthalocyanines was developed and used to discriminate musts prepared from different varieties of grapes. Nanostructured films of iron, nickel and copper phthalocyanines were deposited on Pt/quartz crystals through the Layer by Layer technique by alternating layers of the corresponding phthalocyanine and poly-allylamine hydrochloride. Simultaneous electrochemical and mass measurements were used to study the mass changes accompanying the oxidation of electroactive species present in must samples obtained from six Spanish varieties of grapes (Juan García, Prieto Picudo, Mencía Regadío, Cabernet Sauvignon, Garnacha and Tempranillo. The mass and voltammetric outputs were processed using three-way models. Parallel Factor Analysis (PARAFAC was successfully used to discriminate the must samples according to their variety. Multi-way partial least squares (N-PLS evidenced the correlations existing between the voltammetric data and the polyphenolic content measured by chemical methods. Similarly, N-PLS showed a correlation between mass outputs and parameters related to the sugar content. These results demonstrated that electronic tongues based on arrays of EQCM sensors can offer advantages over arrays of mass or voltammetric sensors used separately.

Voltammetric detection of antimony in natural water on cathodically pretreated microcrystalline boron doped diamond electrode: A possibility how to eliminate interference of arsenic without surface modification.

Science.gov (United States)

Lukáčová-Chomisteková, Zuzana; Culková, Eva; Bellová, Renata; Melicherčíková, Danica; Durdiak, Jaroslav; Beinrohr, Ernest; Rievaj, Miroslav; Tomčík, Peter

2018-02-01

Very simple and fast electroanalytical method for the detection Sb(III) on chemically unmodified boron-doped diamond electrode (BDDE) has been developed. Voltammetric behavior of antimony was investigated in various acidic supporting electrolytes and the most suitable medium for the determination of Sb(III) on bare BDDE has been 6molL -1 HClO 4 solution. The analytical performance was studied with differential pulse anodic stripping voltammetry (DPASV) with optimized conditions (deposition potential -1V vs. Ag/ AgCl and deposition time 240s). An analysis of possible effects due to the presence of other metal ions (especially As(III)) in the solution was eliminated using NaH 2 PO 4 as supporting electrolyte with addition EDTA as selective complexing agent for Sb(III). Speciation of antimony was also investigated. The detection limit of this analytical strategy achieved value of 1.08 × 10 -7 molL -1 . The proposed method was validated and applied for natural water from former antimony mines as real samples. Copyright © 2017 Elsevier B.V. All rights reserved.

Voltammetric sensor for electrochemical determination of the floral origin of honey based on a zinc oxide nanoparticle modified carbon paste electrode

Directory of Open Access Journals (Sweden)

K. Tiwari

2018-04-01

Full Text Available A new methodology based on cyclic voltammetry using a chemically modified electrode has been developed for the discrimination of the floral origin of honey. This method involves an electronic tongue with an electrochemical sensor made from a carbon paste (CPs electrode where zinc oxide (ZnO nanoparticles are used as an electroactive binder material. The bare CPs electrode is evaluated for comparison. The electrochemical response of the modified electrode in 50 samples of five different floral types of honey has been analysed by the cyclic voltammetric technique. The voltammograms of each floral variety of honey reflect the redox properties of the ZnO nanoparticles present inside the carbon paste matrix and are strongly influenced by the nectar source of honey. Thus, each type of honey provides a characteristic signal which is evaluated by using principal component analysis (PCA and an artificial neural network (ANN. The result of a PCA score plot of the transient responses obtained from the modified carbon paste electrode clearly shows discrimination among the different floral types of honey. The ANN model for floral classification of honey shows more than 90 % accuracy. These results indicate that the ZnO nanoparticles modified carbon paste (ZnO Nps modified CPs electrode can be a useful electrode for discrimination of honey samples from different floral origins.

Ion transfer through solvent polymeric membranes driven by an exponential current flux.

Science.gov (United States)

Molina, A; Torralba, E; González, J; Serna, C; Ortuño, J A

2011-03-21

General analytical equations which govern ion transfer through liquid membranes with one and two polarized interfaces driven by an exponential current flux are derived. Expressions for the transient and stationary E-t, dt/dE-E and dI/dE-E curves are obtained, and the evolution from transient to steady behaviour has been analyzed in depth. We have also shown mathematically that the voltammetric and stationary chronopotentiometric I(N)-E curves are identical (with E being the applied potential for voltammetric techniques and the measured potential for chronopotentiometric techniques), and hence, their derivatives provide identical information.

Development of miniaturized disposable electrochemical systems intended for point of care blood analysis

DEFF Research Database (Denmark)

Musa, Arnaud Emmanuel

to pH changes in a very reproducible way despite their very simple fabrication processes. Moreover, the developed voltammetric system presented the major advantage of limiting the potential issues stemming from the reference half-cell. Indeed, since the measurement principle was based on evaluating...... that significant differences in terms of electrochemical, mechanical and electrical properties exist between these products. The effect of electrochemical and thermal treatments of the screen-printed materials was also investigated. This study resulted in the selection of an optimal electrochemical system used...... species. Moreover, to my knowledge, the use of SP for the development of this type of voltammetric systems has surprisingly only been recently investigated by D. K. Kampouris et al. [1] despite its undeniable advantages. Electrochemical measurements highlighted the promising performances...

Electrochemical maps and movies of the hydrogen evolution reaction on natural crystals of molybdenite (MoS2): basal vs. edge plane activity.

Science.gov (United States)

Bentley, Cameron L; Kang, Minkyung; Maddar, Faduma M; Li, Fengwang; Walker, Marc; Zhang, Jie; Unwin, Patrick R

2017-09-01

Two dimensional (2D) semiconductor materials, such as molybdenum disulfide (MoS 2 ) have attracted considerable interest in a range of chemical and electrochemical applications, for example, as an abundant and low-cost alternative electrocatalyst to platinum for the hydrogen evolution reaction (HER). While it has been proposed that the edge plane of MoS 2 possesses high catalytic activity for the HER relative to the "catalytically inert" basal plane, this conclusion has been drawn mainly from macroscale electrochemical (voltammetric) measurements, which reflect the "average" electrocatalytic behavior of complex electrode ensembles. In this work, we report the first spatially-resolved measurements of HER activity on natural crystals of molybdenite, achieved using voltammetric scanning electrochemical cell microscopy (SECCM), whereby pixel-resolved linear-sweep voltammogram (LSV) measurements have allowed the HER to be visualized at multiple different potentials to construct electrochemical flux movies with nanoscale resolution. Key features of the SECCM technique are that characteristic surface sites can be targeted and analyzed in detail and, further, that the electrocatalyst area is known with good precision (in contrast to many macroscale measurements on supported catalysts). Through correlation of the local voltammetric response with information from scanning electron microscopy (SEM) and atomic force microscopy (AFM) in a multi-microscopy approach , it is demonstrated unequivocally that while the basal plane of bulk MoS 2 (2H crystal phase) possesses significant activity, the HER is greatly facilitated at the edge plane ( e.g. , surface defects such as steps, edges or crevices). Semi-quantitative treatment of the voltammetric data reveals that the HER at the basal plane of MoS 2 has a Tafel slope and exchange current density ( J 0 ) of ∼120 mV per decade and 2.5 × 10 -6 A cm -2 (comparable to polycrystalline Co, Ni, Cu and Au), respectively, while the edge

MWCNTs/Cu(OH)2 nanoparticles/IL nanocomposite modified glassy carbon electrode as a voltammetric sensor for determination of the non-steroidal anti-inflammatory drug diclofenac

International Nuclear Information System (INIS)

Arvand, Majid; Gholizadeh, Tahereh M.; Zanjanchi, Mohammad Ali

2012-01-01

This paper describes the development and utilization of a new nanocomposite consisting of Cu(OH) 2 nanoparticles, hydrophobic ionic liquid 1-ethyl-3-methylimidazolium hexafluorophosphate (EMIMPF 6 ) and multiwalled carbon nanotubes for glassy carbon electrode modification. The nanocomposite was characterized by transmission electron microscopy (TEM), scanning electron microscopy (SEM) along with energy-dispersive X-ray spectroscopy (EDX). The modified electrode was used for electrochemical characterization of diclofenac. Using differential pulse voltammetry, the prepared sensor showed good sensitivity and selectivity with low overpotential for the determination of diclofenac in the range from 0.18 to 119 μM, with a detection limit of 0.04 μM. Electrochemical studies suggested that the MWCNTs/Cu(OH) 2 nanoparticles/IL nanocomposite modified electrode provided a synergistic augmentation on the voltammetric behavior of electrochemical oxidation of diclofenac, which was indicated by the improvement of anodic peak current. Highlights: ► This work examines oxidation of diclofenac at a nanocomposite modified electrode. ► The salient feature of this electrode is large diffusion coefficient. ► The proposed electrode decreased overpotential of diclofenac electrooxidation. ► The modified electrode has good stability and reproducibility.

Electrochemical behavior of the antituberculosis drug isoniazid and its square-wave adsorptive stripping voltammetric estimation in bulk form, tablets and biological fluids at a mercury electrode.

Science.gov (United States)

Ghoneim, M M; el-Baradie, K Y; Tawfik, A

2003-11-24

Isoniazid, pyridine-4-carboxylic acid hydrazide, is an antituberculosis-agent, which is used to prevent the development of clinical tuberculosis. A validated square-wave adsorptive cathodic stripping voltammetric procedure for the trace determination of the bulk drug at the hanging mercury drop electrode (HMDE) has been developed. Under the optimized conditions, (accumulation potential=-0.9 V, accumulation time=50-300 s, scan increment=8 mV, pulse-amplitude=25 mV, frequency=120 Hz and acetate buffer at pH 5.5) isoniazed generated two irreversible cathodic peaks. The first peak current showed a linear dependence with the drug concentration over the range 5 x 10(-10)-21 x 0(-6) M. The mean percentage recoveries, based on the average of five replicate measurements, for 7 x 10(-9) and 5 x 10(-8) M isoniazid were 97.71+/-2.93 and 99.76+/-0.77, respectively. The achieved limits of detection (LOD) and quantitation (LOQ) were 1.18 x 10(-10) and 3.93 x 10(-10) M isoniazid, respectively. The procedure was applied to the assay of the drug in tablets (Isocid and T.B. Zide), spiked human serum and urine with mean percentage recoveries of 97.81+/-1.49, 97.45+/-2.09, and 97.08+/-1.06, respectively. The limits of detection of 1.47 x 10(-9) and 2.4 x 10(-8) M, and quantitation of 4.9 x 10(-9) and 8 x 10(-8) M drug in human serum and urine, respectively, were achieved. The mean values of the various pharmackinetic parameters of isoniazid (C(max), T(max), t(1/2), AUC, and K(e)), estimated from analysis of plasma of two volunteers by means of the proposed procedure were similar to literature values.

Measurement of benzenethiol adsorption to nanostructured Pt, Pd, and PtPd films using Raman spectroelectrochemistry.

Science.gov (United States)

Pomfret, Michael B; Pietron, Jeremy J; Owrutsky, Jeffrey C

2010-05-04

Raman spectroscopy and electrochemical methods were used to study the behavior of the model adsorbate benzenethiol (BT) on nanostructured Pt, Pd, and PtPd electrodes as a function of applied potential. Benzenethiol adsorbs out of ethanolic solutions as the corresponding thiolate, and voltammetric stripping data reveal that BT is oxidatively removed from all of the nanostructured metals upon repeated oxidative and reductive cycling. Oxidative stripping potentials for BT increase in the order Pt oxidizing potentials via cleavage of the Pt-S bond. In contrast, on nanoscale Pd and PtPd, BT is irreversibly lost due to cleavage of BT C-S bonds at oxidizing potentials, which leaves adsorbed sulfur oxides on Pd and PtPd films and effects the desulfurization of BT. While Pd and PtPd films are less sulfur-resistant than Pt films, palladium oxides, which form at higher potentials than Pt oxides, oxidatively desulfurize BT. In situ spectroelectrochemical Raman spectroscopy provides real-time, chemically specific information that complements the cyclic voltammetric data. The combination of these techniques affords a powerful and convenient method for guiding the development of sulfur-tolerant PEMFC catalysts.

Highly sensitive and selective voltammetric detection of mercury(II) using an ITO electrode modified with 5-methyl-2-thiouracil, graphene oxide and gold nanoparticles

International Nuclear Information System (INIS)

Zhou, N.; Chen, H.; Li, J.; Chen, L.

2013-01-01

We have developed an electrochemical sensor for highly selective and sensitive determination of Hg(II). It is based on the specific binding of 5-methyl-2-thiouracil (MTU) and Hg(II) to the surface of an indium tin oxide (ITO) electrode modified with a composite made from graphene oxide (GO) and gold nanoparticles (AuNPs). This leads to a largely enhanced differential pulse voltammetric response for Hg(II). Following optimization of the method, a good linear relationship (R = 0.9920) is found between peak current and the concentration of Hg(II) in the 5.0-110.0 nM range. The limit of detection (LOD) is 0.78 nM at a signal-to-noise ratio of 3. A study on the interference by several metal ions revealed no interferences. The feasibility of this method was demonstrated by the analyses of real water samples. The LODs are 6.9, 1.0 and 1.9 nM for tap water, bottled water and lake water samples, respectively, and recoveries for the water samples spiked with 8.0, 50.0 and 100.0 nM were 83.9-96.8 %, with relative standard deviations ranging from 3.3 % to 5.2 %. (author)

Stripping analysis of nanomolar perchlorate in drinking water with a voltammetric ion-selective electrode based on thin-layer liquid membrane.

Science.gov (United States)

Kim, Yushin; Amemiya, Shigeru

2008-08-01

A highly sensitive analytical method is required for the assessment of nanomolar perchlorate contamination in drinking water as an emerging environmental problem. We developed the novel approach based on a voltammetric ion-selective electrode to enable the electrochemical detection of "redox-inactive" perchlorate at a nanomolar level without its electrolysis. The perchlorate-selective electrode is based on the submicrometer-thick plasticized poly(vinyl chloride) membrane spin-coated on the poly(3-octylthiophene)-modified gold electrode. The liquid membrane serves as the first thin-layer cell for ion-transfer stripping voltammetry to give low detection limits of 0.2-0.5 nM perchlorate in deionized water, commercial bottled water, and tap water under a rotating electrode configuration. The detection limits are not only much lower than the action limit (approximately 246 nM) set by the U.S. Environmental Protection Agency but also are comparable to the detection limits of the most sensitive analytical methods for detecting perchlorate, that is, ion chromatography coupled with a suppressed conductivity detector (0.55 nM) or electrospray ionization mass spectrometry (0.20-0.25 nM). The mass transfer of perchlorate in the thin-layer liquid membrane and aqueous sample as well as its transfer at the interface between the two phases were studied experimentally and theoretically to achieve the low detection limits. The advantages of ion-transfer stripping voltammetry with a thin-layer liquid membrane against traditional ion-selective potentiometry are demonstrated in terms of a detection limit, a response time, and selectivity.

Simultaneous Voltammetric Determination of Acetaminophen and Isoniazid (Hepatotoxicity-Related Drugs) Utilizing Bismuth Oxide Nanorod Modified Screen-Printed Electrochemical Sensing Platforms.

Science.gov (United States)

Mahmoud, Bahaa G; Khairy, Mohamed; Rashwan, Farouk A; Banks, Craig E

2017-02-07

To overcome the recent outbreaks of hepatotoxicity-related drugs, a new analytical tool for the continuously determination of these drugs in human fluids is required. Electrochemical-based analytical methods offer an effective, rapid, and simple tool for on-site determination of various organic and inorganic species. However, the design of a sensitive, selective, stable, and reproducible sensor is still a major challenge. In the present manuscript, a facile, one-pot hydrothermal synthesis of bismuth oxide (Bi 2 O 2.33 ) nanostructures (nanorods) was developed. These BiO nanorods were cast onto mass disposable graphite screen-printed electrodes (BiO-SPEs), allowing the ultrasensitive determination of acetaminophen (APAP) in the presence of its common interference isoniazid (INH), which are both found in drug samples. The simultaneous electroanalytical sensing using BiO-SPEs exhibited strong electrocatalytic activity toward the sensing of APAP and INH with an enhanced analytical signal (voltammetric peak) over that achievable at unmodified (bare) SPEs. The electroanalytical sensing of APAP and INH are possible with accessible linear ranges from 0.5 to 1250 μM and 5 to 1760 μM with limits of detection (3σ) of 30 nM and 1.85 μM, respectively. The stability, reproducibility, and repeatability of BiO-SPE were also investigated. The BiO-SPEs were evaluated toward the sensing of APAP and INH in human serum, urine, saliva, and tablet samples. The results presented in this paper demonstrate that BiO-SPEs sensing platforms provide a potential candidate for the accurate determination of APAP and INH within human fluids and pharmaceutical formulations.

Aging time and brand determination of pasteurized milk using a multisensor e-nose combined with a voltammetric e-tongue

International Nuclear Information System (INIS)

Bougrini, Madiha; Tahri, Khalid; Haddi, Zouhair; El Bari, Nezha; Llobet, Eduard; Jaffrezic-Renault, Nicole; Bouchikhi, Benachir

2014-01-01

A combined approach based on a multisensor system to get additional chemical information from liquid samples through the analysis of the solution and its headspace is illustrated and commented. In the present work, innovative analytical techniques, such as a hybrid e-nose and a voltammetric e-tongue were elaborated to differentiate between different pasteurized milk brands and for the exact recognition of their storage days through the data fusion technique of the combined system. The Principal Component Analysis (PCA) has shown an acceptable discrimination of the pasteurized milk brands on the first day of storage, when the two instruments were used independently. Contrariwise, PCA indicated that no clear storage day's discrimination can be drawn when the two instruments are applied separately. Mid-level of abstraction data fusion approach has demonstrated that results obtained by the data fusion approach outperformed the classification results of the e-nose and e-tongue taken individually. Furthermore, the Support Vector Machine (SVM) supervised method was applied to the new subset and confirmed that all storage days were correctly identified. This study can be generalized to several beverage and food products where their quality is based on the perception of odor and flavor. - Highlights: • Five pasteurized milk brands were differentiated using e-nose and e-tongue. • E-tongue allowed a correct distinction of the milk brands comparing to the e-nose. • The combined system allows determining the storage days of pasteurized milk. • No clear storage day’s discrimination can be drawn when applied e-systems separately. • Data fusion method has been successful in the identification of the storage days

Aging time and brand determination of pasteurized milk using a multisensor e-nose combined with a voltammetric e-tongue

Energy Technology Data Exchange (ETDEWEB)

Bougrini, Madiha [Sensor Electronic and Instrumentation Group, Moulay Ismaïl University, Faculty of Sciences, Physics Department, B.P. 11201, Zitoune, Meknes (Morocco); Université de Lyon, Université Claude Bernard Lyon 1, Institut des Sciences Analytiques, UMR CNRS 5280, 5, rue de la Doua, 69100 Villeurbanne Cedex (France); Tahri, Khalid [Sensor Electronic and Instrumentation Group, Moulay Ismaïl University, Faculty of Sciences, Physics Department, B.P. 11201, Zitoune, Meknes (Morocco); Haddi, Zouhair [Sensor Electronic and Instrumentation Group, Moulay Ismaïl University, Faculty of Sciences, Physics Department, B.P. 11201, Zitoune, Meknes (Morocco); MINOS-EMaS, Electronic Engineering Department, Universitat Rovira i Virgili, Avda. Països Catalans, 26, 43007 Tarragona (Spain); El Bari, Nezha [Biotechnology Agroalimentary and Biomedical Analysis Group, Moulay Ismaïl University, Faculty of Sciences, Biology Department, B.P. 11201, Zitoune, Meknes (Morocco); Llobet, Eduard [MINOS-EMaS, Electronic Engineering Department, Universitat Rovira i Virgili, Avda. Països Catalans, 26, 43007 Tarragona (Spain); Jaffrezic-Renault, Nicole [Université de Lyon, Université Claude Bernard Lyon 1, Institut des Sciences Analytiques, UMR CNRS 5280, 5, rue de la Doua, 69100 Villeurbanne Cedex (France); Bouchikhi, Benachir, E-mail: benachir.bouchikhi@gmail.com [Sensor Electronic and Instrumentation Group, Moulay Ismaïl University, Faculty of Sciences, Physics Department, B.P. 11201, Zitoune, Meknes (Morocco)

2014-12-01

A combined approach based on a multisensor system to get additional chemical information from liquid samples through the analysis of the solution and its headspace is illustrated and commented. In the present work, innovative analytical techniques, such as a hybrid e-nose and a voltammetric e-tongue were elaborated to differentiate between different pasteurized milk brands and for the exact recognition of their storage days through the data fusion technique of the combined system. The Principal Component Analysis (PCA) has shown an acceptable discrimination of the pasteurized milk brands on the first day of storage, when the two instruments were used independently. Contrariwise, PCA indicated that no clear storage day's discrimination can be drawn when the two instruments are applied separately. Mid-level of abstraction data fusion approach has demonstrated that results obtained by the data fusion approach outperformed the classification results of the e-nose and e-tongue taken individually. Furthermore, the Support Vector Machine (SVM) supervised method was applied to the new subset and confirmed that all storage days were correctly identified. This study can be generalized to several beverage and food products where their quality is based on the perception of odor and flavor. - Highlights: • Five pasteurized milk brands were differentiated using e-nose and e-tongue. • E-tongue allowed a correct distinction of the milk brands comparing to the e-nose. • The combined system allows determining the storage days of pasteurized milk. • No clear storage day’s discrimination can be drawn when applied e-systems separately. • Data fusion method has been successful in the identification of the storage days.

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

International Nuclear Information System (INIS)

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

2014-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

Zhu, Wencai [Key Laboratory for Colloid and Interface Chemistry of State Education Ministry, School of Chemistry and Chemical Engineering, Shandong University, Jinan 250100 (China); School of Chemistry and Chemical Engineering, Qilu Normal University, Jinan 250013 (China); Huang, Hui; Gao, Xiaochun [Key Laboratory for Colloid and Interface Chemistry of State Education Ministry, School of Chemistry and Chemical Engineering, Shandong University, Jinan 250100 (China); Ma, Houyi, E-mail: hyma@sdu.edu.cn [Key Laboratory for Colloid and Interface Chemistry of State Education Ministry, School of Chemistry and Chemical Engineering, Shandong University, Jinan 250100 (China)

2014-12-01

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

Simultaneous detection of ascorbic acid, uric acid and homovanillic acid at copper modified electrode

International Nuclear Information System (INIS)

Selvaraju, T.; Ramaraj, R.

2007-01-01

The copper was deposited on glassy carbon (GC) and indium tin oxide (ITO) electrodes by electrochemical method. The copper structures on electrode were characterized by atomic force microscope, X-ray diffractometeric pattern and differential pulse voltammetric studies. Optimal conditions for uniform growth of copper structures on the electrode were established. Voltammetric sensor was fabricated using the copper deposited GC electrode for the simultaneous detection and determination of uric acid (UA) and homovanillic acid (HVA) in the presence of excess concentrations of ascorbic acid (AA). The voltammetric signals due to AA and UA oxidation were well separated with a potential difference of 400 mV and AA did not interfere with the measurement of UA and HVA at the GC/Cu electrode. Linear calibration curves were obtained in the concentration range 1-40 μM for AA and 20-50 μM for UA at physiological pH and a detection limit of 10 nM of UA in the presence of 10-fold excess concentrations of AA was achieved. The simultaneous detection of submicromolar concentrations of AA, UA and HVA was achieved at the GC/Cu electrode. The practical utility of the present GC/Cu modified electrode was demonstrated by measuring the AA content in Vitamin C tablet, UA content in human urine and blood serum samples with satisfactory results

MWCNTs/Cu(OH){sub 2} nanoparticles/IL nanocomposite modified glassy carbon electrode as a voltammetric sensor for determination of the non-steroidal anti-inflammatory drug diclofenac

Energy Technology Data Exchange (ETDEWEB)

Arvand, Majid, E-mail: arvand@guilan.ac.ir; Gholizadeh, Tahereh M.; Zanjanchi, Mohammad Ali

2012-08-01

This paper describes the development and utilization of a new nanocomposite consisting of Cu(OH){sub 2} nanoparticles, hydrophobic ionic liquid 1-ethyl-3-methylimidazolium hexafluorophosphate (EMIMPF{sub 6}) and multiwalled carbon nanotubes for glassy carbon electrode modification. The nanocomposite was characterized by transmission electron microscopy (TEM), scanning electron microscopy (SEM) along with energy-dispersive X-ray spectroscopy (EDX). The modified electrode was used for electrochemical characterization of diclofenac. Using differential pulse voltammetry, the prepared sensor showed good sensitivity and selectivity with low overpotential for the determination of diclofenac in the range from 0.18 to 119 {mu}M, with a detection limit of 0.04 {mu}M. Electrochemical studies suggested that the MWCNTs/Cu(OH){sub 2} nanoparticles/IL nanocomposite modified electrode provided a synergistic augmentation on the voltammetric behavior of electrochemical oxidation of diclofenac, which was indicated by the improvement of anodic peak current. Highlights: Black-Right-Pointing-Pointer This work examines oxidation of diclofenac at a nanocomposite modified electrode. Black-Right-Pointing-Pointer The salient feature of this electrode is large diffusion coefficient. Black-Right-Pointing-Pointer The proposed electrode decreased overpotential of diclofenac electrooxidation. Black-Right-Pointing-Pointer The modified electrode has good stability and reproducibility.

Biologically Inspired Materials for Electro-Responsive Coatings and the Photo-Oxidation of Water

Science.gov (United States)

2010-02-01

from the 12-mer li - brary exhibited an over-expression of amide-containing amino acids. Both amides and hydrophilic residues can participate in hydrogen... li =17 73410 7865 [R(int) = 0.0350] 99.9 % Semi-empirical from equivalents 0.7216 and 0.5420 Full-matrix least-squares on F2 7865 / 27 / 442 1.058 R1...Joseph Wang, Gustavo Rivas, Mian Jiang, and Xueji Zhang. Electrochemically induced release of DNA from gold ultramicroelectrodes. Langmuir, 15:6541- 6545

Quantitative determination of glycyrrhizinic acid by square-wave

Directory of Open Access Journals (Sweden)

Aneta Dimitrovska

2003-06-01

Full Text Available Novel adsorptive stripping square-wave voltammetric method as well as a new high-pressure liquid chromatographic method for direct determination of glycyrrhizinic acid in dosage pharmaceutical preparation, used against virus infections, have been developed. Glycyrrhizinic acid is an electrochemically active compound, which undergoes irreversible reduction on a mercury electrode surface in an aqueous medium. Its redox properties were studied thoroughly by means of square-wave voltammetry, as one of the most advanced electroanalytical technique. The voltammetric response depends mainly on the pH of the medium, composition of the supporting electrolyte, as well as the parameters of the excitement signal. It was also observed that the voltammetric properties strongly depend on the accumulation time and potential, revealing significant adsorption of glycyrrhizinic acid onto the mercury electrode surface. Upon this feature, an adsorptive stripping voltammetric method for quantitative determination of glycyrrhizinic acid was developed. A simple, sensitive and precise reversed phase HPLC method with photodiode array UV detection has also been developed, mainly for comparison and conformation of the results obtained with the voltammetric method.

The Use of Silver Solid Amalgam Electrodes for Voltammetric and Amperometric Determination of Nitrated Polyaromatic Compounds Used as Markers of Incomplete Combustion

Directory of Open Access Journals (Sweden)

Oksana Yosypchuk

2012-01-01

Full Text Available Genotoxic nitrated polycyclic aromatic hydrocarbons (NPAHs are formed during incomplete combustion processes by reaction of polycyclic aromatic hydrocarbons (PAHs with atmospheric nitrogen oxides. 1-Nitropyrene, 2-nitrofluorene, and 3-nitrofluoranthene as the dominating substances are used as markers of NPAHs formation by these processes. In the presented study, voltammetric properties and quantification of these compounds and of 5-nitroquinoline (as a representative of environmentally important genotoxic heterocyclic compounds have been investigated using a mercury meniscus modified silver solid amalgam electrode (m-AgSAE, which represent a nontoxic alternative to traditional mercury electrodes. Linear calibration curves over three orders of magnitude and limits of determination mostly in the 10−7 mol L−1 concentration range were obtained using direct current and differential pulse voltammetry. Further, satisfactory HPLC separation of studied analytes in fifteen minutes was achieved using 0.01 mol L−1 phosphate buffer, pH 7.0 : methanol (15 : 85, v/v mobile phase, and C18 reversed stationary phase. Limits of detection of around 1 · 10−5 mol L−1 were achieved using amperometric detection at m-AgSAE in wall-jet arrangement for all studied analytes. Practical applicability of this technique was demonstrated on the determination of 1-nitropyrene, 2-nitrofluorene, 3-nitrofluoranthene, and 5-nitroquinoline in drinking water after their preliminary separation and preconcentration using solid phase extraction with the limits of detection around 1 · 10−6 mol L−1.

Voltammetric fingerprinting of oils and its combination with chemometrics for the detection of extra virgin olive oil adulteration.

Science.gov (United States)

Tsopelas, Fotios; Konstantopoulos, Dimitris; Kakoulidou, Anna Tsantili

2018-07-26

In the present work, two approaches for the voltammetric fingerprinting of oils and their combination with chemometrics were investigated in order to detect the adulteration of extra virgin olive oil with olive pomace oil as well as the most common seed oils, namely sunflower, soybean and corn oil. In particular, cyclic voltammograms of diluted extra virgin olive oils, regular (pure) olive oils (blends of refined olive oils with virgin olive oils), olive pomace oils and seed oils in presence of dichloromethane and 0.1 M of LiClO 4 in EtOH as electrolyte were recorded at a glassy carbon working electrode. Cyclic voltammetry was also employed in methanolic extracts of olive and seed oils. Datapoints of cyclic voltammograms were exported and submitted to Principal Component Analysis (PCA), Partial Least Square- Discriminant Analysis (PLS-DA) and soft independent modeling of class analogy (SIMCA). In diluted oils, PLS-DA provided a clear discrimination between olive oils (extra virgin and regular) and olive pomace/seed oils, while SIMCA showed a clear discrimination of extra virgin olive oil in regard to all other samples. Using methanolic extracts and considering datapoints recorded between 0.6 and 1.3 V, PLS-DA provided more information, resulting in three clusters-extra virgin olive oils, regular olive oils and seed/olive pomace oils-while SIMCA showed inferior performance. For the quantification of extra virgin olive oil adulteration with olive pomace oil or seed oils, a model based on Partial Least Square (PLS) analysis was developed. Detection limit of adulteration in olive oil was found to be 2% (v/v) and the linearity range up to 33% (v/v). Validation and applicability of all models was proved using a suitable test set. In the case of PLS, synthetic oil mixtures with 4 known adulteration levels in the range of 4-26% were also employed as a blind test set. Copyright © 2018 Elsevier B.V. All rights reserved.

A Voltammetric Sensor Based on Chemically Reduced Graphene Oxide-Modified Screen-Printed Carbon Electrode for the Simultaneous Analysis of Uric Acid, Ascorbic Acid and Dopamine

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Prosper Kanyong

2016-12-01

Full Text Available A disposable screen-printed carbon electrode (SPCE modified with chemically reduced graphene oxide (rGO (rGO-SPCE is described. The rGO-SPCE was characterized by UV-Vis and electrochemical impedance spectroscopy, and cyclic voltammetry. The electrode displays excellent electrocatalytic activity towards uric acid (UA, ascorbic acid (AA and dopamine (DA. Three resolved voltammetric peaks (at 183 mV for UA, 273 mV for AA and 317 mV for DA, all vs. Ag/AgCl were found. Differential pulse voltammetry was used to simultaneously detect UA, AA and DA in their ternary mixtures. The linear working range extends from 10 to 3000 μM for UA; 0.1 to 2.5 μM, and 5.0 to 2 × 104 µM for AA; and 0.2 to 80.0 μM and 120.0 to 500 µM for DA, and the limits of detection (S/N = 3 are 0.1, 50.0, and 0.4 μM, respectively. The performance of the sensor was evaluated by analysing spiked human urine samples, and the recoveries were found to be well over 98.0% for the three compounds. These results indicate that the rGO-SPCE represents a sensitive analytical sensing tool for simultaneous analysis of UA, AA and DA.

Spectral and cyclic voltammetric studies on some intramolecularly hydrogen bonded arylhydrazones: Crystal and molecular structure of 2-(2-(3-nitrophenyl)hydrazono)-5,5-dimethylcyclohexane-1,3-dione

Science.gov (United States)

Sethukumar, A.; Arul Prakasam, B.

2010-01-01

A series of arylhydrazone derivatives ( 1- 7) were prepared by the coupling of acetylacetone/dimedone with respective aromatic diazonium salts and characterized by IR, 1H and 13C NMR spectra. The IR and NMR spectral data clearly manifests the effective intramolecular hydrogen bonding in all the cases. Cyclic voltammetric studies certainly indicate that in all the cases the reduced center is C dbnd N bond of hydrazonic moiety. The single crystal X-ray structural analysis of 2-(2-(3-nitrophenyl)hydrazono)-5,5-dimethylcyclohexane-1,3-dione ( 6) is also reported. Single crystal X-ray analysis of 6 evidences the intramolecular hydrogen bonding with the N(2)⋯O(4) distance of 2.642(15) Å, which can be designated as S(6) according to Etter's graph nomenclature. The cyclohexane ring conformation in the molecule ( 6) can be described as an envelope. RAHB studies suggest that the resonance assistance for hydrogen bonding is significantly reduced for the compound ( 6) due to the non-planarity of the six atoms which are involved in resonant cycle S(6) of Etter's graph. The planarity of the resonant cycle S(6) is very much disturbed by the conformational requirement of the cyclohexane ring and hence RAHB concept is less operative in this case.

Estudos da deposição em subtensão de cádmio sobre ouro policristalino na presença de diferentes ânions co-adsorvidos

Directory of Open Access Journals (Sweden)

Santos Mauro C.

2001-01-01

Full Text Available Cadmium UPD on Au was studied by voltammetric and microgravimetric measurements. In the oxide formation/reduction potential region, a mass increasing/decreasing of 32 ng cm-2 was associated to incorporation/elimination of one oxygen per active site. The modifications promoted in the voltammetric and mass profiles by 10-5 M Cd(ClO42 are restricted to potentials more negative than 0.4 V. After a 120 s potential delay at 0.05 V, the positive sweep reveals an anodic peak with charge of 40 muC cm-2 and mass decrease of 22 ng cm-2, associated to Cd ads dissolution. Sulphate or chloride was added to the solution without significant influence, due to the low coverage with Cd or anions.

The Electrochemical Behavior of Dispersions of Spherical Ultramicroelectrodes.

Science.gov (United States)

1986-07-30

means of bipolar electrolyses with dispersions. Polarization equations are predicted for highly simplified models based on the concept of the mixture...three-dimensional electrodes. Bipolar electrolyses on dispersions of spherical particles have been proposed and the behavior of such electrodes in the...photodecomposition of water (e.g. see (32-41)). It should be noted that the size range of the particles which will be most frequently used in dispersion

Computer-controlled Instrumentation for Fast Voltammetry at Ultramicroelectrodes

Czech Academy of Sciences Publication Activity Database

Pospíšil, Lubomír; Fiedler, Jan; Fanelli, N.

2000-01-01

Roč. 71, č. 4 (2000), s. 1804-1810 ISSN 0034-6748 R&D Projects: GA ČR GA203/97/1048; GA MŠk OC D15.10 Institutional research plan: CEZ:AV0Z4040901; CEZ:A54/98:Z4-040-9-ii Subject RIV: CG - Electrochemistry Impact factor: 1.239, year: 2000

A potentiostat featuring an integrator transimpedance amplifier for the measurement of very low currents—Proof-of-principle application in microfluidic separations and voltammetry

Science.gov (United States)

Koutilellis, G. D.; Economou, A.; Efstathiou, C. E.

2016-03-01

This work reports the design and construction of a novel potentiostat which features an integrator transimpedance amplifier as a current-monitoring unit. The integration approach addresses the limitations of the feedback resistor approach used for current monitoring in conventional potentiostat designs. In the present design, measurement of the current is performed by a precision switched integrator transimpedance amplifier operated in the dual sampling mode which enables sub-pA resolution. The potentiostat is suitable for measuring very low currents (typical dynamic range: 5 pA-4.7 μA) with a 16 bit resolution, and it can support 2-, 3- and 4-electrode cell configurations. Its operation was assessed by using it as a detection module in a home-made capillary electrophoresis system for the separation and amperometric detection of paracetamol and p-aminophenol at a 3-electrode microfluidic chip. The potential and limitations of the proposed potentiostat to implement fast potential-scan voltammetric techniques were demonstrated for the case of cyclic voltammetry.

A potentiostat featuring an integrator transimpedance amplifier for the measurement of very low currents--Proof-of-principle application in microfluidic separations and voltammetry.

Science.gov (United States)

Koutilellis, G D; Economou, A; Efstathiou, C E

2016-03-01

This work reports the design and construction of a novel potentiostat which features an integrator transimpedance amplifier as a current-monitoring unit. The integration approach addresses the limitations of the feedback resistor approach used for current monitoring in conventional potentiostat designs. In the present design, measurement of the current is performed by a precision switched integrator transimpedance amplifier operated in the dual sampling mode which enables sub-pA resolution. The potentiostat is suitable for measuring very low currents (typical dynamic range: 5 pA-4.7 μA) with a 16 bit resolution, and it can support 2-, 3- and 4-electrode cell configurations. Its operation was assessed by using it as a detection module in a home-made capillary electrophoresis system for the separation and amperometric detection of paracetamol and p-aminophenol at a 3-electrode microfluidic chip. The potential and limitations of the proposed potentiostat to implement fast potential-scan voltammetric techniques were demonstrated for the case of cyclic voltammetry.

Reduction Pathways of Cyclooctatetraene Iron Tricarbonyl as Examined Using Infrared Spectroelectrochemistry.

Science.gov (United States)

1987-09-25

173/175/179 potentiostat system was used for voltammetric measurements and thin-layer electrolyses . Cyclooctatetraene iron tricarbonyl was synthesised...the subsequent addftion of water . 3 The infrared spectrum for this species contains similar features to those, in Fig. 3B, including a band around 1670

Voltammetric determination of ultratrace levels of cerium(III) using a carbon paste electrode modified with nano-sized cerium-imprinted polymer and multiwalled carbon nanotubes

International Nuclear Information System (INIS)

Alizadeh, Taher; Ganjali, Mohammad Reza; Akhoundian, Maede; Norouzi, Parviz

2016-01-01

A carbon paste electrode was modified with a Ce(III)-imprinted polymer (Ce-IP) and used for voltammetric determination of Ce(III) ions in real water samples. Precipitation polymerization was used for synthesis of the nano-sized Ce-IP from vinylpyridine and methacrylic acid (acting as the complexing ligands and functional monomers), divinylbenzene (cross-linker) and AIBN as the radical starter. The Ce-IP was characterized by scanning electron microscopy and zeta potentials. A carbon paste electrode (CPE) was then impregnated with the Ce-IP and used for the extraction and subsequent determination of Ce(III). Oxidative square wave voltammetry showed the electrode to give a significantly better response than an electrode modified with the non-imprinted polymer. The addition of multiwalled carbon nanotubes to the Ce-IP-modified electrode further improves the signal, thereby increasing the sensitivity of the method. The effects of electrode composition, extraction pH value, volume and time were optimized. The electrode, if operated at a voltage of 1.05 V (vs. Ag/AgCl), displays a linear response to Ce(III) in the 1.0 μM to 25 pM concentration range, and the detection limit is 10 pM (at an S/N ratio of 3). The relative standard deviation of 5 separate determinations is 3.1 %. The method was successfully applied to the determination of Ce(III) in the spiked samples of drinking water and sea water. (author)

Voltammetric Behaviour and Analysis of Fluchloralin

Directory of Open Access Journals (Sweden)

K. Balaji

2010-01-01

Full Text Available The electrochemical reduction behavior of fluchloralin has been studied by D.C.polarography, differential pulse polarography, millicoulometry and controlled potential electrolysis in the universal buffers ranging from 2.0 to 12.0. Kinetic parameters were evaluated and a reduction mechanism was proposed. A simple and rapid differential pulse polarographic method has been developed for the determination of fluchloralin in formulations, grains, soils and spiked water samples. The lower detection limit was found to be 1.5×10-8 M. Both the standard addition and calibration methods were used for the analytical measurements.

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

Energy Technology Data Exchange (ETDEWEB)

Ghanei-Motlagh, Masoud, E-mail: m.ghaneimotlagh@yahoo.com [Young Researchers and Elite Club, Kerman Branch, Islamic Azad University, Kerman (Iran, Islamic Republic of); Taher, Mohammad Ali; Heydari, Abolfazl [Department of Chemistry, Faculty of Sciences, Shahid Bahonar University of Kerman, Kerman (Iran, Islamic Republic of); Ghanei-Motlagh, Reza [Department of Pathobiology, Faculty of Veterinary Medicine, Ferdowsi University of Mashhad, Mashhad (Iran, Islamic Republic of); Gupta, Vinod K. [Department of Chemistry, Indian Institute of Technology Roorkee, Roorkee 247667 (India); Department of Applied Chemistry, University of Johannesburg, Johannesburg (South Africa)

2016-06-01

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

Investigation of synthesized new vanadium(III) complexes of ditolyldithiophosphate ligands by spectroscopic, cyclic voltammetric, DFT, antimicrobial and cytotoxic studies

Science.gov (United States)

Kumar, Sandeep; Syed, Atiya; Andotra, Savit; Kaur, Ramanpreet; Vikas; Pandey, Sushil K.

2018-02-01

Vanadium(III) complexes with sulfur donor dithiophosphate ligands corresponding to [{(ArO)2PS2}3V] and [{(ArO)2PS2}2VCl.L] (Ar = o-, m-, p-CH3C6H4 and p-Cl-m-CH3C6H3; L = NC5H5, P(C6H5)3, have been synthesized and characterized by various physico-chemical techniques like elemental analyses, magnetic studies, ESI-Mass, IR, UV and heteronuclear NMR (1H, 13C and 31P) spectral studies. These analyses have contributed to the prediction of structure: by exhibiting significant v(P-S) and v(Pdbnd S) band shifting in comparative IR spectra; shifting of resonance signal in comparative 31P NMR spectra of ligands and complexes and stability of V(III) ion in the complexed state is confirmed by magnetic and UV studies. Therefore, the six coordinated geometry stabilizing the trivalent vanadium atom in the complexes and adducts, respectively has been confirmed. The cyclic voltammetric analyses presented the redox aptitude of the complex under analysis which can be utilized as catalyst in organic synthesis. The geometry of ligands and complexes has been optimized using density functional theory (DFT). The structural parameters, vibrational bands and energy gaps of frontier orbitals (HOMO-LUMO) have also been calculated. The calculated geometric and spectral results reproduced the experimental data with well agreement. The DFT computed frontier molecular orbitals (HOMO-LUMO) and their energies suggest charge transfer occurs within the complexes. Antimicrobial screening of the complexes against two bacterial strains: Gram-positive, Enterrococcus faecalis and Gram-negative, Eischerichia coli and fungus Fusarium oxysporum have shown potential bioactivity. A preliminary cytotoxic analysis has been carried out using the cultivated human cell lines: lung adeno carcinoma cell line A-549, leukemia cell line THP-1, prostate cancer cell line PC3 and colorectal cancer cell line HCT-116.

Voltammetric behavior of erythromycin ethylsuccinate at a renewable silver-amalgam film electrode and its determination in urine and in a pharmaceutical preparation

International Nuclear Information System (INIS)

Vajdle, Olga; Guzsvány, Valéria; Škorić, Dušan; Anojčić, Jasmina; Jovanov, Pavle; Avramov-Ivić, Milka; Csanádi, János; Kónya, Zoltán

2016-01-01

Highlights: • Voltammetric characterization of erythromycin ethylsuccinate (EES) on Hg(Ag)FE. • Trace level determination of EES by electroreduction based SWV and SW-AdSV methods. • Protonation of the tertiary amino group supports the adsorption of EES on Hg(Ag)FE. • 1 H NMR confirms chemical shifting of tertiary amine methyl proton signals with pH. • Comparative HPLC-DAD measurements were performed for the validation of the methods. - Abstract: Erythromycin, a macrolide antibiotic, has similar antimicrobial spectrum to penicillin and it is widely used, especially in the treatment of patients who are allergic to penicillin. In this work, the application of a renewable silver-amalgam film electrode (Hg(Ag)FE) for the characterization and determination of erythromycin ethylsuccinate (EES), a widely used esterified form of this antibiotic, by means of cyclic voltammetry (CV) and square wave voltammetry (SWV) is presented. In the aqueous Britton-Robinson buffer (pH 5.0–9.0) that served as the supporting electrolyte, one reduction peak of EES was observed in the investigated potential range between −0.75 V and −1.80 V vs SCE, with peak potential maxima ranging from −1.59 V to −1.70 V, which strongly depended on the applied pH, as did the peak shape. For the analytical purposes the pH of 7.0 was selected, since in this electrolyte the EES peak was well-shaped and separated from the background current of the supporting electrolyte in both cases; in the direct cathodic SWV and in the case of square wave adsorptive stripping voltammetry (SW-AdSV). It was established, by the E p -pH correlation, that protons strongly influenced the electrochemical reduction of EES. The CVs recorded between 0.025–0.50 V s −1 at pH 7.0 confirmed that the electrode reaction is adsorption-controlled. Based on the series of 1 H NMR measurements it is proved that the tertiary amino group of EES is mainly in its protonated form at pH 7.0 which may lead, at appropriate

In situ fabricated iodine-adlayer assisted selective electrooxidation of uric acid in alkaline media

Energy Technology Data Exchange (ETDEWEB)

Miah, Md. Rezwan [Department of Electronic Chemistry, Interdisciplinary Graduate School of Science and Engineering, Tokyo Institute of Technology, Mail Box G1-5, 4259 Nagastuta, Midori-ku, Yokohama 226-8502 (Japan)], E-mail: mrmche@yahoo.com; Masud, Jahangir [Department of Electronic Chemistry, Interdisciplinary Graduate School of Science and Engineering, Tokyo Institute of Technology, Mail Box G1-5, 4259 Nagastuta, Midori-ku, Yokohama 226-8502 (Japan); Ohsaka, Takeo [Department of Electronic Chemistry, Interdisciplinary Graduate School of Science and Engineering, Tokyo Institute of Technology, Mail Box G1-5, 4259 Nagastuta, Midori-ku, Yokohama 226-8502 (Japan)], E-mail: ohsaka@echem.titech.ac.jp

2008-12-30

This work presents the electrooxidation of uric acid (UA) at an iodine-adlayer-modified gold, Au (I|Au (poly)) electrode in 0.1 M NaOH solution using cyclic voltammetric, amperometric and open-circuit potential measurement techniques. A tremendous enhancement of the electrode activity towards the electrooxidation of UA was achieved by virtue of the simple modification of the Au (poly) electrode surface with a neutral iodine-adlayer, fabricated in situ through the spontaneous oxidative chemisorption of iodide present in the sample solution. The cyclic voltammetric peak current increases remarkably for the oxidation of UA and the peak potential shifts by 365 mV to the negative direction of potential compared to the bare Au (poly) electrode. Oxidation of ascorbic acid (AA) at the I|Au (poly) electrode takes place at the same potential as that at the bare electrode, but the peak current intensity is almost twice at the bare Au (poly) electrode as compared to the modified one. In the mixture of the AA and UA, the cyclic voltammetric signals corresponding to the oxidations of AA and UA were resolved by 340 mV. The electrode response in the mixture was highly reproducible because of the inhibition of adsorption of oxidation products and UA.

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

Energy Technology Data Exchange (ETDEWEB)

Shahrokhian, Saeed, E-mail: shahrokhian@sharif.edu [Department of Chemistry, Sharif University of Technology, Tehran 11155-3516 (Iran, Islamic Republic of); Institute for Nanoscience and Technology, Sharif University of Technology, Tehran (Iran, Islamic Republic of); Azimzadeh, Mahnaz [Department of Chemistry, Sharif University of Technology, Tehran 11155-3516 (Iran, Islamic Republic of); Amini, Mohammad K. [Department of Chemistry, Isfahan University, Isfahan (Iran, Islamic Republic of)

2015-08-01

A novel voltammetric sensor based on glassy carbon electrode (GCE) modified with a thin film of multi-walled carbon nanotubes (MWCNTs) coated with an electropolymerized layer of tiron-doped polypyrrole was developed and the resulting electrode was applied for the determination of acyclovir (ACV). The surface morphology and property of the modified electrode were characterized by field emission scanning electron microscopy and electrochemical impedance spectroscopy techniques. The electrochemical performance of the modified electrode was investigated by means of linear sweep voltammetry (LSV). The effect of several experimental variables, such as pH of the supporting electrolyte, drop size of the cast MWCNTssuspension, number of electropolymerization cycles and accumulation time was optimized by monitoring the LSV response of the modified electrode toward ACV. The best response was observed at pH 7.0 after accumulation at open circuit for 160 s. Under the optimized conditions, a significant electrochemical improvement was observed toward the electrooxidation of ACV on the modified electrode surface relative to the bare GCE, resulting in a wide linear dynamic range (0.03–10.0 μM) and a low detection limit (10.0 nM) for ACV. Besides high sensitivity, the sensor represented high stability and good reproducibility for ACV analysis, and provided satisfactory results for the determination of this compound in pharmaceutical and clinical preparations. - Highlights: • A simple method was employed to construct a thin film modified electrode. • Tiron-doped polypyrrole was electropolymerized on MWCNT precast glassy carbon electrode. • Electrode surface characterization was performed by microscopic and spectroscopic techniques. • The modified electrode showed nano-molar detection limit for acyclovir. • The modified electrode was applied for the detection of ACV in pharmaceutical and clinical preparations.

Measurement of Nitrate Concentration in Aqueous Media Using an Electrochemical Nanosensor Based on Silver Nanoparticles-Nanocellulose/Graphene Oxide

Directory of Open Access Journals (Sweden)

Majid Shadfar

2017-11-01

Full Text Available Nitrate pollution is at the forefront of groundwater contamination which poses serious environmental and public health hazards.  Nitrate is usually released in solution from agricultural activities and finds its way into groundwater resources. The objective of the present study was to determine, accurately concentrations of nitrate ions in water samples from the environment using sensitive electrochemical methods. For this purpose, a modified glassy carbon electrode modified with a nanocomposite consisting of silver nanoparticles, nanocellulose, and graphene oxide (Ag/NC/GO-GCE was used. The characterization of the nanocomposite was investigated using scanning electron microscope (SEM, X-Ray diffraction (XRD, and electrochemical impedance spectroscopy (EIS. The modified Ag/NC/GO-GCE electrode was used as nanosensor for the electrocatalytic determination of nitrate using the voltammetric method. The effects of the parameters of scan rate, pH, and different nitrate concentrations were studied and the optimum conditions were obtained. A limit of detection of 0.016 µM (S/N=3 was found in the linear range of 0.005 to 10 mM nitrate. The Ag/NC/GO-GCE electrode exhibited a synergistic effect toward voltammetric determination of nitrate in the presence of graphene oxide, nanocellulose, and silver nanocatalyst. The nanosensor developed here showed excellent sensitivity, selectivity, and stability toward nitrate determination in aqueous solutions without any significant interference.

Disposable Electrochemical Immunosensor Diagnosis Device Based on Nanoparticle Probe and Immunochromatographic Strip

Energy Technology Data Exchange (ETDEWEB)

Liu, Guodong; Lin, Ying-Ying; Wang, Jun; Wu, Hong; Wai, Chien M.; Lin, Yuehe

2007-10-15

We describe a disposable electrochemical immunosensor diagnosis device that is based on the immunochromatographic strip technique and an electrochemical immunoassay based on quantum dot (QD, CdS@ZnS) labels. The device takes advantage of the speed and low-cost of the conventional immunochromatographic strip test and the high-sensitivity of the nanoparticle-based electrochemical immunoassay. A sandwich immunoreaction was performed on the immunochromatographic strip, and the captured QD labels in the test zone were determined by highly sensitive stripping voltammetric measurement of the dissolved metallic component (cadmium) with a disposable-screen-printed electrode, which is embedded underneath the membrane on the test zone. The new device coupled with a portable electrochemical analyzer shows great promise for in-field and point-of-care quantitative testing of disease-related protein biomarkers. The parameters (e.g., voltammetric measurement of QD labels, antibody immobilization, the loading amount of QD-antibody, and the immunoreaction time) that govern the sensitivity and reproducibility of the device were optimized with IgG model analyte. The voltammetric response of the optimized device is highly linear over the range of 0.1 to 10 ng mL-1 IgG, and the limit of detection is estimated to be 30 pg mL-1 in association with a 7-min immunoreaction time. The detection limit was improved to 10 pg mL-1 using a 20-min immunoreaction time. The new disposable electrochemical diagnosis device thus provides a more user-friendly, rapid, clinically accurate, less expensive, and quantitative tool for protein detection.

A cyclo olefin polymer microfluidic chip with integrated gold microelectrodes for aqueous ans non-aqueous electrochemistry

DEFF Research Database (Denmark)

Illa, Xavi; Sala, Olga Ordeig; Snakenborg, Detlef

2010-01-01

and 24 m deep channel was fabricated via hot embossing. Cyclic voltammetric measurements were carried out in aqueous and organic media, using a solution consisting of 5 mM ferrocyanide/ferricyanide in 0.5 M KNO3 and 5 mM ferrocene in 0.1 M TBAP/acetonitrile, respectively. Experimental currents obtained...

INHIBICIÓN DE LA ELECTROOXIDACION DE ÁCIDO ASCÓRBICO SOBRE ORO MEDIANTE POLIPIRROL SOBREOXIDADO

Directory of Open Access Journals (Sweden)

Luis Pesetti

2013-01-01

Full Text Available Electroanalytical determination of neurotransmitters in the brain, presents the difficulty of high anion ascorbate concentration, which oxidized at almost the same potential as the neurotransmitters. To avoid this interference, the electrode is recovered with a selective overoxidized polypyrrol (Ppy film, which supresses voltammetric ascorbate wave and the discharge current of neurotransmitter is only observed. The Pyrrol polymerization is made with a stepped voltammetric sweep, between 0.3 V and an anodic potential of approximately 1.0 V in a buffer solution at 0,005 V/sec. With potentiostatic electrolysis at 1.05 V (measured vs. reversible hydrogen electrode, RHE the polymer film is oxidized and it is overoxidized at 1.7 V. During 48 hours, the film remains stable. Then, it slowly losses its properties. The optimum conditions to obtain a good quality film are found in this research.

Electrochemical characterisation of novel screen-printed carbon paste electrodes for voltammetric measurements

Directory of Open Access Journals (Sweden)

Sýs Milan

2017-01-01

Full Text Available This work is focused on the homemade screen-printed carbon paste electrode containing basically graphite powder (or glassy carbon powder, poly(vinylbchloride (PVC and paraffin oil. It compares the electrochemical properties of conventional carbon-based electrodes and prepared screen-printed carbon paste electrodes towards [Fe(CN6]3-/[Fe(CN6]4- and quinone/hydroquinone redox couples. Significant attention is paid to the development of the corresponding carbon inks, printing and the surface characterisation of the resulting electrodes by the scanning electron microscopy. An optimization consisted of the selection of the organic solvent, the optimal content of the used polymer with the chosen paste binder, appropriate isolation of electric contact, etc. Very similar properties of the prepared screen-printed electrodes, containing only corresponding carbon powder and 3 % PVC, with their conventional carbon paste electrode and glassy carbon-based electrodes, were observed during their characterisation. Screen-printed electrodes, with the pasting liquid usually provided satisfactory analytical data. Moreover, they can be used in the flow injection analysis and could undoubtedly replace the carbon paste grooved electrodes. It can be assumed that certain progress in the development of electrode materials was achieved by this research.

Browse Title Index

African Journals Online (AJOL)

Issue, Title. Vol 22, No 2 (2008), Voltammetric determination of heparin based on its interaction with malachite green, Abstract PDF. Xueliang Niu, Weili Zhang, Na Zhao, Wei Sun. Vol 22, No 2 (2008), Voltammetric determination of l-cysteic acid on a 1-[4-(ferrocenyl-ethynyl)phenyl]-1-ethanone modified carbon paste ...

L-tryptophan-induced electron transport across supported lipid bilayers: an alkyl-chain tilt-angle, and bilayer-symmetry dependence.

Science.gov (United States)

Sarangi, Nirod Kumar; Patnaik, Archita

2012-12-21

Molecular orientation-dependent electron transport across supported 1,2-dipalmitoyl-sn-glycero-3-phosphocholine (DPPC) lipid bilayers (SLBs) on semiconducting indium tin oxide (ITO) is reported with an aim towards potential nanobiotechnological applications. A bifunctional strategy is adopted to form symmetric and asymmetric bilayers of DPPC that interact with L-tryptophan, and are analyzed by surface manometry and atomic force microscopy. Polarization-dependent real-time Fourier transform infrared reflection absorption spectroscopy (FT-IRRAS) analysis of these SLBs reveals electrostatic, hydrogen-bonding, and cation-π interactions between the polar head groups of the lipid and the indole side chains. Consequently, a molecular tilt arises from the effective interface dipole, facilitating electron transport across the ITO-anchored SLBs in the presence of an internal Fe(CN)(6)(4-/3-) redox probe. The incorporation of tryptophan enhances the voltammetric features of the SLBs. The estimated electron-transfer rate constants for symmetric and asymmetric bilayers (k(s) = 2.0×10(-2) and 2.8×10(-2) s(-1)) across the two-dimensional (2D) ordered DPPC/tryptophan SLBs are higher compared to pure DPPC SLBs (k(s) = 3.2×10(-3) and 3.9×10(-3) s(-1)). In addition, they are molecular tilt-dependent, as it is the case with the standard apparent rate constants k(app)(0), estimated from electrochemical impedance spectroscopy and bipotentiostatic experiments with a Pt ultramicroelectrode. Lower magnitudes of k(s) and k(app)(0) imply that electrochemical reactions across the ITO-SLB electrodes are kinetically limited and consequently governed by electron tunneling across the SLBs. Standard theoretical rate constants (k(th)(0)) accrued upon electron tunneling comply with the potential-independent electron-tunneling coefficient β = 0.15 Å(-1). Insulator-semiconductor transitions moving from a liquid-expanded to a condensed 2D-phase state of the SLBs are noted, adding a new dimension

Mesoporous film of WO{sub 3}–the “sunlight” assisted decomposition of surfactant in wastewater for voltammetric determination of Pb

Energy Technology Data Exchange (ETDEWEB)

Krasnodębska-Ostręga, Beata, E-mail: bekras@chem.uw.edu.pl; Bielecka, Agnieszka; Biaduń, Ewa; Miecznikowski, Krzysztof, E-mail: kmiecz@chem.uw.edu.pl

2016-12-01

Highlights: • The “sun light” decomposed of surfactants: Sodium dodecyl sulfate and Triton™X-114 in the presence of WO{sub 3}. • Mesoporous WO{sub 3} films use for the degradation of surfactant without any reagents. • The developed procedure is suggested to be a no-reagents method of decomposition of added SDS leads to 100% recovery of added Pb (II). - Abstract: In this paper we present the application of “sunlight” assisted digestion in the presence of WO{sub 3} to the decomposition of dissolved organic matter, using the anionic surfactant sodium dodecyl sulfate (SDS) and the nonionic surfactant (1,1,3,3-tetramethylbutyl)phenyl-polyethylene glycol (Triton™X-114) in natural water samples, prior to the determination of traces residues of lead by stripping voltammetry methods. The results of the study showed firstly that the preparation of reproducible WO{sub 3} layers characterized by high mechanical and chemical resistance was possible, and secondly that it was also possible to obtain a high efficiency of decomposition, equal in efficiency to that of the reference method, which was the hydrogen peroxide oxidation assisted by UV, with evaporation nearly to dryness. The developed procedure is suggested to be a no-reagents method for the decomposition of added SDS, leading to 100% recovery of added Pb (II). The anodic stripping voltammetric curves recorded in solution after 4 h irradiation with UV assisted by WO{sub 3} were repeatable and increased linearly with standard additions, but the data finally obtained were incorrect. The curves recorded in solution after “sunlight” assisted digestion in the presence of WO{sub 3} were repeatable, and increased linearly with an increasing of concentration of standard additions (100% recovery of Pb). In the case of a nonionic surfactant, the decomposition time is at least 6 h. The advantage of the proposed method is the fact that the digestion process does not need the addition of any chemicals for the

Effective Area and Charge Density of Iridium Oxide Neural Electrodes

International Nuclear Information System (INIS)

Harris, Alexander R.; Paolini, Antonio G.; Wallace, Gordon G.

2017-01-01

The effective electrode area and charge density of iridium metal and anodically activated iridium has been measured by optical and electrochemical techniques. The degree of electrode activation could be assessed by changes in electrode colour. The reduction charge, activation charge, number of activation pulses and charge density were all strongly correlated. Activated iridium showed slow electron transfer kinetics for reduction of a dissolved redox species. At fast voltammetric scan rates the linear diffusion electroactive area was unaffected by iridium activation. At slow voltammetric scan rates, the steady state diffusion electroactive area was reduced by iridium activation. The steady state current was consistent with a ring electrode geometry, with lateral resistance reducing the electrode area. Slow electron transfer on activated iridium would require a larger overpotential to reduce or oxidise dissolved species in tissue, limiting the electrodes charge capacity but also reducing the likelihood of generating toxic species in vivo.

A screen-printed carbon electrode modified with gold nanoparticles, poly(3,4-ethylenedioxythiophene), poly(styrene sulfonate) and a molecular imprint for voltammetric determination of nitrofurantoin.

Science.gov (United States)

Dechtrirat, Decha; Yingyuad, Peerada; Prajongtat, Pongthep; Chuenchom, Laemthong; Sriprachuabwong, Chakrit; Tuantranont, Adisorn; Tang, I-Ming

2018-04-23

A molecularly imprinted polymer (MIP) and a nanocomposite prepared from gold nanoparticles (AuNP) and poly(3,4-ethylenedioxythiophene)/poly(styrene sulfonate) (PEDOT:PSS) were deposited on a screen-printed carbon electrode (SPCE). The nanocomposite was prepared by one-pot simultaneous in-situ formation of AuNPs and PEDOT:PSS and was then inkjet-coated onto the SPCE. The MIP film was subsequently placed on the modified SPCE by co-electrodeposition of o-phenylenediamine and resorcinol in the presence of the antibiotic nitrofurantoin (NFT). Using differential pulse voltammetry (DPV), response at the potential of ~ 0.1 V (vs. Ag/AgCl) is linear in 1 nM to 1000 nM NFT concentration range, with a remarkably low detection limit (at S/N = 3) of 0.1 nM. This is two orders of magnitude lower than that of the control MIP sensor without the nanocomposite interlayer, thus showing the beneficial effect of AuNP-PEDOT:PSS. The electrode is highly reproducible (relative standard deviation 3.1% for n = 6) and selective over structurally related molecules. It can be re-used for at least ten times and was found to be stable for at least 45 days. It was successfully applied to the determination of NFT in (spiked) feed matrices and gave good recoveries. Graphical abstract Schematic representation of a voltammetric sensor for the determination of nitrofurantoin. The sensor is based on a screen-printed carbon electrode (SPCE) modified with an inkjet-printed gold nanoparticles-poly(3,4-ethylenedioxythiophene):poly(styrene sulfonate) nanocomposite and a molecularly imprinted polymer.

Glass Electrode Calibration for Use in the Voltammetric ...

African Journals Online (AJOL)

A glass electrode (GE) can be successfully employed to measure pH in the study of metal-ligand equilibria by voltammetry at extremely low pH (between 0 and 2); two consecutive strong acid–strong base titrations involving different base concentrations (recommended to avoid corrosion of the GE in very basic solutions) are ...

Use of voltammetry for in vitro equilibrium and transport studies of ionisable drugs

Directory of Open Access Journals (Sweden)

Matej Velicky

2014-09-01

Full Text Available In this review, we will briefly outline the voltammetric investigations of the transfer of ionisable drugs at the interface between two immiscible electrolyte solutions. The voltammetric techniques enable the determination of some key in vitro properties of ionisable drugs, including partition coefficient, diffusion coefficient and membrane permeability. Some successful applications will be highlighted, together with the background methodologies.

Adsorption of organic layers over electrodeposited magnetite (Fe3O4) thin films

International Nuclear Information System (INIS)

Cortes, M.; Gomez, E.; Sadler, J.; Valles, E.

2011-01-01

Research highlights: → Adherent low roughness magnetite films ranging from 80 nm to 3.75 μm-thick were electrodeposited on Au/glass substrates under galvanostatic control. → X-ray diffraction and magnetic measurements corroborates the purity of the electrodeposited magnetite. → Both dodecanethiol and oleic acid are shown to adsorb on the magnetite prepared at low temperature, significantly inducing the hydrophobicity of the surface. → Contact angle and voltammetric measurements, as well as XPS confirm the monolayers formation. - Abstract: The formation of monolayers of two organic compounds (oleic acid and dodecanethiol) over magnetite films was studied. Magnetite films ranging from 80 nm to 3.75 μm-thick were electrodeposited on Au on glass substrates under galvanostatic control, with deposition parameters optimized for minimum surface roughness. Films were characterised by SEM and AFM, showing granular deposits with a low rms roughness of 5-40 nm measured over an area of 1 μm 2 . The growth rate was estimated by measuring cross-sections of the thin films. Pure magnetite with an fcc structure is observed in XRD diffractograms. The adsorption of both oleic acid and dodecanethiol on the magnetite films was tested by immersing them in ethanol solutions containing the organic molecules, for different deposition time, temperature and cleaning procedure. Monolayer formation in both cases was studied by contact angle and voltammetric measurements, as well as XPS.

A strategy to promote the electroactive platform adopting poly(o-anisidine)-silver nanocomposites probed for the voltammetric detection of NADH and dopamine.

Science.gov (United States)

Sangamithirai, D; Munusamy, S; Narayanan, V; Stephen, A

2017-11-01

A study on the voltammetric detection of NADH (β-nicotinamide adenine dinucleotide), Dopamine (DA) and their simultaneous determination is presented in this work. The electrochemical sensor was fabricated with the hybrid nanocomposites of poly(o-anisidine) and silver nanoparticles prepared by simple and cost-effective insitu chemical oxidative polymerization technique. The nanocomposites were synthesized with different (w/w) ratios of o-anisidine and silver by increasing the amount of o-anisidine in each, by keeping silver at a fixed quantity. The XRD patterns revealed the semi-crystalline nature of poly(o-anisidine) and the face centered cubic structure of silver. The presence of silver in its metallic state and the formation of nanocomposite were established by XPS analysis. Raman studies suggested the presence of site-selective interaction between poly(o-anisidine) and silver. HRTEM studies revealed the formation of polymer matrix type nanocomposite with the embedment of silver nanoparticles. The sensing performance of the materials were studied via cyclic voltammetry, differential pulse voltammetry and chronoamperometry techniques. Fabricated sensor with 3:1 (w/w) ratio of poly(o-anisidine) and silver exhibited good catalytic activity towards the detection of NADH and DA in terms of potential and current response, when compared to others. Several important electrochemical parameters regulating the performance of the sensor have been evaluated. Under the optimum condition, differential pulse voltammetry method exhibited the linear response in the range of 0.03 to 900μM and 5 to 270μM with a low detection limit of 0.006μM and 0.052μM for NADH and DA, respectively. The modified electrodes exhibited good sensitivity, stability, reproducibility and selectivity with well-separated oxidation peaks for NADH and DA in the simultaneous determination of their binary mixture. The analytical performance of the nanocomposite as an electrochemical sensor was also

Electroanalysis of cardioselective beta-adrenoreceptor blocking agent acebutolol by disposable graphite pencil electrodes with detailed redox mechanism

Directory of Open Access Journals (Sweden)

Atmanand M. Bagoji

2016-12-01

Full Text Available A simple economic graphite pencil electrode (GPE was used for analysis of cardioselective, hydrophilic-adrenoreceptor blocking agent, acebutolol (ACBT using the cyclic voltammetric, linear sweep voltammetric, differential pulse voltammetric (DPV, and square-wave voltammetric (SWV techniques. The dependence of the current on pH, concentration, and scan rate was investigated to optimize the experimental condition for determination of ACBT. The electrochemical behavior of the ACBT at GPE was a diffusion-controlled process. A probable electro-redox mechanism was proposed. Under the optimal conditions, the anodic peak current was linearly proportional to the concentration of ACBT in the range from 1.00 to 15.0 μM with a limit of detection 1.26 × 10−8 M for DPV and 1.28 × 10−8 M for the SWV. This method was applied for quantitative determination of the ACBT levels in urine as real samples. The obtained recovery ranges for ACBT in urine were from 95.4 to101% as found by the standard addition technique. Further interference study was also carried with some common interfering substances.

Monitoring of beer fermentation based on hybrid electronic tongue.

Science.gov (United States)

Kutyła-Olesiuk, Anna; Zaborowski, Michał; Prokaryn, Piotr; Ciosek, Patrycja

2012-10-01

Monitoring of biotechnological processes, including fermentation is extremely important because of the rapidly occurring changes in the composition of the samples during the production. In the case of beer, the analysis of physicochemical parameters allows for the determination of the stage of fermentation process and the control of its possible perturbations. As a tool to control the beer production process a sensor array can be used, composed of potentiometric and voltammetric sensors (so-called hybrid Electronic Tongue, h-ET). The aim of this study is to apply electronic tongue system to distinguish samples obtained during alcoholic fermentation. The samples originate from batch of homemade beer fermentation and from two stages of the process: fermentation reaction and maturation of beer. The applied sensor array consists of 10 miniaturized ion-selective electrodes (potentiometric ET) and silicon based 3-electrode voltammetric transducers (voltammetric ET). The obtained results were processed using Partial Least Squares (PLS) and Partial Least Squares-Discriminant Analysis (PLS-DA). For potentiometric data, voltammetric data, and combined potentiometric and voltammetric data, comparison of the classification ability was conducted based on Root Mean Squared Error (RMSE), sensitivity, specificity, and coefficient F calculation. It is shown, that in the contrast to the separately used techniques, the developed hybrid system allowed for a better characterization of the beer samples. Data fusion in hybrid ET enables to obtain better results both in qualitative analysis (RMSE, specificity, sensitivity) and in quantitative analysis (RMSE, R(2), a, b). Copyright © 2012 Elsevier B.V. All rights reserved.

Voltammetric Investigation Of Hydrothermal Iron Speciation

Directory of Open Access Journals (Sweden)

Charlotte eKleint

2016-05-01

Full Text Available Hydrothermal vent fluids are highly enriched in iron (Fe compared to ambient seawater, and organic ligands may play a role in facilitating the transport of some hydrothermal Fe into the open ocean. This is important since Fe is a limiting micronutrient for primary production in large parts of the world`s surface ocean. We have investigated the concentration and speciation of Fe in several vent fluid and plume samples from the Nifonea vent field, Coriolis Troughs, New Hebrides Island Arc, South Pacific Ocean using competitive ligand exchange - adsorptive cathodic stripping voltammetry (CLE - AdCSV with salicylaldoxime (SA as the artificial ligand. Our results for total dissolved Fe (dFe in the buoyant hydrothermal plume samples showed concentrations up to 3.86 µM dFe with only a small fraction between 1.1% and 11.8% being chemically labile. Iron binding ligand concentrations ([L] were found in µM level with strong conditional stability constants up to log K[L],Fe3+ of 22.9. Within the non-buoyant hydrothermal plume above the Nifonea vent field, up to 84.7% of the available Fe is chemically labile and [L] concentrations up to 97 nM were measured. [L] was consistently in excess of Felab, indicating that all available Fe is being complexed, which in combination with high Felab values in the non-buoyant plume, signifies that a high fraction of hydrothermal dFe is potentially being transported away from the plume into the surrounding waters, contributing to the global oceanic Fe budget.

Determination of polyphenol content and colour index in wines through PEDOT-modified electrodes.

Science.gov (United States)

Pigani, Laura; Rioli, Cristina; Foca, Giorgia; Ulrici, Alessandro; Seeber, Renato; Terzi, Fabio; Zanardi, Chiara

2016-10-01

Poly(3,4-ethylenedioxythiophene)-modified electrodes have been used for the estimation of the polyphenolic content and of the colour index of different samples of wines. Synthetic wine solutions, prepared with different amount of oenocyanins, have been analysed spectrophotometrically and electrochemically in order to find a correlation between the total polyphenolic content or colour index and the current peak. The regression curves obtained have been used as external calibration lines for the analysis of several commercial wines, ranging from white to dark red wines. In this way, a rapid estimation of the total polyphenolic content and of the colour index may be accomplished from a single voltammetric measurement. Furthermore, principal component analysis has also been used to evaluate the effect of total polyphenolic content and colour index on the whole voltammetric signals within a selected potential range, both for the synthetic solutions and for the commercial products. Graphical abstract Electrochemical sensors for the rapid determination of colour index and polyphenol content in wines.

Construction and characterization of nonenzymatic glucose sensor from recycling of Co, Cu and Mn from spent batteries

International Nuclear Information System (INIS)

Selvatici, Livia Serra; Favalessa, Luiza Botan; Loureiro, Eduardo dos Santos; Dixini, Pedro Vitor Morbach; Freitas, Marcos Benedito Jose de; Celante, Vinicius Guilherme

2016-01-01

Full text: In this work, Co, Cu and MnO 2 films were synthesized from the electrochemical recycling of spent Li-ion and alkaline batteries and applied as non-enzymatic electrochemical sensors for glucose determination in aqueous solution. The batteries were dismantled, physically separated into different constituents and leached solution of acetic acid 3:1 v/v. The films were synthesized in potentiostatic condition with E =-0.90 V and fixed charge density of 10 C.cm -2 on glassy carbon substrate with area equal to 3.0 mm 2 . Measurements of X-ray diffraction showed the Co structures (111), Cu (101) and MnO 2 (110). By analysis of scanning electron microscopy, a homogeneous coating of the surface was observed without the presence of surface irregularities. For energy dispersive X-ray, Co, Cu, Mn and O were observed. These films were subsequently used in determining glucose in aqueous solution by measures of successive voltammetric cycles in solutions of concentration varying from 0.1 to 0.5 g/l. These solutions were related to anodic peak current (I peak ), relative oxidation of glucose in glucolactona, the concentration of the solution, obtaining a linear correlation coefficient of 0.989. The sensor stability was measured in 20 voltammetric cycles in each solution, obtaining a correlation coefficient equal to 0978, being stable in the measurements. (author)

Voltammetric determination of metal impurities on semiconductor surface

International Nuclear Information System (INIS)

Knyazeva, E.P.; Mokrousov, G.M.; Volkova, V.N.

1995-01-01

A modification of voltamperometric method used for analysis of semiconductor surfaces which make it possible to exclude a contact between surface and background solution. This technique is based on solubility of elemental metal forms in low melting electroconductor systems (e.g., in mercury. The voltampere characteristics of amalgams formed are then studied. The suggested method is simple, rapid, and makes it possible to perform a nondestructive qualitative analysis of the sample surface area measuring about 10 -3 cm -2 and more. 4 refs.; 2 figs

Scanning electrochemical microscopy. 47. Imaging electrocatalytic activity for oxygen reduction in an acidic medium by the tip generation-substrate collection mode.

Science.gov (United States)

Fernández, José L; Bard, Allen J

2003-07-01

The oxygen reduction reaction (ORR) in acidic medium was studied on different electrode materials by scanning electrochemical microscopy (SECM) operating in a new variation of the tip generation-substrate collection mode. An ultramicroelectrode tip placed close to the substrate electrode oxidizes water to oxygen at a constant current. The substrate is held at a potential where the tip-generated oxygen is reduced and the resulting substrate current is measured. By changing the substrate potential, it is possible to obtain a polarization (current-potential) curve, which depends on the electrocatalytic activity of the substrate material. The main difference between this mode and the classical feedback SECM mode of operation is that the feedback diffusion process is not required for the measurement, allowing its application for studying the ORR in acidic solutions. Activity-sensitive images of heterogeneous surfaces, e.g., with Pt and Au electrodes, were obtained from the substrate current when the x-y plane was scanned with the tip. The usefulness of this technique for imaging electrocatalytic activity of smooth metallic electrodes and of highly dispersed fuel cell-type electrocatalysts was demonstrated. The application of this method to the combinatorial chemical analysis of electrode materials and electrocatalysts is discussed.

Amorphous silicon carbide ultramicroelectrode arrays for neural stimulation and recording

Science.gov (United States)

Deku, Felix; Cohen, Yarden; Joshi-Imre, Alexandra; Kanneganti, Aswini; Gardner, Timothy J.; Cogan, Stuart F.

2018-02-01

Objective. Foreign body response to indwelling cortical microelectrodes limits the reliability of neural stimulation and recording, particularly for extended chronic applications in behaving animals. The extent to which this response compromises the chronic stability of neural devices depends on many factors including the materials used in the electrode construction, the size, and geometry of the indwelling structure. Here, we report on the development of microelectrode arrays (MEAs) based on amorphous silicon carbide (a-SiC). Approach. This technology utilizes a-SiC for its chronic stability and employs semiconductor manufacturing processes to create MEAs with small shank dimensions. The a-SiC films were deposited by plasma enhanced chemical vapor deposition and patterned by thin-film photolithographic techniques. To improve stimulation and recording capabilities with small contact areas, we investigated low impedance coatings on the electrode sites. The assembled devices were characterized in phosphate buffered saline for their electrochemical properties. Main results. MEAs utilizing a-SiC as both the primary structural element and encapsulation were fabricated successfully. These a-SiC MEAs had 16 penetrating shanks. Each shank has a cross-sectional area less than 60 µm2 and electrode sites with a geometric surface area varying from 20 to 200 µm2. Electrode coatings of TiN and SIROF reduced 1 kHz electrode impedance to less than 100 kΩ from ~2.8 MΩ for 100 µm2 Au electrode sites and increased the charge injection capacities to values greater than 3 mC cm‑2. Finally, we demonstrated functionality by recording neural activity from basal ganglia nucleus of Zebra Finches and motor cortex of rat. Significance. The a-SiC MEAs provide a significant advancement in the development of microelectrodes that over the years has relied on silicon platforms for device manufacture. These flexible a-SiC MEAs have the potential for decreased tissue damage and reduced foreign body response. The technique is promising and has potential for clinical translation and large scale manufacturing.

Examinations of content of heavy metals in municipal solid waste and produced compost

International Nuclear Information System (INIS)

Golimowski, J.; Tykarska, A.; Orzechowska, K.

1993-01-01

The basic methods of utilization of municipal solid waste are biothermic and aerobic methods to compost. The content of heavy metals in composts depends on the initial their content in wastes as well as on the compost process. The voltammetric method has been applied for measurement of concentration of Zn, Cd, Pb, Cu, Cr, Ni and Hg in the waste and composts samples. (author). 24 refs, 2 figs, 3 tabs

Determination of the stoichiometric rate in UO2 samples

International Nuclear Information System (INIS)

Moura, Sergio C.; Lima, Nelson B. de; Sassine, Andre; Bustillos, Jose Oscar Vega

2000-01-01

The gravimetric and voltammetric methods for determination of non-stoichiometric O/U ratio in uranium dioxide used as nuclear fuel are discussed in this work. The oxidation of uranium oxide is very complex due to many phase changes. Gravimetric and voltammetric methods do not detect phase changes. The results of this work shown that, to evaluate both methods is requiring to be done Rietveld methods by X-ray diffraction data to identify the uranium oxide phase changes. (author)

Study of non stoichiometric uranium dioxide samples (UO2)

International Nuclear Information System (INIS)

Moura, Sergio C.; Lima, Nelson B. de; Bustillos, Jose O.V.

1999-01-01

The gravimetric and voltammetric methods for determination of non-stoichiometric O/U ratio in uranium dioxide used as nuclear fuel are discussed in this work. The oxidation of uranium oxide is very complex due to many phase changes. gravimetric and voltammetric methods do not detect phase changes. The results of this work shown that, to evaluate both methods is requiring to be done Rietveld methods by x-ray diffraction data to identify the uranium oxide phase changes. (author)

Direct in situ measurement of dissolved zinc in the presence of zinc oxide nanoparticles using anodic stripping voltammetry.

Science.gov (United States)

Jiang, Chuanjia; Hsu-Kim, Heileen

2014-11-01

The wide use of metal-based nanomaterials such as zinc oxide (ZnO) nanoparticles (NPs) has generated concerns regarding their environmental and health risks. For ZnO NPs, their toxicity in aquatic systems often depends on the release of dissolved zinc species, and the rate of dissolution is influenced by water chemistry, including the presence of zinc-chelating ligands. A challenge, however, remains in quantifying the dissolution of ZnO NPs, particularly for time scales that are short enough to determine rates. This paper reports the application of anodic stripping voltammetry (ASV) with a hanging mercury drop electrode to directly measure the concentration of dissolved zinc in ZnO NP suspensions, without separation of the ZnO NPs from the aqueous phase. The effects of the deposition time and the electrochemical potential scan rate on the ASV measurement were consistent with expectations for dissolved phase measurements. The dissolved zinc concentration measured by ASV ([Zn]ASV) was compared with that measured by inductively coupled plasma mass spectrometry (ICP-MS) after ultracentrifugation ([Zn]ICP-MS), for four types of ZnO NPs with different coatings and primary particle diameters. For small ZnO NPs (4-5 nm), [Zn]ASV was 20% higher than [Zn]ICP-MS, suggesting that these small NPs contributed to the voltammetric measurement. For larger ZnO NPs (approximately 20 nm), [Zn]ASV was (79 ± 19)% of [Zn]ICP-MS, despite the high concentrations of ZnO NPs in suspension. Using ASV, the dissolution of ZnO NPs was studied, with or without Suwannee River Fulvic Acid (SRFA). Although SRFA diminished the ASV stripping current, dissolution of 20 nm ZnO NPs was significantly promoted at high fulvic acid to ZnO NP ratios. The ASV method described in this paper provides a useful tool for studying the dissolution kinetics of ZnO NPs in complex environmental matrices.

Electrochemical determination of copper ions in spirit drinks using carbon paste electrode modified with biochar.

Science.gov (United States)

Oliveira, Paulo Roberto; Lamy-Mendes, Alyne C; Rezende, Edivaltrys Inayve Pissinati; Mangrich, Antonio Sálvio; Marcolino, Luiz Humberto; Bergamini, Márcio F

2015-03-15

This work describes for first time the use of biochar as electrode modifier in combination with differential pulse adsorptive stripping voltammetric (DPAdSV) techniques for preconcentration and determination of copper (II) ions in spirit drinks samples (Cachaça, Vodka, Gin and Tequila). Using the best set of the experimental conditions a linear response for copper ions in the concentration range of 1.5 × 10(-6) to 3.1 × 10(-5) mol L(-1) with a Limit of Detection (LOD) of 4.0 × 10(-7) mol L(-1). The repeatability of the proposed sensor using the same electrode surface was measured as 3.6% and 6.6% using different electrodes. The effect of foreign species on the voltammetric response was also evaluated. Determination of copper ions content in different samples of spirit drinks samples was also realized adopting inductively coupled plasma optical emission spectroscopy (ICP-OES) and the results achieved are in agreement at a 95% of confidence level. Copyright © 2014 Elsevier Ltd. All rights reserved.

New and highly sensitive assay for L-5-hydroxytryptophan decarboxylase activity by high-performance liquid chromatography-voltammetry.

Science.gov (United States)

Rahman, M K; Nagatsu, T; Kato, T

1980-12-12

This paper describes a new, inexpensive and highly sensitive assay for aromatic L-amino acid decarboxylase (AADC) activity, using L-5-hydroxytryptophan (L-5-HTP) as substrate, in rat and human brains and serum by high-performance liquid chromatography (HPLC) with voltammetric detection. L-5-HTP was used as substrate and D-5-HTP for the blank. After isolating serotonin (5-HT) formed enzymatically from L-5-HTP on a small Amberlite CG-50 column, the 5-HT was eluted with hydrochloric acid and assayed by HPLC with a voltammetric detector. N-Methyldopamine was added to each incubation mixture as an internal standard. This method is sensitive enough to measure 5-HT, formed by the enzyme, 100 fmol to 140 pmol or more. An advantage of this method is that one can incubate the enzyme for longer time (up to 150 min), as compared with AADC assay using L-DOPA as substrate, resulting in a very high sensitivity. By using this new method, AADC activity was discovered in rat serum.

A novel type of electrochemical sensor based on ferromagnetic carbon-encapsulated iron nanoparticles for direct determination of hemoglobin in blood samples.

Science.gov (United States)

Matysiak, Edyta; Donten, Mikolaj; Kowalczyk, Agata; Bystrzejewski, Michal; Grudzinski, Ireneusz P; Nowicka, Anna M

2015-02-15

An effective, fast, facile and direct electrochemical method of determination of hemoglobin (Hb) in blood sample without any sample preparation is described. The method is accomplished by using the ferromagnetic electrode modifier (carbon-encapsulated iron nanoparticles) and an external magnetic field. The successful voltammetric determination of hemoglobin is achieved in PBS buffer as well as in the whole blood sample. The obtained results show the excellent electroactivity of Hb. The measurements are of high sensitivity and good reproducibility. The detection limit is estimated to be 0.7 pM. The electrochemical determination data were compared with the gravimetric data obtained with a quartz crystal microbalance. The agreement between these results is very good. The changes of the electrode surface morphology before and after Hb detection are monitored by electron microscopy. The functionality of the electrochemical sensor is tested with human and rat blood samples. The concentration of hemoglobin in the blood samples determined by using voltammetric/gravimetric detection is in perfect agreement with the data obtained from typical clinical analysis. Copyright © 2014 Elsevier B.V. All rights reserved.

QUANTIFICATION OF LEAD AND CADMIUM IN POULTRY AND BIRD GAME MEAT BY SQUARE WAVE ANODIC STRIPPING VOLTAMMETRY

OpenAIRE

2011-01-01

Abstract 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 have been found suitable to reduce ma...

Evaluation of the Standard Ion Transfer Potentials for PVC Plasticized Membranes from Voltammetric Measurements

Czech Academy of Sciences Publication Activity Database

Langmaier, Jan; Stejskalová, Květoslava; Samec, Zdeněk

2001-01-01

Roč. 496, č. 1 (2001), s. 143-147 ISSN 0022-0728. [Symposium in Kyoto. Kyoto, 02.03.2000] R&D Projects: GA AV ČR IAA4040902 Institutional research plan: CEZ:AV0Z4040901 Keywords : ion voltammetry * PVC plasticized membrane * standard ion transfer potential Subject RIV: CG - Electrochemistry Impact factor: 1.960, year: 2001

Promotion of the oxidation of carbon monoxide at stepped platinum single-crystal electrodes in alkaline media by lithium and beryllium cations.

Science.gov (United States)

Stoffelsma, Chantal; Rodriguez, Paramaconi; Garcia, Gonzalo; Garcia-Araez, Nuria; Strmcnik, Dusan; Marković, Nenad M; Koper, Marc T M

2010-11-17

The role of alkali cations (Li(+), Na(+), K(+), Cs(+), and Be(2+)) on the blank voltammetric response and the oxidative stripping of carbon monoxide from stepped Pt single-crystal electrodes in alkaline media has been investigated by cyclic voltammetry. A strong influence of the nature of the cation on both the blank voltammetric profile and the CO oxidation is observed and related to the influence of the cation on the specific adsorption of OH on the platinum surface. Especially Li(+) and Be(2+) cations markedly affect the adsorption of OH and thereby have a significant promoting effect on CO(ads) oxidation. The voltammetric experiments suggest that, on Pt(111), the influence of Li(+) (and Be(2+)) is primarily through a weakening of the repulsive interactions between the OH in the OH adlayer, whereas in the presence of steps also, the onset of OH adsorption is at a lower potential, both on steps and on terraces.

Sensitive determination of citrinin based on molecular imprinted electrochemical sensor

Science.gov (United States)

Atar, Necip; Yola, Mehmet Lütfi; Eren, Tanju

2016-01-01

In this report, a novel molecular imprinted voltammetric sensor based on glassy carbon electrode (GCE) modified with platinum nanoparticles (PtNPs) involved in a polyoxometalate (H3PW12O40, POM) functionalized reduced graphene oxide (rGO) was prepared for the determination of citrinin (CIT). The developed surfaces were characterized by using scanning electron microscope (SEM), transmission electron microscope (TEM), X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD) method. CIT imprinted GCE was prepared via electropolymerization process of 80.0 mM pyrrole as monomer in the presence of phosphate buffer solution (pH 6.0) containing 20.0 mM CIT. The linearity range and the detection limit of the developed method were calculated as 1.0 × 10-12-1.0 × 10-10 M and 2.0 × 10-13 M, respectively. In addition, the voltammetric sensor was applied to rye samples. The stability and selectivity of the voltammetric sensor were also reported.

A DNA biosensor based on the electrocatalytic oxidation of amine by a threading intercalator

International Nuclear Information System (INIS)

Gao Zhiqiang; Tansil, Natalia

2009-01-01

An electrochemical biosensor for the detection of DNA based a peptide nucleic acid (PNA) capture probe (CP) modified indium tin oxide electrode (ITO) is described in this report. After hybridization, a threading intercalator, N,N'-bis[(3-propyl)-imidazole]-1,4,5,8-naphthalene diimide (PIND) imidazole complexed with Ru(bpy) 2 Cl (PIND-Ru, bpy = 2,2'-bipyridine), was introduced to the biosensor. PIND-Ru selectively intercalated to double-stranded DNA (ds-DNA) and became immobilized on the biosensor surface. Voltammetric tests showed highly stable and reversible electrochemical oxidation/reduction processes and the peak currents can directly be utilized for DNA quantification. When the tests were conducted in an amine-containing medium, Tris-HCl buffer for example, a remarkable improvement in the voltammetric response and noticeable enhancements of voltammetric and amperometric sensitivities were observed due to the electrocatalytic activity of the [Ru(bpy) 2 Cl] redox moieties. Electrocatalytic current was observed when as little as 3.0 attomoles of DNA was present in the sample solution

Square-wave voltammetric determination of fungicide fenfuram in real samples on bare boron-doped diamond electrode, and its corrosion properties on stainless steels used to produce agricultural tools

International Nuclear Information System (INIS)

Brycht, Mariola; Skrzypek, Sławomira; Kaczmarska, Kinga; Burnat, Barbara; Leniart, Andrzej; Gutowska, Natalia

2015-01-01

Graphical abstract: Display Omitted -- Highlights: • A bare boron-doped diamond electrode was first used to determine fenfuram. • A sensitive voltammetric procedure for the determination of fenfuram was developed. • The sensor showed high sensitivity, selectivity, and wide linear range. • The procedure was successfully applied to detect fenfuram in real samples. • The effect of fenfuram on the uniform and pitting corrosion of steel was stated. -- Abstract: A simple, selective, and sensitive electroanalytical method for the determination of a novel fungicide, fenfuram (Fnf), on a bare boron-doped diamond electrode (BDDE) using square-wave voltammetry (SWV) was developed. For the first time, the electrochemical oxidation of Fnf at BDDE at about 1.5 V vs. Ag/AgCl reference electrode in 0.35 mol L −1 sulfuric acid was investigated. To select the optimum experimental conditions, the effects of the supporting electrolyte, pH, frequency, amplitude, and step potential were studied. The developed method allowed the determination of Fnf in the concentration range of 2.4 × 10 −5 to 2.6 × 10 −4 mol L −1 (LOD = 6.3 × 10 −6 mol L −1 , LOQ = 2.1 × 10 −5 mol L −1 ). The validation of the method was carried out. The proposed procedure was successfully applied to determine Fnf in the spiked natural water samples collected from Polish rivers and in the spiked triticale seed samples by the standard addition method. To understand the Fnf electrode mechanism, the cyclic voltammetry (CV) technique was applied. The oxidation mechanism was also confirmed using mass spectrometry with the electrospray ionization (ESI-MS) technique. Using electrochemical techniques, the effect of Fnf on the corrosion properties of stainless steel which is used to produce agricultural tools was studied

Salts purification and redox potential measurement for the molten LiF-ThF4-UF4 mixture

International Nuclear Information System (INIS)

Afonichkin, V.; Bovet, A.; Shishkin, V.

2010-01-01

The 'dry' techniques of producing and clearing of some metals fluorides, their mixtures and cakes of a given composition obtained without usage gaseous HF for experiments under the Project ISTC No. 3749 are developed. The products of synthesizing and purification of oxygen-containing compounds, are studied by methods X-ray diffraction analysis, gravimetry or IR spectrometry. The experimental studies confirmed that solid NH 4 HF 2 can be efficiently used instead of an unsafe and corrosive HF gas for removal of oxygen-containing impurities from metal fluorides and for conversion of uranium and thorium dioxides to anhydrous tetra-fluorides. These processes do not require expensive equipment and special measures of safety. The electrochemical behavior of UF 4 solutions in a melt 77 LiF-23ThF 4 (mole%) was studied by cyclic voltammetry. Formal analysis of the obtained dependencies showed that in our experimental conditions the recharge U(IV) to U(III) is qualitatively consistent with voltammetric criteria and can be classified as reversible. However, the results of mathematical processing of voltammograms show that the basic calculated characteristics of this reaction differ from the theoretical values corresponding one-electron process controlled by the diffusion rate. This indicates quasi-reversibility of the studied reaction. (authors)

Characterization of carbon nanotubes decorated with NiFe2O4 magnetic nanoparticles as a novel electrochemical sensor: Application for highly selective determination of sotalol using voltammetry

International Nuclear Information System (INIS)

Ensafi, Ali A.; Allafchian, Ali R.; Rezaei, B.; Mohammadzadeh, R.

2013-01-01

A magnetic nano‐composite of multiwall carbon nanotube, decorated with NiFe 2 O 4 nanoparticles, was synthesized with citrate sol–gel method. The multiwall carbon nanotubes decorated with NiFe 2 O 4 nanoparticles (NiFe 2 O 4 –MWCNTs) were characterized with different methods such as Fourier transform infrared spectroscopy (FT‐IR), transmission electron microscopy (TEM), atomic force microscopy (AFM), vibrating sample magnetometer (VSM), cyclic voltammetry (CV), and electrochemical impedance spectroscopy (EIS). The new nano-composite acts as a suitable electrocatalyst for the oxidation of sotalol at a potential of 500 mV at the surface of the modified electrode. Linear sweep voltammetry exhibited two wide linear dynamic ranges of 0.5–1000 μmol L −1 sotalol with a detection limit of 0.09 μmol L −1 . The modified electrode was used as a novel electrochemical sensor for the determination of sotalol in real samples such as pharmaceutical, patient and safe human urine. - Graphical abstract: Multiwall carbon nanotube, decorated with NiFe 2 O 4 nanoparticles, was prepared using citrate sol–gel method. We characterized the new nanoparticles with different spectroscopic and voltammetric methods. The nano sensor was used as a voltammetric sensor for the determination of trace amounts of sotalol at pH 7.0. Highlights: ► We synthesized and prepared new sensor, multiwall carbon nanotubes decorated with NiFe 2 O 4 . ► Several spectroscopic and voltammetric methods were used to study its characteristics. ► The nanoparticles act as suitable electrocatalyst for the oxidation of sotalol. ► Sotalol could be measured as low as 0.09 μmol L −1 using linear sweep voltammetry.

Photoinducedly electrochemical preparation of Prussian blue film and electrochemical modification of the film with cetyltrimethylammonium cation

Energy Technology Data Exchange (ETDEWEB)

Liu Shouqing, E-mail: shouqing_liu@hotmail.co [Key Laboratory of Environmental Functional Materials of Jiangsu Province, College of Chemistry and Bioengineering, Suzhou University of Science and Technology, Suzhou 215009 (China); Li Hua; Sun Weihui; Wang Xiaomei; Chen Zhigang [Key Laboratory of Environmental Functional Materials of Jiangsu Province, College of Chemistry and Bioengineering, Suzhou University of Science and Technology, Suzhou 215009 (China); Xu Jingjuan; Ju Huangxian; Chen Hongyuan [Key Laboratory of Analytical Chemistry for Life Science, Ministry of Education, Nanjing University, Nanjing 210093 (China)

2011-04-15

Research highlights: {yields} Cetyltrimethylammonium cations work as counter ions in Prussian blue film was observed and confirmed by cyclic voltammetry, Fourier transform infrared spectroscopy, X-ray powder diffraction measurements, scanning electronic microscopy and transmission electron microscope for the first time. {yields} Because the cetyltrimethylammonium cations in Prussian blue film are hydrophobic, the Prussian blue film is very stable even in alkali solution, which provides a technical basis for fabrication of stable biosensors. - Abstract: This work presents a photoinducedly electrochemical preparation of Prussian blue from a single sodium nitroprusside and insertion of cetyltrimethylammonium cations into Prussian blue as counter ions. The product of photoinducedly electrochemical reactions has a couple of voltammetric peaks at E{sup o} = 0.266 V in 0.2 mol l{sup -1} KCl solution, the measurements of X-ray powder diffraction and FT-IR spectroscopy show that it is Prussian blue (PB). The formation mechanism of a pre-photochemical reaction and subsequent electrochemical reaction is suggested. The cyclic voltammetric treatment of the freshly as-prepared PB film in 1.0 mmol l{sup -1} cetyltrimethylammonium (CTA) bromide solution leads to the insertion of cetyltrimethylammonium cations into the channels of Prussian blue, which substitutes for potassium ions as counter ions in Prussian blue. The Prussian blue containing CTA counter ions shows two couples of voltammetric peaks at E{sup o} = -0.106 V and E{sup o} = 0.249 V in 0.2 mol l{sup -1} KCl solution containing 1.0 mmol l{sup -1} cetyltrimethylammonium bromide. Compared with the electrochemical behaviors of KFeFe(CN){sub 6} in 0.1 mol l{sup -1} KOH alkali solution, CTAFeFe(CN){sub 6} shows relatively durable voltammetric currents due to the hydrophobic effects of cetyltrimethylammonium. The diffusion coefficients for CTA and potassium cations were estimated to be D{sub CTA} 1.25 x 10{sup -12} cm{sup 2} s

Resistive and magnetoresistive properties of BiSrCaCuO granulated films

International Nuclear Information System (INIS)

Mal'tsev, V.A.; Kulikovskij, A.V.; Kustikov, E.V.; Morozov, D.Yu.; Sokolov, Yu.S.

1995-01-01

Transport properties of superconducting bridges produced by laser etching of granulated films BiSrCaCuO have been studied. Analysis of nonlinear voltammetric characteristics of the bridges permits making the conclusion on the change in the character of conductivity (two-dimensional-three dimensional system), when approaching the critical point. Measurements of magnetoresistance of the samples suggest a possibility of application of high-temperature superconducting bridges in Bi-system as sensors of weak magnetic fields. 11 refs.; 4 figs

Controlled sp(2) Functionalization of Boron Doped Diamond as a Route for the Fabrication of Robust and Nernstian pH Electrodes.

Science.gov (United States)

Ayres, Zoë J; Borrill, Alexandra J; Newland, Jonathan C; Newton, Mark E; Macpherson, Julie V

2016-01-05

The development of a voltammetric boron doped diamond (BDD) pH sensor is described. To obtain pH sensitivity, laser micromachining (ablation) is utilized to introduce controlled regions of sp(2) carbon into a high quality polycrystalline BDD electrode. The resulting sp(2) carbon is activated to produce electrochemically reducible quinone groups using a high temperature acid treatment, followed by anodic polarization. Once activated, no further treatment is required. The quinone groups show a linear (R(2) = 0.999) and Nernstian (59 mV/(pH unit)) pH-dependent reductive current-voltage response over a large analyzable pH range, from pH 2 to pH 12. Using the laser approach, it is possible to optimize sp(2) coverage on the BDD surface, such that a measurable pH response is recorded, while minimizing background currents arising from oxygen reduction reactions on sp(2) carbon in the potential region of interest. This enables the sensor to be used in aerated solutions, boding well for in situ analysis. The voltammetric response of the electrode is not compromised by the presence of excess metal ions such as Pb(2+), Cd(2+), Cu(2+), and Zn(2+). Furthermore, the pH sensor is stable over a 3 month period (the current time period of testing), can be stored in air between measurements, requires no reactivation of the surface between measurements, and can be reproducibly fabricated using the proposed approach. The efficacy of this pH sensor in a real-world sample is demonstrated with pH measurements in U.K. seawater.

Electronic properties of thermally formed thin iron oxide films

International Nuclear Information System (INIS)

Wielant, J.; Goossens, V.; Hausbrand, R.; Terryn, H.

2007-01-01

The oxide layer, present between an organic coating and the substrate, guarantees adhesion of the coating and plays a determinating role in the delamination rate of the organic coating. The purpose of this study is to compare the resistive and semiconducting properties of thermal oxides formed on steel in two different atmospheres at 250 deg. C: an oxygen rich atmosphere, air, and an oxygen deficient atmosphere, N 2 . In N 2 , a magnetite layer grows while in air a duplex oxide film forms composed by an inner magnetite layer and a thin outer hematite scale. The heat treatment for different amounts of time at high temperature was used as method to sample the thickness variation and change in electronic and semiconducting properties of the thermal oxide layers. Firstly, linear voltammetric measurements were performed to have a first insight in the electrochemical behavior of the thermal oxides in a borate buffer solution. Electrochemical impedance spectroscopy in the same buffer combined with the Mott-Schottky analysis were used to determine the semiconducting properties of the thermal oxides. By spectroscopic ellipsometry (SE) and atomic force microscopy (AFM), respectively, the thickness and roughness of the oxide layers were determined supporting the physical interpretation of the voltammetric and EIS data. These measurements clearly showed that oxide layers with different constitution, oxide resistance, flatband potential and doping concentration can be grown by changing the atmosphere

Increased sensitivity of anodic stripping voltammetry at the hanging mercury drop electrode by ultracathodic deposition

Energy Technology Data Exchange (ETDEWEB)

Rodrigues, Jose A.; Rodrigues, Carlos M.; Almeida, Paulo J.; Valente, Ines M.; Goncalves, Luis M. [Requimte - Departamento de Quimica e Bioquimica, Faculdade de Ciencias, Universidade do Porto, Rua do Campo Alegre, no. 687, 4169-007 Porto (Portugal); Compton, Richard G. [Department of Chemistry, Physical and Theoretical Chemistry Laboratory, Oxford University, South Parks Road, Oxford OX1 3QZ (United Kingdom); Barros, Aquiles A., E-mail: ajbarros@fc.up.pt [Requimte - Departamento de Quimica e Bioquimica, Faculdade de Ciencias, Universidade do Porto, Rua do Campo Alegre, no. 687, 4169-007 Porto (Portugal)

2011-09-09

Highlights: {yields} At very cathodic accumulation potentials (overpotential deposition) the voltammetric signals of Zn{sup 2+}, Cd{sup 2+}, Pb{sup 2+} and Cu{sup 2+} increase. {yields} 5 to 10-fold signal increase is obtained. {yields} This effect is likely due to mercury drop oscillation at such cathodic potentials. {yields} This effect is also likely due to added local convection at the mercury drop surface caused by the evolution of hydrogen bubbles. - Abstract: An improved approach to the anodic stripping voltammetric (ASV) determination of heavy metals, using the hanging mercury drop electrode (HMDE), is reported. It was discovered that using very cathodic accumulation potentials, at which the solvent reduction occurs (overpotential deposition), the voltammetric signals of zinc(II), cadmium(II), lead(II) and copper(II) increase. When compared with the classical methodology a 5 to 10-fold signal increase is obtained. This effect is likely due to both mercury drop oscillation at such cathodic potentials and added local convection at the mercury drop surface caused by the evolution of hydrogen bubbles.

SQUARE WAVE CATHODIC STRIPPING VOLTAMMETRY ADSORPTIVE FOR NICKEL AND COBALT ANALYSIS

Directory of Open Access Journals (Sweden)

Saryati Saryati

2010-06-01

Full Text Available The adsorptive stripping voltammetric determination of Ni and Co based on adsorption of the Ni/Co and dimethylglioxime (DMG complex on a hanging mercury drop electrode is studied. The reduction current of the adsorbed DMG complex is measured by square wave cathodic stripping voltammetry method. The effect of various parameters such as ligand concentration, pH of supporting electrolytic, adsorption potential and adsorption time on the current peak of Ni and Co voltammogram were studied. Optimum condition of this method are supporting electrolyte pH 9, DMG concentration 5×10 -4 M, adsorption potential -0.7 V vs Ag/AgCl and adsorption time 180 second. A linier relationship between the current peak and Ni or Co concentration was obtained in the range 5 - 30 ng/mL and the detection limit 0.6 ng/ml for both Ni and Co. The recovery of Ni and Co were 98.11-104.17% using standard biological materials with RSD 2.59 - 10.37%. Based on ";t"; test can be conclude that the result are nearly equal to the standard reference material.   Keywords: adsorptive stripping voltammetric, dimethylglioxime complex, nickel, cobalt

Elektrochemické stanovení Fomesafenu

OpenAIRE

Maška, Jan

2013-01-01

The submitted work deals with the application of voltammetric determination of Fomesafen using non-traditional mercury meniscus modified silver solid amalgam electrode on model samples of Fomesafen in real aqueous matrices of drinking and river water. This method of measurement has been developed and optimized in my bachelor thesis, which the diploma thesis is related to. Fomesafen belongs to a group of herbicides used on a mass scale in the late 20th century in the USA and in many countries ...

An electrochemical study of natural and chemically controlled eumelanin

Science.gov (United States)

Xu, Ri; Prontera, Carmela Tania; Di Mauro, Eduardo; Pezzella, Alessandro; Soavi, Francesca; Santato, Clara

2017-12-01

Eumelanin is the most common form of the pigment melanin in the human body, with functions including antioxidant behavior, metal chelation, and free radical scavenging. This biopigment is of interest for biologically derived batteries and supercapacitors. In this work, we characterized the voltammetric properties of chemically controlled eumelanins produced from 5,6-dihydroxyindole (DHI) and 5,6-dihydroxyindole-2-carboxylic acid (DHICA) building blocks, namely, DHI-melanin, DHICA-melanin, and natural eumelanin, extracted from the ink sac of cuttlefish, Sepia melanin. Eumelanin electrodes were studied for their cyclic voltammetric properties in acidic buffers including Na+, K+, NH4+, and Cu2+ ions.

Electrochemical Study of Esculetin Nitration by Digital Simulation of Cyclic Voltammograms

Directory of Open Access Journals (Sweden)

Lida Khalafi

2013-01-01

Full Text Available The reaction of electrochemically generated o-quinones from oxidation of esculetin as Michael acceptor with nitrite ion as nucleophile has been studied using cyclic voltammetry. The reaction mechanism is believed to be EC, including oxidation of catechol moiety of esculetin followed by Michael addition of nitrite ion. The observed homogeneous rate constants (obs for reactions were estimated by comparing the experimental voltammetric responses with the digitally simulated results based on the proposed mechanism. Also the effects of pH and nucleophile concentration on voltammetric behavior and the rate constants of chemical reactions were described.

Voltammetric and Chronopotentiometric Measurements with Nucleic Acid-Modified Mercury Film on a Glassy Carbon Electrode

Czech Academy of Sciences Publication Activity Database

Kubičárová, Tatiana; Fojta, Miroslav; Vidic, J.; Tomschik, Miroslav; Suznjevic, D.; Paleček, Emil

2000-01-01

Roč. 12, - (2000), s. 1390-1396 ISSN 1040-0397 R&D Projects: GA ČR GV204/97/K084; GA ČR GA204/98/P091 Institutional research plan: CEZ:AV0Z5004920 Subject RIV: BO - Biophysics Impact factor: 1.972, year: 2000

Observation of nanometer-sized electro-active defects in insulating layers by fluorescence microscopy and electrochemistry.

Science.gov (United States)

Renault, Christophe; Marchuk, Kyle; Ahn, Hyun S; Titus, Eric J; Kim, Jiyeon; Willets, Katherine A; Bard, Allen J

2015-06-02

We report a method to study electro-active defects in passivated electrodes. This method couples fluorescence microscopy and electrochemistry to localize and size electro-active defects. The method was validated by comparison with a scanning probe technique, scanning electrochemical microscopy. We used our method for studying electro-active defects in thin TiO2 layers electrodeposited on 25 μm diameter Pt ultramicroelectrodes (UMEs). The permeability of the TiO2 layer was estimated by measuring the oxidation of ferrocenemethanol at the UME. Blocking of current ranging from 91.4 to 99.8% was achieved. Electro-active defects with an average radius ranging between 9 and 90 nm were observed in these TiO2 blocking layers. The distribution of electro-active defects over the TiO2 layer is highly inhomogeneous and the number of electro-active defect increases for lower degree of current blocking. The interest of the proposed technique is the possibility to quickly (less than 15 min) image samples as large as several hundreds of μm(2) while being able to detect electro-active defects of only a few tens of nm in radius.

Voltammetric determination of arsenic in high iron and manganese groundwaters.

Science.gov (United States)

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.

Synthesis and Electronic Properties of Length-Defined 9,10-Anthrylene-Butadiynylene Oligomers.

Science.gov (United States)

Nagaoka, Maiko; Tsurumaki, Eiji; Nishiuchi, Mai; Iwanaga, Tetsuo; Toyota, Shinji

2018-05-18

Linear π-conjugated oligomers consisting of anthracene and diacetylene units were readily synthesized by a one-pot process that involved desilylation and oxidative coupling from appropriate building units. We were able to isolate length-defined oligomers ranging from 2-mer to 6-mer as stable and soluble solids. The bathochromic shifts in the UV-vis spectra suggested that the π-conjugation was extended with elongation of the linear chain. Cyclic voltammetric measurements showed characteristic reversible oxidation waves that were dependent on the number of anthracene units.

Clay matrix voltammetry

International Nuclear Information System (INIS)

Perdicakis, Michel

2012-01-01

Document available in extended abstract form only. In many countries, it is planned that the long life highly radioactive nuclear spent fuel will be stored in deep argillaceous rocks. The sites selected for this purpose are anoxic and satisfy several recommendations as mechanical stability, low permeability and low redox potential. Pyrite (FeS 2 ), iron(II) carbonate, iron(II) bearing clays and organic matter that are present in very small amounts (about 1% w:w) in soils play a major role in their reactivity and are considered today as responsible for the low redox potential values of these sites. In this communication, we describe an electrochemical technique derived from 'Salt matrix voltammetry' and allowing the almost in-situ voltammetric characterization of air-sensitive samples of soils after the only addition of the minimum humidity required for electrolytic conduction. Figure 1 shows the principle of the developed technique. It consists in the entrapment of the clay sample between a graphite working electrode and a silver counter/quasi-reference electrode. The sample was previously humidified by passing a water saturated inert gas through the electrochemical cell. The technique leads to well-defined voltammetric responses of the electro-active components of the clays. Figure 2 shows a typical voltammogram relative to a Callovo-Oxfordian argillite sample from Bure, the French place planned for the underground nuclear waste disposal. During the direct scan, one can clearly distinguish the anodic voltammetric signals for the oxidation of the iron (II) species associated with the clay and the oxidation of pyrite. The reverse scan displays a small cathodic signal for the reduction of iron (III) associated with the clay that demonstrates that the majority of the previously oxidized iron (II) species were transformed into iron (III) oxides reducible at lower potentials. When a second voltammetric cycle is performed, one can notice that the signal for iron (II

Novel acyclonucleoside analog bearing a 1,2,4-triazole–Schiff base: Synthesis, characterization and analytical studies using square wave-adsorptive stripping voltammetry and HPLC

Directory of Open Access Journals (Sweden)

Ali F. Alghamdi

2017-09-01

Full Text Available New acyclonucleoside analogs tethered by a 1,2,4-triazole scaffold were synthesized through the condensation of 4-amino-5-(2-phenyleth-1-yl-2,4-dihydro-3H-1,2,4-triazole-3-thione (2 with benzaldehyde followed by the alkylation of the resulting Schiff base (3with 2-bromoethanol, 3-chloropropanol and/or 3-chloropropan-1,2-diol. Voltammetric studies were carried out for the analysis of 1 × 10−6 mol L−1 of the newly synthesized acyclonucleoside analogs (4–6 using square wave-adsorptive stripping voltammetry (SW-AdSV. The sharp voltammetric peak and high reduction current were recorded using a Britton–Robinson B–R pH 10 buffer at Ep = −1250 mV on the hanging mercury drop surface (HMDE and Ag/AgCl reference electrode. Several experimental conditions were studied, such as the supporting electrolytes, the pH, and the accumulation time, as well as the potential, the scan rate, the frequency and the step potential for 4-benzylideneamino-5-(2-phenyleth-1-yl-3-[(2,3-dihydroxyprop-1-ylthio]-1,2,4-triazole (6. The analytical performance of the voltammetric technique was investigated through the analysis of the calibration curve, the detection limit, the recovery and the stability. The voltammetric analytical applications were evaluated by the recovery of compound (6 in the urine and plasma samples. The HPLC technique was also applied for the separation of compound (6 from interference using a C-18 (5 μm column with UV detection at 254 nm.

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

Science.gov (United States)

Gumustas, Mehmet; Ozkan, Sibel A

2010-05-01

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

Visualized attribute analysis approach for characterization and quantification of rice taste flavor using electronic tongue

Energy Technology Data Exchange (ETDEWEB)

Lu, Lin; Hu, Xianqiao [Rice Product Quality Supervision and Inspection Center, Ministry of Agriculture, China National Rice Research Institute, Hangzhou 310006 (China); Tian, Shiyi; Deng, Shaoping [College of Food Science and Biotechnology, Zhejiang Gongshang University, Hangzhou 310035 (China); Zhu, Zhiwei, E-mail: 615834652@qq.com [Rice Product Quality Supervision and Inspection Center, Ministry of Agriculture, China National Rice Research Institute, Hangzhou 310006 (China)

2016-05-05

This paper deals with a novel visualized attributive analysis approach for characterization and quantification of rice taste flavor attributes (softness, stickiness, sweetness and aroma) employing a multifrequency large-amplitude pulse voltammetric electronic tongue. Data preprocessing methods including Principal Component Analysis (PCA) and Fast Fourier Transform (FFT) were provided. An attribute characterization graph was represented for visualization of the interactive response in which each attribute responded by specific electrodes and frequencies. The model was trained using signal data from electronic tongue and attribute scores from artificial evaluation. The correlation coefficients for all attributes were over 0.9, resulting in good predictive ability of attributive analysis model preprocessed by FFT. This approach extracted more effective information about linear relationship between electronic tongue and taste flavor attribute. Results indicated that this approach can accurately quantify taste flavor attributes, and can be an efficient tool for data processing in a voltammetric electronic tongue system. - Graphical abstract: Schematic process for visualized attributive analysis approach using multifrequency large-amplitude pulse voltammetric electronic tongue for determination of rice taste flavor attribute. (a) sample; (b) sensors in electronic tongue; (c) excitation voltage program and response current signal from MLAPS; (d) similarity data matrix by data preprocessing and similarity extraction; (e) feature data matrix of attribute; (f) attribute characterization graph; (g) attribute scores predicted by the model. - Highlights: • Multifrequency large-amplitude pulse voltammetric electronic tongue was used. • A visualized attributive analysis approach was created as an efficient tool for data processing. • Rice taste flavor attribute was determined and predicted. • The attribute characterization graph was represented for visualization of the

Enzyme-immobilized SiO2-Si electrode: Fast interfacial electron transfer with preserved enzymatic activity

Science.gov (United States)

Wang, Gang; Yau, Siu-Tung

2005-12-01

The enzyme, glucose oxidase (GOx), is immobilized using electrostatic interaction on the native oxide of heavily doped n-type silicon. Voltammetric measurement shows that the immobilized GOx gives rise to a very fast enzyme-silicon interfacial electron transfer rate constant of 7.9s-1. The measurement also suggests that the enzyme retains its native conformation when immobilized on the silicon surface. The preserved native conformation of GOx is further confirmed by testing the enzymatic activity of the immobilized GOx using glucose. The GOx-immobilized silicon is shown to behave as a glucose sensor that detects glucose with concentrations as low as 50μM.

Increased sensitivity of anodic stripping voltammetry at the hanging mercury drop electrode by ultracathodic deposition.

Science.gov (United States)

Rodrigues, José A; Rodrigues, Carlos M; Almeida, Paulo J; Valente, Inês M; Gonçalves, Luís M; Compton, Richard G; Barros, Aquiles A

2011-09-09

An improved approach to the anodic stripping voltammetric (ASV) determination of heavy metals, using the hanging mercury drop electrode (HMDE), is reported. It was discovered that using very cathodic accumulation potentials, at which the solvent reduction occurs (overpotential deposition), the voltammetric signals of zinc(II), cadmium(II), lead(II) and copper(II) increase. When compared with the classical methodology a 5 to 10-fold signal increase is obtained. This effect is likely due to both mercury drop oscillation at such cathodic potentials and added local convection at the mercury drop surface caused by the evolution of hydrogen bubbles. Copyright © 2011 Elsevier B.V. All rights reserved.

An electrochemical study of natural and chemically controlled eumelanin

Directory of Open Access Journals (Sweden)

Ri Xu

2017-12-01

Full Text Available Eumelanin is the most common form of the pigment melanin in the human body, with functions including antioxidant behavior, metal chelation, and free radical scavenging. This biopigment is of interest for biologically derived batteries and supercapacitors. In this work, we characterized the voltammetric properties of chemically controlled eumelanins produced from 5,6-dihydroxyindole (DHI and 5,6-dihydroxyindole-2-carboxylic acid (DHICA building blocks, namely, DHI-melanin, DHICA-melanin, and natural eumelanin, extracted from the ink sac of cuttlefish, Sepia melanin. Eumelanin electrodes were studied for their cyclic voltammetric properties in acidic buffers including Na+, K+, NH4+, and Cu2+ ions.

Characterization and supercapacitor application of coin-like β-nickel hydroxide nanoplates

International Nuclear Information System (INIS)

Li Hongliang; Liu Suqin; Huang Chenghuan; Zhou Zhi; Li Yanhua; Fang Dong

2011-01-01

Coin-like nickel hydroxide nanoplates are synthesized via a simple coordination homogeneous precipitation method. The structure and morphology of as-prepared products are characterized by X-ray diffraction, Fourier transform infrared spectroscopy, transmission electron microscopy and scanning electron microscopy. It is demonstrated that the products are typical β-nickel hydroxide with bunches coin-like nanoplates morphology. The electrochemical properties of coin-like β-Ni(OH) 2 are examined by cyclic voltammetric, chronopotentiometry and electrochemical impedance spectroscope. Cyclic voltammetric studies show that the electrodes have good reversibility. A specific capacitance of 1532 F g −1 is obtained at a charge/discharge current density of 0.2 A g −1 .

A Mediated BOD Biosensor Based on Immobilized B. Subtilis on Three-Dimensional Porous Graphene-Polypyrrole Composite

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Jingfang Hu

2017-11-01

Full Text Available We have developed a novel mediated biochemical oxygen demand (BOD biosensor based on immobilized Bacillus subtilis (B. subtilis on three-dimensional (3D porous graphene-polypyrrole (rGO-PPy composite. The 3D porous rGO-PPy composite was prepared using hydrothermal method following with electropolymerization. Then the 3D porous rGO-PPy composite was used as a support for immobilizing negatively charged B. subtilis denoted as rGO-PPy-B through coordination and electrostatic interaction. Further, the prepared rGO-PPy-B was used as a microbial biofilm for establishing a mediated BOD biosensor with ferricyanide as an electronic acceptor. The indirect determination of BOD was performed by electrochemical measuring ferrocyanide generated from a reduced ferricyanide mediator using interdigited ultramicroelectrode array (IUDA as the working electrode. The experimental results suggested a good linear relationship between the amperometric responses and BOD standard concentrations from 4 to 60 mg/L, with a limit detection of 1.8 mg/L (S/N ≥ 3. The electrochemical measurement of real water samples showed a good agreement with the conventional BOD5 method, and the good anti-interference as well as the long-term stability were well demonstrated, indicating that the proposed mediated BOD biosensor in this study holds a potential practical application of real water monitoring.

Kinetics of oxygen reduction reaction at electrochemically fabricated tin-palladium bimetallic electrocatalyst in acidic media

Energy Technology Data Exchange (ETDEWEB)

Miah, Md. Rezwan, E-mail: mrmche@yahoo.co [Department of Electronic Chemistry, Interdisciplinary Graduate School of Science and Engineering, Tokyo Institute of Technology, Mail Box G1-5, 4259 Nagatsuta, Midori-ku, Yokohama 226-8502 (Japan); Masud, Jahangir [Department of Electronic Chemistry, Interdisciplinary Graduate School of Science and Engineering, Tokyo Institute of Technology, Mail Box G1-5, 4259 Nagatsuta, Midori-ku, Yokohama 226-8502 (Japan); Ohsaka, Takeo, E-mail: ohsaka@echem.titech.ac.j [Department of Electronic Chemistry, Interdisciplinary Graduate School of Science and Engineering, Tokyo Institute of Technology, Mail Box G1-5, 4259 Nagatsuta, Midori-ku, Yokohama 226-8502 (Japan)

2010-12-15

In the present article, oxygen reduction reaction (ORR) at electrochemically fabricated tin-palladium (Sn-Pd) bimetallic electrocatalyst-modified glassy carbon (GC) electrode (Sn-Pd/GC electrode) in acidic media is addressed. Hydrodynamic voltammetric measurements were employed with a view to evaluating various kinetic parameters of the ORR at the Sn-Pd/GC electrode. The obtained results obviously demonstrated that the Sn-Pd bimetallic electrocatalyt substantially promoted the activity of the GC electrode and drove the ORR through an exclusive one-step four-electron pathway forming H{sub 2}O as the final product.

Kinetics of oxygen reduction reaction at electrochemically fabricated tin-palladium bimetallic electrocatalyst in acidic media

International Nuclear Information System (INIS)

Miah, Md. Rezwan; Masud, Jahangir; Ohsaka, Takeo

2010-01-01

In the present article, oxygen reduction reaction (ORR) at electrochemically fabricated tin-palladium (Sn-Pd) bimetallic electrocatalyst-modified glassy carbon (GC) electrode (Sn-Pd/GC electrode) in acidic media is addressed. Hydrodynamic voltammetric measurements were employed with a view to evaluating various kinetic parameters of the ORR at the Sn-Pd/GC electrode. The obtained results obviously demonstrated that the Sn-Pd bimetallic electrocatalyt substantially promoted the activity of the GC electrode and drove the ORR through an exclusive one-step four-electron pathway forming H 2 O as the final product.

Planejamento fatorial e superfície de resposta: otimização de um método voltamétrico para a determinação de ag(i empregando um eletrodo de pasta de nanotubos de carbono

Directory of Open Access Journals (Sweden)

Fernando Campanhã Vicentini

2011-01-01

Full Text Available A factorial design applied in a voltammetric stripping method for the measurement of Ag(I in natural water is described. The procedure is based on the effective pre-concentration of silver ions on electrode surface. The calibration graph was linear in the silver concentration range from 7.92 x 10"7 to 1.07 x 10"5 mol L"1 with a detection limit of 3.81 x 10-7 mol L-1. The determination of Ag(I in natural water samples was carried out satisfactory with the proposed electrode.

Electrodeposition synthesis and electrochemical properties of nanostructured γ-MnO 2 films

Science.gov (United States)

Chou, Shulei; Cheng, Fangyi; Chen, Jun

The thin films of carambola-like γ-MnO 2 nanoflakes with about 20 nm in thickness and at least 200 nm in width were prepared on nickel sheets by combination of potentiostatic and cyclic voltammetric electrodeposition techniques. The as-prepared MnO 2 nanomaterials, which were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), and X-ray photoelectron spectroscopy (XPS), were used as the active material of the positive electrode for primary alkaline Zn/MnO 2 batteries and electrochemical supercapacitors. Electrochemical measurements showed that the MnO 2 nanoflake films displayed high potential plateau (around 1.0 V versus Zn) in primary Zn/MnO 2 batteries at the discharge current density of 500 mA g -1 and high specific capacitance of 240 F g -1 at the current density of 1 mA cm -2. This indicated the potential application of carambola-like γ-MnO 2 nanoflakes in high-power batteries and electrochemical supercapacitors. The growth process for the one- and three-dimensional nanostructured MnO 2 was discussed on the basis of potentiostatic and cyclic voltammetric techniques. The present synthesis method can be extended to the preparation of other nanostructured metal-oxide films.

Determination of acrylamide in dry feedstuff for dogs and cats

Directory of Open Access Journals (Sweden)

Helena Veselá

2013-01-01

Full Text Available Acrylamide is considered to be an endogenous contaminant of food and feedstuff. Attention is paid to the acrylamide content in human nutrition products; however, there is lack of data about its concentrations in feedstuff. The aim of this study was to use a newly developed adsorptive stripping voltammetry procedure for determination of acrylamide concentrations in five and three different kinds of dog and cat dry feedstuff, respectively. The applied analytical procedure consists of a solvent extraction in ultrasound bath, followed by voltammetric measurement at the hanging mercury drop electrode in ammonia buffer. The accuracy of the method was verified by use of standard reference materials. The range of acrylamide concentration found in samples of dry dog and cat feedstuff ranged from 106 to 358 μg/kg, and from 66 to 269 μg/kg, respectively. The precision of analyses expressed in form of the relative standard deviations ranged between 0.6–1.7%. The voltammetric procedure appears to be a reliable, sensitive, rapid and low-cost analytical technique for the determination of acrylamide in food and feedstuff. The concentrations of acrylamide found in feedstuff were relatively moderate but it is undoubtedly necessary to monitor its concentrations in future.

The improvement of SiO2 nanotubes electrochemical behavior by hydrogen atmosphere thermal treatment

Science.gov (United States)

Spataru, Nicolae; Anastasescu, Crina; Radu, Mihai Marian; Balint, Ioan; Negrila, Catalin; Spataru, Tanta; Fujishima, Akira

2018-06-01

Highly defected SiO2 nanotubes (SiO2-NT) were obtained by a simple sol-gel procedure followed by calcination. Boron-doped diamond (BDD) polycrystalline films coated with SiO2-NT were used as working electrodes and, unexpectedly, cyclic voltammetric experiments have shown that the concentration of both positive and negative defects at the surface is high enough to enable redox processes involving positively charged Ru(bpy)32+/3+ to occur. Conversely, no electrochemical activity was put into evidence for Fe(CN)63-/4- species, most likely as a result of the strong electrostatic repulsion exerted by the negatively charged SiO2 surface. The concentration of surface defects was further increased by a subsequent thermal treatment in a hydrogen atmosphere which, as EIS measurements have shown, significantly promotes Ru(bpy)32+ anodic oxidation. Digital simulation of the voltammetric responses demonstrated that this treatment does not lead to a similar increase of the number of electron-donor sites. It was also found that methanol anodic oxidation at hydrogenated SiO2-NT-supported platinum results in Tafel slopes of 116-220 mV decade-1, comparable to those reported for both conventional PtRu and Pt-oxide catalysts.

Electrodeposition synthesis and electrochemical properties of nanostructured {gamma}-MnO{sub 2} films

Energy Technology Data Exchange (ETDEWEB)

Chou, Shulei; Cheng, Fangyi; Chen, Jun [Institute of New Energy Material Chemistry, Nankai University, Tianjin 300071 (China)

2006-11-08

The thin films of carambola-like {gamma}-MnO{sub 2} nanoflakes with about 20nm in thickness and at least 200nm in width were prepared on nickel sheets by combination of potentiostatic and cyclic voltammetric electrodeposition techniques. The as-prepared MnO{sub 2} nanomaterials, which were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), and X-ray photoelectron spectroscopy (XPS), were used as the active material of the positive electrode for primary alkaline Zn/MnO{sub 2} batteries and electrochemical supercapacitors. Electrochemical measurements showed that the MnO{sub 2} nanoflake films displayed high potential plateau (around 1.0V versus Zn) in primary Zn/MnO{sub 2} batteries at the discharge current density of 500mAg{sup -1} and high specific capacitance of 240Fg{sup -1} at the current density of 1mAcm{sup -2}. This indicated the potential application of carambola-like {gamma}-MnO{sub 2} nanoflakes in high-power batteries and electrochemical supercapacitors. The growth process for the one- and three-dimensional nanostructured MnO{sub 2} was discussed on the basis of potentiostatic and cyclic voltammetric techniques. The present synthesis method can be extended to the preparation of other nanostructured metal-oxide films. (author)

A novel electrochemical platform based on carbon nanofibers and tri-metallic nanoparticles of gold, nickel and cobalt for the quantification of ethyl paraben

International Nuclear Information System (INIS)

Baytak, Aysegul Kutluay; Teker, Tugce; Duzmen, Sehriban; Aslanoglu, Mehmet

2017-01-01

A composite of carbon nanofibers (CNFs) and tri-metallic nanoparticles of gold, cobalt and nickel were used for the preparation of a novel voltammetric platform. The proposed voltammetric platform was utilized for quantifying ethyl paraben (EPB) in pharmaceutical and cosmetic products. The electrode layers were characterized by utilizing X-ray diffraction method (XRD) and Fourier transform infrared spectroscopy (FTIR). The electrode system, (Au-Ni-Co)NPs-CNFs/GCE, exhibited high catalytic activity and enhanced the electrochemical behaviour of EPB compared with several other electrodes. The proposed composite layer based electrode produced a well-defined oxidation peak at 0.760 V. The determination of EPB was carried out by square wave voltammetry (SWV). The electrode produced a linear plot with a concentration range from 1.0 × 10 −9 to 1.0 × 10 −7 M at (Au-Ni-Co)NPs-CNFs/GCE. The composite material enabled a detection limit of 3.5 × 10 −10 M for EPB. Good reproducibility, high precision and excellent accuracy for EPB were obtained at (Au-Ni-Co)NPs-CNFs/GCE. The composite layer based platform was successfully applied for the quantification of EPB in pharmaceutical and cosmetic products. The sensitive quantification of EPB is of great importance for the public health care. Furthermore, data show that EPB binds to DNA via intercalation with a binding constant of 2.51 (± 0.40) × 10 4 . - Highlights: • CNFs and (Au-Ni-Co) nanoparticles were used to prepare a novel platform. • (Au-Ni-Co)NPs-CNFs/GCE has improved the voltammetric behaviour of EPB. • The voltammetric platform yielded a detection limit of 0.35 nM for EPB. • The platform was successfully applied to cosmetic and pharmaceutical samples. EPB could bind to DNA via intercalation.

A novel electrochemical platform based on carbon nanofibers and tri-metallic nanoparticles of gold, nickel and cobalt for the quantification of ethyl paraben

Energy Technology Data Exchange (ETDEWEB)

Baytak, Aysegul Kutluay, E-mail: a.kutluay@harran.edu.tr [Department of Medical Laboratory, Vocational School of Health Services, Harran University, Şanlıurfa 63510 (Turkey); Teker, Tugce; Duzmen, Sehriban [Department of Chemistry, Harran University, Şanlıurfa 63510 (Turkey); Aslanoglu, Mehmet, E-mail: maslanoglu@harran.edu.tr [Department of Chemistry, Harran University, Şanlıurfa 63510 (Turkey)

2017-03-01

A composite of carbon nanofibers (CNFs) and tri-metallic nanoparticles of gold, cobalt and nickel were used for the preparation of a novel voltammetric platform. The proposed voltammetric platform was utilized for quantifying ethyl paraben (EPB) in pharmaceutical and cosmetic products. The electrode layers were characterized by utilizing X-ray diffraction method (XRD) and Fourier transform infrared spectroscopy (FTIR). The electrode system, (Au-Ni-Co)NPs-CNFs/GCE, exhibited high catalytic activity and enhanced the electrochemical behaviour of EPB compared with several other electrodes. The proposed composite layer based electrode produced a well-defined oxidation peak at 0.760 V. The determination of EPB was carried out by square wave voltammetry (SWV). The electrode produced a linear plot with a concentration range from 1.0 × 10{sup −9} to 1.0 × 10{sup −7} M at (Au-Ni-Co)NPs-CNFs/GCE. The composite material enabled a detection limit of 3.5 × 10{sup −10} M for EPB. Good reproducibility, high precision and excellent accuracy for EPB were obtained at (Au-Ni-Co)NPs-CNFs/GCE. The composite layer based platform was successfully applied for the quantification of EPB in pharmaceutical and cosmetic products. The sensitive quantification of EPB is of great importance for the public health care. Furthermore, data show that EPB binds to DNA via intercalation with a binding constant of 2.51 (± 0.40) × 10{sup 4}. - Highlights: • CNFs and (Au-Ni-Co) nanoparticles were used to prepare a novel platform. • (Au-Ni-Co)NPs-CNFs/GCE has improved the voltammetric behaviour of EPB. • The voltammetric platform yielded a detection limit of 0.35 nM for EPB. • The platform was successfully applied to cosmetic and pharmaceutical samples. EPB could bind to DNA via intercalation.

Measuring the relative hydrogen-bonding strengths of alcohols in aprotic organic solvents.

Science.gov (United States)

Tessensohn, Malcolm E; Lee, Melvyn; Hirao, Hajime; Webster, Richard D

2015-01-12

Voltammetric experiments with 9,10-anthraquinone and 1,4-benzoquinone performed under controlled moisture conditions indicate that the hydrogen-bond strengths of alcohols in aprotic organic solvents can be differentiated by the electrochemical parameter ΔEp (red) =|Ep (red(1)) -Ep (red(2)) |, which is the potential separation between the two one-electron reduction processes. This electrochemical parameter is inversely related to the strength of the interactions and can be used to differentiate between primary, secondary, tertiary alcohols, and even diols, as it is sensitive to both their steric and electronic properties. The results are highly reproducible across two solvents with substantially different hydrogen-bonding properties (CH3 CN and CH2 Cl2 ) and are supported by density functional theory calculations. This indicates that the numerous solvent-alcohol interactions are less significant than the quinone-alcohol hydrogen-bonding interactions. The utility of ΔEp (red) was illustrated by comparisons between 1) 3,3,3-trifluoro-n-propanol and 1,3-difluoroisopropanol and 2) ethylene glycol and 2,2,2-trifluoroethanol. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

electrochemical behaviour and voltammetric determination

African Journals Online (AJOL)

The detection limit was found to be 5.00 x 10-7 M Geshoidin. For eight successive .... dark to protect it from light. The required .... during the first scan of the voltammogram is an indication of the existence of weak adsorption of the oxidation .... The detection limit (three times signal-to-noise ratio) was found to be 5.00 x. 10-7 M ...

VOLTAMMETRIC DETERMINATION OF TINIDAZOLE IN ...

African Journals Online (AJOL)

tablet samples showed the potential applicability of the developed method for the determination of tinidazole in ... determination of TNZ in real samples like tablets, injection, urine and biological fluids [24-27]. Almost all ..... during the storage.

Electrochemical ion transfer mediated by a lipophilic Os(ii)/Os(iii) dinonyl bipyridyl probe incorporated in thin film membranes.

Science.gov (United States)

Jansod, Sutida; Wang, Lu; Cuartero, Maria; Bakker, Eric

2017-09-28

A new lipophilic dinonyl bipyridyl Os(ii)/Os(iii) complex successfully mediates ion transfer processes across voltammetric thin membranes. An added lipophilic cation-exchanger may impose voltammetric anion or cation transfer waves of Gaussian shape that are reversible and repeatable. The peak potential is found to shift with the ion concentration in agreement with the Nernst equation. The addition of tridodecylmethylammonium nitrate to the polymeric film dramatically reduces the peak separation from 240 mV to 65 mV, and the peak width to a near-theoretical value of 85 mV, which agrees with a surface confined process. It is suggested that the cationic additive serves as a phase transfer catalyst.

Anodic stripping voltammetry – ASV for determination of heavy metals

International Nuclear Information System (INIS)

Barón-Jaimez, J; Joya, M R; Barba-Ortega, J

2013-01-01

Although voltammetric methods presented a number of difficulties in its early stages, nowadays ''ASV'' anodic stripping voltammetry is considered one of the most sensitive electro-analytical and suitable for trace-level determination of many metals and compounds in environmental samples, clinical and industrial. Its sensitivity is attributed to the combination of a step of pre-concentration effective together with an electrochemical advanced measurement of accumulated analyte. This paper presents an overview of the voltammetry, which includes a group of electro-analytical methods, in them the information about analyte is obtained from measurements of the current flowing in an electrochemical cell when applied a potential difference to an suitable electrode system

Influência da acidez do meio sobre a síntese e o comportamento redox do polipirrol Influence of the medium acidity on the synthesis and redox behavior of polypyrrole

Directory of Open Access Journals (Sweden)

Márcia T. Giacomini

1999-09-01

Full Text Available The influence of acidity on the synthesis and redox behavior of polypyrrole films was studied using galvanostatic and potentiodynamic techniques employing aqueous solutions formed by H2SO4/Na2SO4 , HCl/NaCl and HCl/CsCl. The chemical structure of the films were investigated using the FTIR technique. The polymer behavior as a function of the pH used in the cyclic voltammetric measurements is explained in terms of the mechanism responsible for the charge compensation formed during the polymer chain oxidation. From the FTIR measurements, it is seen that the water nucleophilic attack during the synthesis, does not occur under the experimental conditions employed in this work.

Trace determination of yttrium and some heavy rare-earths by adsorptive stripping voltammetry

International Nuclear Information System (INIS)

Wang, J.; Zadeii, J.M.

1986-01-01

The interfacial and redox behaviour of rare-earth chelates the Solochrome Violet RS are exploited for developing a sensitive adsorptive stripping procedure. Yttrium and heavy rare earths such as dysprosium, holmium and ytterbium can thus be measured at ng/ml levels and below, by controlled adsorptive accumulation of the metal chelate at the hanging mercury drop electrode, followed by voltammetric measurement of the surface species. With a 3-min preconcentration time, the detection limit ranges from 5 x 10 -10 to 1.4 x 10 -9 M. The relative standard deviation at the 7 ng/ml level ranges from 4 to 7%. A separation method is required to differentiate between the individual rare-earth metals. (author)

Nafion/2,2'-bipyridyl-modified bismuth film electrode for anodic stripping voltammetry

International Nuclear Information System (INIS)

Torma, Ferenc; Kadar, Mihaly; Toth, Klara; Tatar, Eniko

2008-01-01

This paper describes the fabrication, characterisation and the application of a Nafion/2,2'-bipyridyl/bismuth composite film-coated glassy carbon electrode (NC(Bpy)BiFE) for the anodic stripping voltammetric determination of trace metal ions (Zn 2+ , Cd 2+ and Pb 2+ ). The NC(Bpy)BiFE electrode is prepared by first applying a 2.5 mm 3 drop of a coating solution containing 0.5 wt% Nafion and 0.1% (w/v) 2,2'-bipyridil (Bpy) onto the surface of a glassy carbon electrode, while the Bi film was plated in situ simultaneously with the target metal ions at -1.4 V. The main advantage of the polymer coated bismuth film electrode is that the sensitivity of the stripping responses is increased considerably due to the incorporation of the neutral chelating agent of 2,2'-bipyridyl (Bpy) in the Nafion film, while the Nafion coating improved the mechanical stability of the bismuth film and its resistance to the interference of surfactants. The key experimental parameters relevant to both the electrode fabrication and the voltammetric measurement were optimized on the basis of the stripping signals. With a 2 min deposition time in the presence of oxygen, linear calibration curves were obtained in a wide concentration range (about 2-0.001 μM) with detection limits of 8.6 nM (0.56 μg dm -3 ) for Zn 2+ , 1.1 nM (0.12 μg dm -3 ) for Cd 2+ and 0.37 nM (0.077 μg dm -3 ) for Pb 2+ . For nine successive preconcentration/determination/electrode renewal experiments the standard deviations were between 3 and 5% at 1.2 μM for zinc and 0.3-0.3 μM concentration level for lead and cadmium, respectively, and the method exhibited excellent selectivity in the presence of the excess of several potential interfering metal ions. The analytical utility of the stripping voltammetric method elaborated was tested in the assay of heavy metals in some real samples and the method was validated by ICP-MS technique

Adsorptive stripping voltammetric behaviour of copper complexes of some heterocyclic azo compounds.

Science.gov (United States)

Farias, P A; Ferreira, S L; Ohara, A K; Bastos, M B; Goulart, M S

1992-10-01

Controlled adsorptive accumulation of copper complexed with TAN, TAC, TAR and TAM (heterocyclic azo-compounds) on a static mercury drop electrode provides the basis for the direct stripping measurement of this element in the nanomolar concentration level. The ligand TAN exhibited great sensitivity and better separation of the peak current of the ligand in relation to the complex. The reduction current of adsorbed complex ions of copper is measured by linear scan cathodic stripping voltammetry, preceded by a period of accumulation of a few minutes. The peak potential is at approximately -0.37 V vs. Ag/AgCl. Optimal experimental parameters were found to be a TAN concentration of 1 x 10(-5)M, an accumulation potential of -0.22 V, and a solution pH of 3.7 (acetate buffer). The detection limit is 0.8nM after a 5-min accumulation with a stirred solution, and the response is linear up to 50 mug/l. Many common cations and anions do not interfere in the determination of copper. The interference of titanium is eliminated by addition of fluoride ion. Results are reported for a fresh water sample.

Poly-Alizarin red S/multiwalled carbon nanotube modified glassy carbon electrode for the boost up of electrocatalytic activity towards the investigation of dopamine and simultaneous resolution in the presence of 5-HT: A voltammetric study

International Nuclear Information System (INIS)

Reddaiah, K.; Madhusudana Reddy, T.; Venkata Ramana, D.K.; Subba Rao, Y.

2016-01-01

Poly-Alizarin red S/multiwalled carbon nanotube film on the surface of glassy carbon electrode (poly-AzrS/MWCNT/GCE) was synthesized by electrochemical process and was used for the sensitive and selective determination of dopamine (DA) by employing voltammetric techniques. The electrocatalytic response of the modified electrode was found to exhibit admirable activity. The simultaneous determination of dopamine in the presence of serotonin (5-HT) was found to exhibit very good response at poly-AzrS/MWCNTs/GCE. The effect of pH, scan rate, accumulation time and concentration of dopamine was studied at the developed poly-AzrS/MWCNTs/GCE. The poly-AzrS/MWCNTs/GCE exhibited an efficient electron mediating behavior together with well resolved peaks for dopamine, in 0.1 mol/dm"3 phosphate buffer (PBS) solution of pH 7.0. The limit of detection (LOD) and limit of quantification (LOQ) were found to be as 1.89 × 10"−"7 mol/dm"3 and 6.312 × 10"−"7 mol/dm"3 respectively with a dynamic range from 1 × 10"−"6 to 1.8 × 10"−"5 mol/dm"3. The interfacial electron transfer behavior of DA was studied by electrochemical impedance spectroscopy (EIS); the studies showed that the charge transfer rate was enhanced at poly-AzrS/MWCNTs/GCE when compared with bare GCE and poly-AzrS/GCE. - Highlights: • The poly-AzrS/MWCNTs/GCE showed good sensitivity towards DA sensing. • The sensor reduced the overoxidation potentials for DA. • This electrode was successfully used for simultaneous sensing of DA and 5-HT. • The electrode was effectively used for the determination of DA in pharmaceutical formulations.

Poly-Alizarin red S/multiwalled carbon nanotube modified glassy carbon electrode for the boost up of electrocatalytic activity towards the investigation of dopamine and simultaneous resolution in the presence of 5-HT: A voltammetric study

Energy Technology Data Exchange (ETDEWEB)

Reddaiah, K. [Electrochemical Research Laboratory, Department of Chemistry, S.V.U. College of Sciences, Sri Venkateswara University, Tirupati 517 502, Andhra Pradesh (India); Madhusudana Reddy, T., E-mail: tmsreddysvu@gmail.com [Electrochemical Research Laboratory, Department of Chemistry, S.V.U. College of Sciences, Sri Venkateswara University, Tirupati 517 502, Andhra Pradesh (India); Department of Chemistry, University of Minnesota, 207 Pleasant Street SE, Minneapolis, MN 55455 (United States); Venkata Ramana, D.K. [Department of Safety Engineering, Dongguk University, 123 Dongdae-ro, Gyeongju, Gyeongbuk 780 714 (Korea, Republic of); Subba Rao, Y. [DST-PURSE Centre, Sri Venkateswara University, Tirupati 517502, Andhra Pradesh (India)

2016-05-01

Poly-Alizarin red S/multiwalled carbon nanotube film on the surface of glassy carbon electrode (poly-AzrS/MWCNT/GCE) was synthesized by electrochemical process and was used for the sensitive and selective determination of dopamine (DA) by employing voltammetric techniques. The electrocatalytic response of the modified electrode was found to exhibit admirable activity. The simultaneous determination of dopamine in the presence of serotonin (5-HT) was found to exhibit very good response at poly-AzrS/MWCNTs/GCE. The effect of pH, scan rate, accumulation time and concentration of dopamine was studied at the developed poly-AzrS/MWCNTs/GCE. The poly-AzrS/MWCNTs/GCE exhibited an efficient electron mediating behavior together with well resolved peaks for dopamine, in 0.1 mol/dm{sup 3} phosphate buffer (PBS) solution of pH 7.0. The limit of detection (LOD) and limit of quantification (LOQ) were found to be as 1.89 × 10{sup −7} mol/dm{sup 3} and 6.312 × 10{sup −7} mol/dm{sup 3} respectively with a dynamic range from 1 × 10{sup −6} to 1.8 × 10{sup −5} mol/dm{sup 3}. The interfacial electron transfer behavior of DA was studied by electrochemical impedance spectroscopy (EIS); the studies showed that the charge transfer rate was enhanced at poly-AzrS/MWCNTs/GCE when compared with bare GCE and poly-AzrS/GCE. - Highlights: • The poly-AzrS/MWCNTs/GCE showed good sensitivity towards DA sensing. • The sensor reduced the overoxidation potentials for DA. • This electrode was successfully used for simultaneous sensing of DA and 5-HT. • The electrode was effectively used for the determination of DA in pharmaceutical formulations.

An Investigation of the Interaction between Resazurin and Cd 2+ ...

African Journals Online (AJOL)

resazurin. The voltammetric data were compared with the data obtained using spectrophotometric methods and were observed to be in good agreement. Keywords: Resazurin, Cadmium, Zinc, Electrochemistry, Spectroscopy, Metal Complexes ...

Ultramicroeletrodos. Parte II: construção e aplicações

Directory of Open Access Journals (Sweden)

Silva S. M.

1998-01-01

Full Text Available This work describes the techniques of construction and several applications of ultramicroelectrodes in electrochemistry and electroanalytical chemistry. Disc shaped UME are produced by embedding metal wires on insulating materials such as glass or epoxy resin. In the field of electrochemistry, UME have been applied in studies of the hydrogen evolution reaction and the electrocrystallization of metals. The negligible values of sensibility for ohmic drop and the enhanced mass transport rate by spherical diffusion are the main advantages of UME in these applications. New important conclusions regarding the phenomena under study were drawn from the experimental results. The applications in electroanalytical chemistry involved the determination of contaminants such as heavy metals and nitrites in natural waters and food products. The use of UME requires little sample manipulation and, in general, no need for oxygen removal or the addition of supporting electrolytes.

COMPARAÇÃO DE PROCESSAMENTOS MATEMÁTICOS DE DADOS VOLTAMÉTRICOS: APLICAÇÃO NA DETERMINAÇÃO SIMULTÂNEA DE FLUOROQUINOLONAS

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Luiz H. de Oliveira

2015-12-01

Full Text Available This paper describes a comparative study between the procedures of deconvolution and the second-order derivative of square wave voltammograms to achieve separation of the voltammetric peaks of levofloxacin (LEVO and norfloxacin (NOR, for their simultaneous quantification in urine samples. The obtained results indicate that the use of second-derivative voltammograms coupled with carbon screen-printed electrodes is the most efficient approach for completely separating the voltammetric peaks of LEVO and NOR. In addition, this approach has produced detection limits lower than 1.0 µmol L-1 and a wide linear range for both drugs. The proposed method was successfully used to simultaneously determine LEVO and NOR in spiked human and bovine urine samples with recovery percentages close to 100% for all analyzed samples.

Simple Synthesis and Enhanced Performance of Graphene Oxide-Gold Composites

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Min Song

2012-01-01

Full Text Available Graphene oxide-gold composites were prepared by one-step reaction in aqueous solution, where the gold nanoparticles were deposited on the graphene oxide during their synthesis process. Transmission electron morphology, X-ray diffraction, Roman spectra, and UV-Vis absorption spectra were used to characterize the obtained composites. Furthermore, based on the BET analysis results, it was found that the surface area of the composite film was obviously enhanced compared with the synthesized graphene oxide. Electrochemical measurements indicated that the modification of the composites on electrode could efficiently enhance the voltammetric response, suggesting the potential application for making electrochemical sensors.

Comparison of multivariate preprocessing techniques as applied to electronic tongue based pattern classification for black tea

International Nuclear Information System (INIS)

Palit, Mousumi; Tudu, Bipan; Bhattacharyya, Nabarun; Dutta, Ankur; Dutta, Pallab Kumar; Jana, Arun; Bandyopadhyay, Rajib; Chatterjee, Anutosh

2010-01-01

In an electronic tongue, preprocessing on raw data precedes pattern analysis and choice of the appropriate preprocessing technique is crucial for the performance of the pattern classifier. While attempting to classify different grades of black tea using a voltammetric electronic tongue, different preprocessing techniques have been explored and a comparison of their performances is presented in this paper. The preprocessing techniques are compared first by a quantitative measurement of separability followed by principle component analysis; and then two different supervised pattern recognition models based on neural networks are used to evaluate the performance of the preprocessing techniques.

Electrochemistry at a Metal Nanoparticle on a Tunneling Film: A Steady-State Model of Current Densities at a Tunneling Ultramicroelectrode.

Science.gov (United States)

Hill, Caleb M; Kim, Jiyeon; Bard, Allen J

2015-09-09

Here, a new methodology is proposed for treating electrochemical current densities in metal-insulator-metal nanoparticle (M-I-MNP) systems. The described model provides broad, practical insights about MNP-mediated electron transfer to redox species in solution, where electron transfer from the underlying electrode to a MNP via tunneling and heterogeneous electron transfer from the MNP to redox species in solution are treated as sequential steps. Tunneling is treated through an adaptation of the Simmons model of tunneling in metal-insulator-metal structures, and explicit equations are provided for tunneling currents, which demonstrate the effect of various experimental parameters, such as insulator thickness and MNP size. Overall, a general approach is demonstrated for determining experimental conditions where tunneling will have a measurable impact on the electrochemistry of M-I-MNP systems.

Electrochemical quantification of the Alzheimer’s disease amyloid-β (1–40 using amyloid-β fibrillization promoting peptide

Directory of Open Access Journals (Sweden)

Satoshi Fujii

2015-12-01

Full Text Available Amyloid-β peptide (Aβ is believed to be an important biomarker for the early diagnosis of Alzheimer’s disease. Therefore, practical and reliable methods to assay Aβ levels have been coveted. In this study, a rapid, sensitive, and selective electrochemical method for Aβ(1–40 detection using Cu2+ redox cycling on peptide-modified gold electrodes was developed. A 19-residue peptide that can promote Aβ fibrillization (AFPP was immobilized onto a gold electrode. After incubating an Aβ solution with the modified electrode for 1 h, a Cu2+ solution was added and cyclic voltammetry measurements were conducted. The voltammetric response was found to be proportional to the Aβ(1–40 concentration in the 0.1–5 μM range, and a detection limit of 18 nM was achieved. Washing with sodium hydroxide and ethylenediaminetetraacetate solutions easily reinitialized the modified electrode. Results obtained using the reinitialized electrode showed good reproducibility. Furthermore, when another amyloidogenic and Cu2+-binding protein amylin was used as the target, no voltammetric response was observed. These results indicate that the AFPP-modified electrode provides a promising, label-free, sensitive, selective, cost-effective, and easy method for the quantification of Aβ. Keywords: Amyloid-β, Alzheimer’s disease (AD, Fibrillization, Electrochemical detection, Nanobiochip, Cu redox

Effect of oxygen implantation on the electrochemical properties of palladium

International Nuclear Information System (INIS)

Fujihana, T.; Ueshima, M.; Takahashi, K.; Iwaki, M.

1995-01-01

Hydrogen presence in metals has significant effects on their properties. A stress caused by hydrogen migration leads to cracks in metals. The suppression of hydrogen incorporation for the protection of such hydrogen embrittlement is one of the most important subjects for industrial engineering. In contrast, the development of active materials for hydrogen absorption and desorption reactions is expected to make a potable storage of hydrogen which is clean and virtually inexhaustible fuel. The electrochemical properties of O + -implanted Pd measured by cyclic voltammetry in a 0.25 mol dm -3 H 2 SO 4 solution were investigated in relation to their composition and structure. Implantation of 16 O + was performed with doses between 10 17 and 10 18 ions cm -2 at 150 keV, and at nearly room temperature. SIMS, ERD combined with RBS, and XRD were used to analyze the composition depth profile and structure of O + -implanted Pd surface layers. The H atoms were accumulated with a gaussian distribution and carbon materials containing the solid solution of PdCx (x = 0.13--0.15) were also formed in the near surface layers during O + -implantation. The distribution of implanted oxygen changed from gaussian to trapezoidal as the dose increased, accompanied by the crystal growth of Pd(OH) 2 , and simultaneously, the amount of accumulated H atoms increased. The voltammetric measurements revealed that with an increase in the dose, the hydrogen absorption was suppressed at the early stage of sweep cycles, and at the final stage, the redox reaction of both hydrogen and Pd was activated. From these results, the authors propose that the carbon materials containing the PdCx formed during O + -implantation suppress the hydrogen absorption, and the metallic Pd like a Pd-black formed by the reduction of Pd(OH) 2 during voltammetric measurements causes the electrochemical activation of O + -implanted Pd

Sensitive determination of citrinin based on molecular imprinted electrochemical sensor

Energy Technology Data Exchange (ETDEWEB)

Atar, Necip [Department of Chemical Engineering, Faculty of Engineering, Pamukkale University, Denizli (Turkey); Yola, Mehmet Lütfi, E-mail: mehmetyola@gmail.com [Department of Metallurgical and Materials Engineering, Faculty of Engineering, Sinop University, Sinop (Turkey); Eren, Tanju [Department of Chemical Engineering, Faculty of Engineering, Pamukkale University, Denizli (Turkey)

2016-01-30

Graphical abstract: - Highlights: • Citrinin-imprinted electrochemical sensor is developed for the sensitive detection of citrinin. • The nanomaterial and citrinin-imprinted surfaces were characterized by several methods. • Citrinin-imprinted electrochemical sensor is sensitive and selective in analysis of food. • Citrinin-imprinted electrochemical sensor is preferred to the other methods. - Abstract: In this report, a novel molecular imprinted voltammetric sensor based on glassy carbon electrode (GCE) modified with platinum nanoparticles (PtNPs) involved in a polyoxometalate (H{sub 3}PW{sub 12}O{sub 40}, POM) functionalized reduced graphene oxide (rGO) was prepared for the determination of citrinin (CIT). The developed surfaces were characterized by using scanning electron microscope (SEM), transmission electron microscope (TEM), X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD) method. CIT imprinted GCE was prepared via electropolymerization process of 80.0 mM pyrrole as monomer in the presence of phosphate buffer solution (pH 6.0) containing 20.0 mM CIT. The linearity range and the detection limit of the developed method were calculated as 1.0 × 10{sup −12}–1.0 × 10{sup −10} M and 2.0 × 10{sup −13} M, respectively. In addition, the voltammetric sensor was applied to rye samples. The stability and selectivity of the voltammetric sensor were also reported.

Sensitive determination of citrinin based on molecular imprinted electrochemical sensor

International Nuclear Information System (INIS)

Atar, Necip; Yola, Mehmet Lütfi; Eren, Tanju

2016-01-01

Graphical abstract: - Highlights: • Citrinin-imprinted electrochemical sensor is developed for the sensitive detection of citrinin. • The nanomaterial and citrinin-imprinted surfaces were characterized by several methods. • Citrinin-imprinted electrochemical sensor is sensitive and selective in analysis of food. • Citrinin-imprinted electrochemical sensor is preferred to the other methods. - Abstract: In this report, a novel molecular imprinted voltammetric sensor based on glassy carbon electrode (GCE) modified with platinum nanoparticles (PtNPs) involved in a polyoxometalate (H_3PW_1_2O_4_0, POM) functionalized reduced graphene oxide (rGO) was prepared for the determination of citrinin (CIT). The developed surfaces were characterized by using scanning electron microscope (SEM), transmission electron microscope (TEM), X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD) method. CIT imprinted GCE was prepared via electropolymerization process of 80.0 mM pyrrole as monomer in the presence of phosphate buffer solution (pH 6.0) containing 20.0 mM CIT. The linearity range and the detection limit of the developed method were calculated as 1.0 × 10"−"1"2–1.0 × 10"−"1"0 M and 2.0 × 10"−"1"3 M, respectively. In addition, the voltammetric sensor was applied to rye samples. The stability and selectivity of the voltammetric sensor were also reported.

CdTe amplification nanoplatforms capped with thioglycolic acid for electrochemical aptasensing of ultra-traces of ATP

Energy Technology Data Exchange (ETDEWEB)

Shamsipur, Mojtaba, E-mail: mshamsipur@yahoo.com [Department of Chemistry, Razi University, P.O. Box 67149-67346, Kermanshah (Iran, Islamic Republic of); Farzin, Leila [Department of Analytical Chemistry, School of Chemistry, College of Science, University of Tehran, P.O. Box 14174-66191, Tehran (Iran, Islamic Republic of); Tabrizi, Mahmoud Amouzadeh [Research Center for Science and Technology in Medicine,Tehran University of Medical Sciences, P.O. Box 14197-33131, Tehran (Iran, Islamic Republic of); Shanehsaz, Maryam [Analytical Chemistry Research Laboratory, Mobin Shimi Azma Company, P.O. Box 14768-44949, Tehran (Iran, Islamic Republic of)

2016-12-01

A “signal off” voltammetric aptasensor was developed for the sensitive and selective detection of ultra-low levels of adenosine triphosphate (ATP). For this purpose, a new strategy based on the principle of recognition-induced switching of aptamers from DNA/DNA duplex to DNA/target complex was designed using thioglycolic acid (TGA)-capped CdTe quantum dots (QDs) as the signal amplifying nano-platforms. Owing to the small size, high surface-to-volume ratio and good conductivity, quantum dots were immobilized on the electrode surface for signal amplification. In this work, methylene blue (MB) adsorbed to DNA was used as a sensitive redox reporter. The intensity of voltammetric signal of MB was found to decrease linearly upon ATP addition over a concentration range of 0.1 nM to 1.6 μM with a correlation coefficient of 0.9924. Under optimized conditions, the aptasensor was able to selectively detect ATP with a limit of detection of 45 pM at 3σ. The results also demonstrated that the QDs-based amplification strategy could be feasible for ATP assay and presented a potential universal method for other small biomolecular aptasensors. - Highlights: • A “signal off” voltammetric aptasensor has been reported. • The DPV technique was used for the determination of ATP. • The determination of ATP up to 1.6 μM with a detection limit 45 pM, respectively.

Electrochemical study and flow injection analysis of paracetamol in pharmaceutical formulations based on screen-printed electrodes and carbon nanotubes

International Nuclear Information System (INIS)

Fanjul-Bolado, Pablo; Lamas-Ardisana, Pedro Jose; Hernandez-Santos, David; Costa-Garcia, Agustin

2009-01-01

Acetaminophenol or paracetamol is one of the most commonly used analgesics in pharmaceutical formulations. Acetaminophen is electroactive and voltammetric mechanistic studies for the electrode processes of the acetaminophenol/N-acetyl-p-quinoneimine redox system are presented. Carbon nanotubes modified screen-printed electrodes with enhanced electron transfer properties are used for the study of the electrochemical-chemical oxidation mechanism of paracetamol at pH 2.0. Quantitative analysis of paracetamol by using its oxidation process (in a Britton-Robinson buffer solution pH 10.0) at +0.20 V (vs. an Ag pseudoreference electrode) on an untreated screen-printed carbon electrode (SPCE) was carried out. Thus, a cyclic voltammetric based reproducible determination of acetaminophen (R.S.D., 2.2%) in the range 2.5 x 10 -6 M to 1 x 10 -3 M, was obtained. However, when SPCEs are used as amperometric detectors coupled to a flow injection analysis (FIA) system, the detection limit achieved for paracetamol was 1 x 10 -7 M, one order of magnitude lower than that obtained by voltammetric analysis. The repeatability of the amperometric detection with the same SPCE is 2% for 15 successive injections of 10 -5 M acetaminophen and do not present any memory effect. Finally, the applicability of using screen-printed carbon electrodes for the electrochemical detection of paracetamol (i.e. for quality control analysis) was demonstrated by using two commercial pharmaceutical products.

Potentiometric Titrations for Measuring the Capacitance of Colloidal Photodoped ZnO Nanocrystals.

Science.gov (United States)

Brozek, Carl K; Hartstein, Kimberly H; Gamelin, Daniel R

2016-08-24

Colloidal semiconductor nanocrystals offer a unique opportunity to bridge molecular and bulk semiconductor redox phenomena. Here, potentiometric titration is demonstrated as a method for quantifying the Fermi levels and charging potentials of free-standing colloidal n-type ZnO nanocrystals possessing between 0 and 20 conduction-band electrons per nanocrystal, corresponding to carrier densities between 0 and 1.2 × 10(20) cm(-3). Potentiometric titration of colloidal semiconductor nanocrystals has not been described previously, and little precedent exists for analogous potentiometric titration of any soluble reductants involving so many electrons. Linear changes in Fermi level vs charge-carrier density are observed for each ensemble of nanocrystals, with slopes that depend on the nanocrystal size. Analysis indicates that the ensemble nanocrystal capacitance is governed by classical surface electrical double layers, showing no evidence of quantum contributions. Systematic shifts in the Fermi level are also observed with specific changes in the identity of the charge-compensating countercation. As a simple and contactless alternative to more common thin-film-based voltammetric techniques, potentiometric titration offers a powerful new approach for quantifying the redox properties of colloidal semiconductor nanocrystals.

2018-04-06T22:48:29Z https://www.ajol.info/index.php/all/oai oai:ojs ...

African Journals Online (AJOL)

article/61361 2018-04-06T22:48:29Z bcse:ART Voltammetric determination of chloramphenicol at electrochemically pretreated glassy carbon electrode Alemu, Hailemichael; Department of Chemistry and Chemical Technology, National University ...

and Cobalt (II)

African Journals Online (AJOL)

studies using cyclic voltammetric techniques on Pb (bi-dptmd) (SCN)2 indicate ... Dotentials. Controlled potential electrolyses (CPE) were performed at a rotating .... silver and thallium porphyrins, where the central cation is reduced and then.

A simple and sensitive method for determination of Norfloxacin in pharmaceutical preparations

Directory of Open Access Journals (Sweden)

Zhuo Ye

2015-06-01

Full Text Available In this approach, a new voltammetric method for determination of norfloxacin was proposed with high sensitivity and wider detection linear range. The used voltammetric sensor was fabricated simply by coating a layer of graphene oxide (GO and Nafion composited film on glassy carbon electrode. The advantage of proposed method was sensitive electrochemical response for norfloxacin, which was attributed to the excellent electrical conductivity of GO and the accumulating function of Nafion under optimum experimental conditions, the present method revealed a good linear response for determination of norfloxacin in the range of 1×10-8mol/L-7×10-6 mol/L with a detection limit of 5×10-9 mol/L. The proposed method was successfully applied in the determination of norfloxacin in capsules with satisfactory results.

Electrooxidation of antihistamine drug methdilazine and its analysis in human urine and blood samples

Directory of Open Access Journals (Sweden)

Nagaraj P. Shetti

2016-12-01

Full Text Available The electrochemical oxidation of an antihistamine drug, methdilazine, was studied in 9.2 pH with 0.2 M phosphate buffer as supporting electrolyte at 25 ± 0.2°C. Glassy carbon electrode was used to perform the experiment at cyclic voltammetry, linear sweep voltammetry and differential pulse voltammetric techniques. The dependence of the current on pH, concentration and scan rate were investigated. Differential pulse voltammetric technique was adopted to know the linear relation between peak current and methdilazine concentration. The linear response was obtained in the range of 3.0 μM–1.0 mM with a detection limit of 0.1 μM. The proposed method was also applied for the quantitative determination of methdilazine in pharmaceuticals and biological samples.

Electrochemical and spectroscopic studies of uranium(IV), -(V), and -(VI) in carbonate-bicarbonate buffers

International Nuclear Information System (INIS)

Wester, D.W.; Sullivan, J.C.

1980-01-01

Recently a need for more detailed knowledge of the chemistry of actinide ions in basic media has arisen in connection with deducing their chemistry in the environment. In this work the results of polarographic, cyclic voltammetric, and spectroscopic studies of U(IV), -(V), and -(VI) in carbonate and bicarbonate media are reported. Polarographic studies were in excellent agreement with those reported previously. Cyclic voltammetric scans confirmed the irreversible reduction to U(V) in both solutions, but disproportionation of the U(V) was observed only in the bicarbonate solutions. The oxidation of U(V) in carbonate was followed spectroscopically for the first time. Reduction in bicarbonate produced U(IV), the spectrum of which is now reported and the oxidation of which was also followed spectroscopically for the first time

Palladium nanoparticles anchored on graphene nanosheets: Methanol, ethanol oxidation reactions and their kinetic studies

KAUST Repository

Nagaraju, Doddahalli H.; Devaraj, Sappani; Balaya, Palani

2014-01-01

nanosheets. The electro-catalytic activity of Gra/Pd nanocomposites toward methanol and ethanol oxidation in alkaline medium was evaluated by cyclic voltammetric studies. 1:1 Gra/Pd nanocomposite exhibited good electro-catalytic activity and efficient

Graphene-based hybrid for enantioselective sensing applications.

Science.gov (United States)

Zor, Erhan; Morales-Narváez, Eden; Alpaydin, Sabri; Bingol, Haluk; Ersoz, Mustafa; Merkoçi, Arben

2017-01-15

Chirality is a major field of research of chemical biology and is essential in pharmacology. Accordingly, approaches for distinguishing between different chiral forms of a compound are of great interest. We report on an efficient and generic enantioselective sensor that is achieved by coupling reduced graphene oxide with γ-cyclodextrin (rGO/γ-CD). The enantioselective sensing capability of the resulting structure was operated in both electrical and optical mode for of tryptophan enantiomers (D-/L-Trp). In this sense, voltammetric and photoluminescence measurements were conducted and the experimental results were compared to molecular docking method. We gain insight into the occurring recognition mechanism with selectivity toward D- and L-Trp as shown in voltammetric, photoluminescence and molecular docking responses. As an enantioselective solid phase on an electrochemical transducer, thanks to the different dimensional interaction of enantiomers with hybrid material, a discrepancy occurs in the Gibbs free energy leading to a difference in oxidation peak potential as observed in electrochemical measurements. The optical sensing principle is based on the energy transfer phenomenon that occurs between photoexcited D-/L-Trp enantiomers and rGO/γ-CD giving rise to an enantioselective photoluminescence quenching due to the tendency of chiral enantiomers to form complexes with γ-CD in different molecular orientations as demonstrated by molecular docking studies. The approach, which is the first demonstration of applicability of molecular docking to show both enantioselective electrochemical and photoluminescence quenching capabilities of a graphene-related hybrid material, is truly new and may have broad interest in combination of experimental and computational methods for enantiosensing of chiral molecules. Copyright © 2016 Elsevier B.V. All rights reserved.

Redox-dependent spatially resolved electrochemistry at graphene and graphite step edges.

Science.gov (United States)

Güell, Aleix G; Cuharuc, Anatolii S; Kim, Yang-Rae; Zhang, Guohui; Tan, Sze-yin; Ebejer, Neil; Unwin, Patrick R

2015-04-28

The electrochemical (EC) behavior of mechanically exfoliated graphene and highly oriented pyrolytic graphite (HOPG) is studied at high spatial resolution in aqueous solutions using Ru(NH3)6(3+/2+) as a redox probe whose standard potential sits close to the intrinsic Fermi level of graphene and graphite. When scanning electrochemical cell microscopy (SECCM) data are coupled with that from complementary techniques (AFM, micro-Raman) applied to the same sample area, different time-dependent EC activity between the basal planes and step edges is revealed. In contrast, other redox couples (ferrocene derivatives) whose potential is further removed from the intrinsic Fermi level of graphene and graphite show uniform and high activity (close to diffusion-control). Macroscopic voltammetric measurements in different environments reveal that the time-dependent behavior after HOPG cleavage, peculiar to Ru(NH3)6(3+/2+), is not associated particularly with any surface contaminants but is reasonably attributed to the spontaneous delamination of the HOPG with time to create partially coupled graphene layers, further supported by conductive AFM measurements. This process has a major impact on the density of states of graphene and graphite edges, particularly at the intrinsic Fermi level to which Ru(NH3)6(3+/2+) is most sensitive. Through the use of an improved voltammetric mode of SECCM, we produce movies of potential-resolved and spatially resolved HOPG activity, revealing how enhanced activity at step edges is a subtle effect for Ru(NH3)6(3+/2+). These latter studies allow us to propose a microscopic model to interpret the EC response of graphene (basal plane and edges) and aged HOPG considering the nontrivial electronic band structure.

A VERSATILIDADE DO ELETRODO DE GOTA PENDENTE DE MERCÚRIO EM QUÍMICA ANALÍTICA - UMA REVISÃO SOBRE RECENTES APLICAÇÕES

Directory of Open Access Journals (Sweden)

Chalder Nogueira Nunes

Full Text Available Voltammetry using mercury electrode as working electrode has been employed in the determination of organic and inorganic compounds in several samples. A review on the applications of this analytical tool is present, covering the period of the last ten years. The emphasis of this work is directed to the hanging mercury drop electrode (HMDE, its advantages, disadvantages and applications. Voltammetric measurements are easily carried out, and present low cost. The review discusses that the use of mercury in the measurements can be a limitation due the toxicity of the element. However, nowadays the necessary of volume of Hg in the measurements is very small, and it can be reused. Thus, the correct disposal of the small amount of waste generated can be minimize environmental risks and human health, according to the principles of Green Chemistry.

Voltammetric Behaviour and Analysis of Fluchloralin

OpenAIRE

K. Balaji; C. Sridevi; N. Ananda Kumar Reddy; K. Mohana Muni Sidda Reddy; C. Suresh Reddy

2010-01-01

The electrochemical reduction behavior of fluchloralin has been studied by D.C.polarography, differential pulse polarography, millicoulometry and controlled potential electrolysis in the universal buffers ranging from 2.0 to 12.0. Kinetic parameters were evaluated and a reduction mechanism was proposed. A simple and rapid differential pulse polarographic method has been developed for the determination of fluchloralin in formulations, grains, soils and spiked water samples. The lower detection...

Adsorptive Cathodic Stripping Voltammetric Determination of ...

African Journals Online (AJOL)

International Pharmaceutical Abstract, Chemical Abstracts, Embase, Index Copernicus, EBSCO, African. Index Medicus ... The bioavailable salt forms of ciprofloxacin in the market are ... A standard stock solution of 500 ... CyberScan pH 510 (Eutech Instruments Pte Ltd., .... variation (5%) of the most important variables i.e..

Adsorptive Cathodic Stripping Voltammetric Determination of ...

African Journals Online (AJOL)

in spiked human urine with no matrix effect (i.e. LLOQ 0.01 μg/ml, precision (RSD < 15%) and accuracy. (85 – 115%)) ... use in quality control and pharmacokinetics studies. ... subsequently approved by US Food and Drug ... high performance liquid chromatography (HPLC) ... factors, the optimizer function of Modde software.

Adsorptive Cathodic Stripping Voltammetric Determination of ...

African Journals Online (AJOL)

Department of Analytical Chemistry and Toxicology, Hanoi University of Pharmacy, 13-15 Le .... factors, the optimizer function of Modde software ... implementing this experiment design, other ... influence of the interaction of buffer pH with.

Electrochemical behavior of monolayer and bilayer graphene.

Science.gov (United States)

Valota, Anna T; Kinloch, Ian A; Novoselov, Kostya S; Casiraghi, Cinzia; Eckmann, Axel; Hill, Ernie W; Dryfe, Robert A W

2011-11-22

Results of a study on the electrochemical properties of exfoliated single and multilayer graphene flakes are presented. Graphene flakes were deposited on silicon/silicon oxide wafers to enable fast and accurate characterization by optical microscopy and Raman spectroscopy. Conductive silver paint and silver wires were used to fabricate contacts; epoxy resin was employed as a masking coating in order to expose a stable, well-defined area of graphene. Both multilayer and monolayer graphene microelectrodes showed quasi-reversible behavior during voltammetric measurements in potassium ferricyanide. However, the standard heterogeneous charge transfer rate constant, k°, was estimated to be higher for monolayer graphene flakes. © 2011 American Chemical Society

Optimization of the use of carbon paste electrodes (CPE for electrochemical study of the chalcopyrite

Directory of Open Access Journals (Sweden)

Daniela G. Horta

2009-01-01

Full Text Available The use of carbon paste electrodes (CPE of mineral sulfides can be useful for electrochemical studies to overcome problems by using massive ones. Using CPE-chalcopyrite some variables were electrochemically evaluated. These variables were: (i the atmosphere of preparation (air or argon of CPE and elapsed time till its use; (ii scan rate for voltammetric measurements and (iii chalcopyrite concentration in the CPE. Based on cyclic voltammetry, open-circuit potential and electrochemical impedance results the recommendations are: oxygen-free atmosphere to prepare and kept the CPE until around two ours, scan rates from 10 to 40 mV s-1, and chalcopyrite concentrations > 20%.

The effect of preparation parameters i thermal decomposition of ruthenium dioxide electrodes on chlorine elctro-catalytic activity

Energy Technology Data Exchange (ETDEWEB)

Luu, Tran Le; Kim, Choon Soo; Kim, Ji Ye; Kim, Seong Hwan; Yoon, Je Yong [Dept. of Chemical and Biological Engineering, Institute of Chemical Process, Seoul National University,Seoul (Korea, Republic of)

2015-05-15

When fabricating a RuO{sub 2} electrode, the high electro-catalytic activity in chlorine evolution is considered as one of the most important factors. Thermal decomposition method carried out under various fabrication conditions including the types of solvents, precursors, and calcination times have led to the enhancement electro-catalytic activity of RuO{sub 2} electrode in chlorine evolution. Nevertheless, it has not been fully investigated how these parameters directly affect to the chlorine evolution efficiency in the RuO{sub 2} electrode. Therefore, the aim of this study was to investigate the effect on the chlorine evolution in RuO{sub 2} electrodes, depending upon the preparation parameters including solvents, precursors, and calcination times. As major results, the chlorine evolution efficiency was dominantly affected by these three major preparation parameters. The RuO{sub 2} electrode fabricated with ethanol as the solvent showed highest chlorine evolution efficiency. The choice of Ru(AcAc){sub 3} as precursor and the increase of the calcination time up to 3 h are also the good choices for increasing chlorine electrocatalytic activities. The chlorine evolution efficiency was not significantly related to the total voltammetric charge but to the outer voltammetric charge, which is affected by the morphology of the RuO{sub 2} electrode surface. The size and number of cracks on the electrode surfaces or the outer voltammetric charges increased with easily evaporated solvents, decomposed precursors, and tensile stress from longer thermal treatments.

The effect of preparation parameters i thermal decomposition of ruthenium dioxide electrodes on chlorine elctro-catalytic activity

International Nuclear Information System (INIS)

Luu, Tran Le; Kim, Choon Soo; Kim, Ji Ye; Kim, Seong Hwan; Yoon, Je Yong

2015-01-01

When fabricating a RuO_2 electrode, the high electro-catalytic activity in chlorine evolution is considered as one of the most important factors. Thermal decomposition method carried out under various fabrication conditions including the types of solvents, precursors, and calcination times have led to the enhancement electro-catalytic activity of RuO_2 electrode in chlorine evolution. Nevertheless, it has not been fully investigated how these parameters directly affect to the chlorine evolution efficiency in the RuO_2 electrode. Therefore, the aim of this study was to investigate the effect on the chlorine evolution in RuO_2 electrodes, depending upon the preparation parameters including solvents, precursors, and calcination times. As major results, the chlorine evolution efficiency was dominantly affected by these three major preparation parameters. The RuO_2 electrode fabricated with ethanol as the solvent showed highest chlorine evolution efficiency. The choice of Ru(AcAc)_3 as precursor and the increase of the calcination time up to 3 h are also the good choices for increasing chlorine electrocatalytic activities. The chlorine evolution efficiency was not significantly related to the total voltammetric charge but to the outer voltammetric charge, which is affected by the morphology of the RuO_2 electrode surface. The size and number of cracks on the electrode surfaces or the outer voltammetric charges increased with easily evaporated solvents, decomposed precursors, and tensile stress from longer thermal treatments

Chalcogenide oxygen reduction reaction catalysis: X-ray photoelectron spectroscopy with Ru, Ru/Se and Ru/S samples emersed from aqueous media

Energy Technology Data Exchange (ETDEWEB)

Lewera, A. [Department of Chemistry, University of Illinois at Urbana-Champaign, Urbana, IL 61801 (United States); Department of Chemistry, Warsaw University, Pasteura 1, 02-093 Warsaw (Poland); Inukai, J. [Clean Energy Research Center, University of Yamanashi, 7-32 Miyamae-cho, Kofu 400-0006 (Japan); Zhou, W.P. [Department of Chemistry, University of Illinois at Urbana-Champaign, Urbana, IL 61801 (United States); Cao, D. [Department of Chemistry, University of Illinois at Urbana-Champaign, Urbana, IL 61801 (United States); College of Material Science and Chemical Engineering, Harbin Engineering University, Harbin 150001 (China); Duong, H.T. [Department of Chemistry, University of Illinois at Urbana-Champaign, Urbana, IL 61801 (United States); Alonso-Vante, N. [Laboratory of Electrocatalysis, UMR-CNRS 6503, University of Poitiers, F-86022 Poitiers (France)]. E-mail: Nicolas.Alonso.Vante@univ-poitiers.fr; Wieckowski, A. [Department of Chemistry, University of Illinois at Urbana-Champaign, Urbana, IL 61801 (United States)]. E-mail: andrzej@scs.uiuc.edu

2007-05-10

Oxygen reduction Ru/Se and Ru/S fuel cell surface chalcogenide catalysts were prepared via chemical reaction of reduced Ru nanoparticles with selenium and sulfur in xylenes [D. Cao, A. Wieckowski, J. Inukai, N. Alonso-Vante, J. Electrochem. Soc. 153 (2006) A869]. The chalcogenide samples - as well as the starting chalcogens-free Ru nanoparticle material - were immobilized on a gold disk for X-ray Photoelectron Spectroscopy (XPS) characterization. While we found oxygen in most of the samples, predominantly from Ru oxides, we conclude that the oxygen on Ru/S may be located in subsurface sites: the subsurface oxygen. We also found that the transformation of the oxidized Ru black to metallic Ru required intensive electrochemical treatment, including hydrogen evolution. In contrast, five cyclic voltammetric scans in the potential range from 0.00 and 0.75 V versus RHE were sufficient to remove the oxygen forms from Ru/Se and, to a large extent, from Ru/S. We therefore conclude that Ru metal is protected against oxidation to Ru oxides by the chalcogens additives. The voltammetric treatment in the 0.00 and 0.75 V range also removed the SeO{sub 2} or SO {sub x} forms leaving anionic/elemental Se or S on the surface. Upon larger amplitude voltammetric cycling, from 0.00 to 1.20 V versus RHE, both Se and S were dissolved and the dissolution process was coincidental with the oxygen growth in/on the Ru samples.

Chalcogenide oxygen reduction reaction catalysis: X-ray photoelectron spectroscopy with Ru, Ru/Se and Ru/S samples emersed from aqueous media

International Nuclear Information System (INIS)

Lewera, A.; Inukai, J.; Zhou, W.P.; Cao, D.; Duong, H.T.; Alonso-Vante, N.; Wieckowski, A.

2007-01-01

Oxygen reduction Ru/Se and Ru/S fuel cell surface chalcogenide catalysts were prepared via chemical reaction of reduced Ru nanoparticles with selenium and sulfur in xylenes [D. Cao, A. Wieckowski, J. Inukai, N. Alonso-Vante, J. Electrochem. Soc. 153 (2006) A869]. The chalcogenide samples - as well as the starting chalcogens-free Ru nanoparticle material - were immobilized on a gold disk for X-ray Photoelectron Spectroscopy (XPS) characterization. While we found oxygen in most of the samples, predominantly from Ru oxides, we conclude that the oxygen on Ru/S may be located in subsurface sites: the subsurface oxygen. We also found that the transformation of the oxidized Ru black to metallic Ru required intensive electrochemical treatment, including hydrogen evolution. In contrast, five cyclic voltammetric scans in the potential range from 0.00 and 0.75 V versus RHE were sufficient to remove the oxygen forms from Ru/Se and, to a large extent, from Ru/S. We therefore conclude that Ru metal is protected against oxidation to Ru oxides by the chalcogens additives. The voltammetric treatment in the 0.00 and 0.75 V range also removed the SeO 2 or SO x forms leaving anionic/elemental Se or S on the surface. Upon larger amplitude voltammetric cycling, from 0.00 to 1.20 V versus RHE, both Se and S were dissolved and the dissolution process was coincidental with the oxygen growth in/on the Ru samples

Electrochemical study and flow injection analysis of paracetamol in pharmaceutical formulations based on screen-printed electrodes and carbon nanotubes

Energy Technology Data Exchange (ETDEWEB)

Fanjul-Bolado, Pablo [DropSens, S.L., Edificio Severo Ochoa, Campus El Cristo, 33006 Oviedo, Asturias (Spain); Lamas-Ardisana, Pedro Jose [Departamento de Quimica Fisica y Analitica, Universidad de Oviedo, Julian Claveria 8, 33006 Oviedo, Asturias (Spain); Hernandez-Santos, David [DropSens, S.L., Edificio Severo Ochoa, Campus El Cristo, 33006 Oviedo, Asturias (Spain); Costa-Garcia, Agustin, E-mail: costa@fq.uniovi.es [Departamento de Quimica Fisica y Analitica, Universidad de Oviedo, Julian Claveria 8, 33006 Oviedo, Asturias (Spain)

2009-04-13

Acetaminophenol or paracetamol is one of the most commonly used analgesics in pharmaceutical formulations. Acetaminophen is electroactive and voltammetric mechanistic studies for the electrode processes of the acetaminophenol/N-acetyl-p-quinoneimine redox system are presented. Carbon nanotubes modified screen-printed electrodes with enhanced electron transfer properties are used for the study of the electrochemical-chemical oxidation mechanism of paracetamol at pH 2.0. Quantitative analysis of paracetamol by using its oxidation process (in a Britton-Robinson buffer solution pH 10.0) at +0.20 V (vs. an Ag pseudoreference electrode) on an untreated screen-printed carbon electrode (SPCE) was carried out. Thus, a cyclic voltammetric based reproducible determination of acetaminophen (R.S.D., 2.2%) in the range 2.5 x 10{sup -6} M to 1 x 10{sup -3} M, was obtained. However, when SPCEs are used as amperometric detectors coupled to a flow injection analysis (FIA) system, the detection limit achieved for paracetamol was 1 x 10{sup -7} M, one order of magnitude lower than that obtained by voltammetric analysis. The repeatability of the amperometric detection with the same SPCE is 2% for 15 successive injections of 10{sup -5} M acetaminophen and do not present any memory effect. Finally, the applicability of using screen-printed carbon electrodes for the electrochemical detection of paracetamol (i.e. for quality control analysis) was demonstrated by using two commercial pharmaceutical products.

Nucleation and growth phenomena of cadmium at tungsten in basic aluminum chloride/1-methyl-3-ethylimidazolium chloride ionic liquid

International Nuclear Information System (INIS)

Rao, G.M.; Wilkes, J.S.

1990-01-01

This paper presents a study to investigate the mechanism of the electrodeposition of cadmium in a basic melt using cyclic voltammetric chronoamperometric and chronopotention metric methods at tungsten electrode. In addition, proton nuclear magnetic resonance data are presented

Electrochemical Studies for Cation Recognition with Diazo-Coupled Calix[4]arenes

Directory of Open Access Journals (Sweden)

Bongsu Kim

2015-01-01

Full Text Available The electrochemical properties of diazophenylcalix[4]arenes bearing ortho-carboxyl group (o-CAC and ortho-ester group (o-EAC, respectively, in the presence of various metal ions were investigated by voltammetry in CH3CN. o-CAC and o-EAC showed voltammetric changes toward divalent metal ions and no significant changes with monovalent alkali metal ions. However, o-CAC preferentially binds with alkaline earth and transition metal ions, whereas no significant changes in voltammetric signals are observed in o-EAC with alkaline earth metal ions. o-EAC only binds with other transition metal ions. This can be explained on metal ion complexation-induced release of proton from the azophenol to the quinone-hydrazone tautomer followed by internal complexation of the metal ion with aid of nitrogen atoms and ortho-carbonyl groups in the diazophenylazocalix[4]arenes.

Electrochemical detection of rutin with a carbon ionic liquid electrode modified by Nafion, graphene oxide and ionic liquid composite

International Nuclear Information System (INIS)

Hu, S.; Xiang, J.; Zhang, L.; Zhu, H.; Liu, S.; Sun, W.

2012-01-01

We report on a carbon ionic liquid electrode modified with a composite made from Nafion, graphene oxide and ionic liquid, and its application to the sensitive determination of rutin. The modified electrode was characterized by cyclic voltammetry and electrochemical impedance spectroscopy. It shows excellent cyclic voltammetric and differential pulse voltammetric performance due to the presence of nanoscale graphene oxide and the ionic liquid, and their interaction. A pair of well-defined redox peaks of rutin appears at pH 3.0, and the reduction peak current is linearly related to its concentration in the range from 0.08 μM to 0.1 mM with a detection limit of 0.016 μM (at 3σ). The modified electrode displays excellent selectivity and good stability, and was successfully applied to the determination of rutin in tablets with good recovery. (author)

Electrochemical monitoring of citric acid production by Aspergillus niger

International Nuclear Information System (INIS)

Kutyła-Olesiuk, Anna; Wawrzyniak, Urszula E.; Ciosek, Patrycja; Wróblewski, Wojciech

2014-01-01

Highlights: • Citric acid fermentation process (production) by Aspergillus niger. • Qualitative/quantitative monitoring of standard culture and culture infected with yeast. • Electronic tongue based on potentiometric and voltammetric sensors. • Evaluation of the progress and the correctness of the fermentation process. • The highest classification abilities of the hybrid electronic tongue. - Abstract: Hybrid electronic tongue was developed for the monitoring of citric acid production by Aspergillus niger. The system based on various potentiometric/voltammetric sensors and appropriate chemometric techniques provided correct qualitative and quantitative classification of the samples collected during standard Aspergillus niger culture and culture infected with yeast. The performance of the proposed approach was compared with the monitoring of the fermentation process carried out using classical methods. The results obtained proved, that the designed hybrid electronic tongue was able to evaluate the progress and correctness of the fermentation process

Electrochemical monitoring of citric acid production by Aspergillus niger

Energy Technology Data Exchange (ETDEWEB)

Kutyła-Olesiuk, Anna; Wawrzyniak, Urszula E.; Ciosek, Patrycja; Wróblewski, Wojciech, E-mail: wuwu@ch.pw.edu.pl

2014-05-01

Highlights: • Citric acid fermentation process (production) by Aspergillus niger. • Qualitative/quantitative monitoring of standard culture and culture infected with yeast. • Electronic tongue based on potentiometric and voltammetric sensors. • Evaluation of the progress and the correctness of the fermentation process. • The highest classification abilities of the hybrid electronic tongue. - Abstract: Hybrid electronic tongue was developed for the monitoring of citric acid production by Aspergillus niger. The system based on various potentiometric/voltammetric sensors and appropriate chemometric techniques provided correct qualitative and quantitative classification of the samples collected during standard Aspergillus niger culture and culture infected with yeast. The performance of the proposed approach was compared with the monitoring of the fermentation process carried out using classical methods. The results obtained proved, that the designed hybrid electronic tongue was able to evaluate the progress and correctness of the fermentation process.

Morphological and electrochemical studies of spherical boron doped diamond electrodes

Energy Technology Data Exchange (ETDEWEB)

Mendes de Barros, R.C. [IQ/USP, Av. Lineu Prestes, 748, Bloco 2 Superior, Cidade Universitaria, Sao Paulo/SP, 05508-900 (Brazil); Ferreira, N.G. [LAS/INPE, Av. dos Astronautas, 1758, Jardim da Granja, Sao Jose dos Campos/SP, 12245-970 (Brazil); Azevedo, A.F. [LAS/INPE, Av. dos Astronautas, 1758, Jardim da Granja, Sao Jose dos Campos/SP, 12245-970 (Brazil); Corat, E.J. [LAS/INPE, Av. dos Astronautas, 1758, Jardim da Granja, Sao Jose dos Campos/SP, 12245-970 (Brazil); Sumodjo, P.T.A. [IQ/USP, Av. Lineu Prestes, 748, Bloco 2 Superior, Cidade Universitaria, Sao Paulo/SP, 05508-900 (Brazil); Serrano, S.H.P. [IQ/USP, Av. Lineu Prestes, 748, Bloco 2 Superior, Cidade Universitaria, Sao Paulo/SP, 05508-900 (Brazil)]. E-mail: shps@iq.usp.br

2006-08-14

Morphological and electrochemical characteristics of boron doped diamond electrode in new geometric shape are presented. The main purpose of this study is a comparison among voltammetric behavior of planar glassy carbon electrode (GCE), planar boron doped diamond electrode (PDDE) and spherical boron doped diamond electrode (SDDE), obtained from similar experimental parameters. SDDE was obtained by the growth of boron doped film on textured molybdenum tip. This electrode does not present microelectrode characteristics. However, its voltammetric peak current, determined at low scan rates, is largest associated to the smallest {delta}E {sub p} values for ferrocyanide system when compared with PDDE or GCE. In addition, the capacitance is about 200 times smaller than that for GCE. These results show that the analytical performance of boron doped diamond electrodes can be implemented just by the change of sensor geometry, from plane to spherical shape.

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

Science.gov (United States)

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.

Catalyst Degradation in High Temperature Proton Exchange Membrane Fuel Cells Based on Acid Doped Polybenzimidazole Membranes

DEFF Research Database (Denmark)

Cleemann, Lars Nilausen; Buazar, F.; Li, Qingfeng

2013-01-01

and multi‐walled carbon nanotubes were used as supports for electrode catalysts and evaluated in accelerated durability tests under potential cycling at 150 °C. Measurements of open circuit voltage, area specific resistance and hydrogen permeation through the membrane were carried out, indicating little...... contribution of the membrane degradation to the performance losses during the potential cycling tests. As the major mechanism of the fuel cell performance degradation, the electrochemical active area of the cathodic catalysts showed a steady decrease in the cyclic voltammetric measurements, which was also......Degradation of carbon supported platinum catalysts is a major failure mode for the long term durability of high temperature proton exchange membrane fuel cells based on phosphoric acid doped polybenzimidazole membranes. With Vulcan carbon black as a reference, thermally treated carbon black...

Enhancement of ethanol oxidation at Pt and PtRu nanoparticles dispersed over hybrid zirconia-rhodium supports

Science.gov (United States)

Rutkowska, Iwona A.; Koster, Margaretta D.; Blanchard, Gary J.; Kulesza, Pawel J.

2014-12-01

A catalytic material for electrooxidation of ethanol that utilizes PtRu nanoparticles dispersed over thin films of rhodium-free and rhodium-containing zirconia (ZrO2) supports is described here. The enhancement of electrocatalytic activity (particularly in the potential range as low as 0.25-0.5 V vs. RHE), that has been achieved by dispersing PtRu nanoparticles (loading, 100 μg cm-2) over the hybrid Rh-ZrO2 support composed of nanostructured zirconia and metallic rhodium particles, is clearly evident from comparison of the respective voltammetric and chronoamperometric current densities recorded at room temperature (22 °C) in 0.5 mol dm-3 H2SO4 containing 0.5 mol dm-3 ethanol. Porous ZrO2 nanostructures, that provide a large population of hydroxyl groups in acidic medium in the vicinity of PtRu sites, are expected to facilitate the ruthenium-induced removal of passivating CO adsorbates from platinum, as is apparent from the diagnostic experiments with a small organic molecule such as methanol. Although Rh itself does not show directly any activity toward ethanol oxidation, the metal is expected to facilitate C-C bond splitting in C2H5OH. It has also been found during parallel voltammetric and chronoamperometric measurements that the hybrid Rh-ZrO2 support increases activity of the platinum component itself toward ethanol oxidation in the low potential range.

Electrocatalytic oxidation of deferiprone and its determination on a carbon nanotube-modified glassy carbon electrode

Energy Technology Data Exchange (ETDEWEB)

Yadegari, H. [Department of Chemistry, Faculty of Science, K.N. Toosi University of Technology, P.O. Box 16315-1618, Tehran (Iran, Islamic Republic of); Jabbari, A. [Department of Chemistry, Faculty of Science, K.N. Toosi University of Technology, P.O. Box 16315-1618, Tehran (Iran, Islamic Republic of)], E-mail: jabbari@kntu.ac.ir; Heli, H.; Moosavi-Movahedi, A.A. [Institute of Biochemistry and Biophysics, University of Tehran, Tehran (Iran, Islamic Republic of); Karimian, K. [Arasto Pharmaceutical Chemicals Inc., Tehran (Iran, Islamic Republic of); Khodadadi, A. [Department of Chemical Engineering, Faculty of Engineering, University of Tehran, Tehran (Iran, Islamic Republic of)

2008-02-15

The electrochemical behavior of the anti-thalassemia and anti-HIV replication drug, deferiprone, was investigated on a carbon nanotube-modified glassy carbon (GC-CNT) electrode in phosphate buffer solution, pH 7.40 (PBS). During oxidation of deferiprone, two irreversible anodic peaks, with E{sub 1}{sup 0}=452 and E{sub 2}{sup 0}=906mV, appeared, using GC-CNT. Cyclic voltammetric study indicated that the oxidation process is irreversible and diffusion controlled. The number of exchanged electrons in the electro-oxidation process was obtained, and the data indicated that deferiprone is oxidized via two two-electron steps. The results revealed that carbon nanotube (CNT) promotes the rate of oxidation by increasing the peak current, so that deferiprone is oxidized at lower potentials, which thermodynamically is more favorable. This result was confirmed by impedance measurements. The diffusion coefficient, electron-transfer coefficient and heterogeneous electron-transfer rate constant of deferiprone were found to be 1.49 x 10{sup -6} cm{sup 2} s{sup -1}, 0.44, and 3.83 x 10{sup -3} cm s{sup -1}, respectively. A sensitive, simple and time-saving differential-pulse voltammetric procedure was developed for the analysis of deferiprone. Using the proposed method, deferiprone can be determined with a detection limit of 5.25 x 10{sup -7} M. The applicability of the method to direct assays of spiked human serum and urine fluids is described.

Graphite Screen-Printed Electrodes Applied for the Accurate and Reagentless Sensing of pH.

Science.gov (United States)

Galdino, Flávia E; Smith, Jamie P; Kwamou, Sophie I; Kampouris, Dimitrios K; Iniesta, Jesus; Smith, Graham C; Bonacin, Juliano A; Banks, Craig E

2015-12-01

A reagentless pH sensor based upon disposable and economical graphite screen-printed electrodes (GSPEs) is demonstrated for the first time. The voltammetric pH sensor utilizes GSPEs which are chemically pretreated to form surface immobilized oxygenated species that, when their redox behavior is monitored, give a Nernstian response over a large pH range (1-13). An excellent experimental correlation is observed between the voltammetric potential and pH over the entire pH range of 1-13 providing a simple approach with which to monitor solution pH. Such a linear response over this dynamic pH range is not usually expected but rather deviation from linearity is encountered at alkaline pH values; absence of this has previously been attributed to a change in the pKa value of surface immobilized groups from that of solution phase species. This non-deviation, which is observed here in the case of our facile produced reagentless pH sensor and also reported in the literature for pH sensitive compounds immobilized upon carbon electrodes/surfaces, where a linear response is observed over the entire pH range, is explained alternatively for the first time. The performance of the GSPE pH sensor is also directly compared with a glass pH probe and applied to the measurement of pH in "real" unbuffered samples where an excellent correlation between the two protocols is observed validating the proposed GSPE pH sensor.

Electrochemical modification of a pyrolytic graphite sheet for improved negative electrode performance in the vanadium redox flow battery

Science.gov (United States)

Kabir, Humayun; Gyan, Isaiah O.; Francis Cheng, I.

2017-02-01

The vanadium redox flow battery is a promising technology for buffering renewable energies. It is recognized that negative electrode is the limitation in this device where there are problems of slow heterogeneous electron transfer (HET) of V3+/2+ and parasitic H2 evolution. Any methods aimed at addressing one of these barriers must assess the effects on the other. We examine electrochemical enhancement of a common commercially available material. Treatment of Panasonic pyrolytic graphite sheets is through oxidation at 2.1 V vs. Ag/AgCl for 1 min in 1 M H2SO4. This increases the standard HET rate for V3+/2+ from 3.2 × 10-7 to 1 × 10-3 cm/s, one of the highest in literature and shifts voltammetric reductive peak potential from -1.0 V to -0.65 V in 50 mM V3+ in 1 M H2SO4. Infrared analysis of the surfaces indicates formation of Csbnd OH, Cdbnd O, and Csbnd O functionalities. These groups catalyze HET with V3+/2+ as hypothesized by Skyllas-Kasacos. Also of significance is that electrode modification decreases the fraction of the current directed towards H2 evolution. This proportion decreases by two orders of a magnitude from 12% to 0.1% as measured at the respective voltammetric peak potentials of -1.0 V (pristine) and -0.65 V (modified).

An investigation of 2,5-di-tertbutyl-1,4-bis(methoxyethoxy)benzene in ether-based electrolytes

Energy Technology Data Exchange (ETDEWEB)

Su, Liang; Ferrandon, Magali; Barton, John L.; de la Rosa, Noel Upia; Vaughey, John T.; Brushett, Fikile R.

2017-08-01

The identification and development of conductive electrolytes with high concentrations of redox active species is key to realizing energy-dense nonaqueous flow batteries. Herein, we explore the use of ether solvents (1,3-dioxolane (DOL), 1,2-dimethoxyethane (DME), diethylene glycol dimethyl ether (DEGDME), and tetraethylene glycol dimethyl ether (TEGDME)) as the basis for redox electrolytes containing a lithium ion supporting salt (LiBF4 or LiTFSI) and 2,5-di-tert-butyl-1,4-bis(2-methoxyethoxy)benzene (DBBB) as an active material. An automated high-throughput platform is employed to screen various electrolyte compositions by measuring solution conductivity and solute solubility as a function of solvent and salt type, component concentration, and temperature. Subsequently, the electrochemical and transport properties of select redox electrolytes are characterized by cyclic voltammetry using glassy carbon disk electrodes and by linear sweep voltammetry using carbon fiber ultramicroelectrodes. In general, improvements in electrolyte conductivity and solute solubility are observed with ether-based formulations as compared to previously reported propylene carbonate (PC)-based formulations. In particular, the addition of DOL to a DME-based electrolyte increases the conductivity and decreases the temperature for solubilization at high LiTFSI and DBBB concentrations. The redox behavior of DBBB remains consistent across the range of concentrations tested while the diffusion coefficient scales with changes in solution viscosity.

Journal of Chemical Sciences | Indian Academy of Sciences

Indian Academy of Sciences (India)

Home; Journals; Journal of Chemical Sciences; Volume 121; Issue 2. Voltammetric behaviour of levodopa and its quantification in pharmaceuticals using a -cyclodextrine doped poly (2,5-diaminobenzenesulfonic acid) modified electrode. Mehmet Aslanoglu Aysegul Kutluay Sultan Goktas Serpil Karabulut. Full Papers ...

A Comparison of Fully Automated Methods of Data Analysis and Computer Assisted Heuristic Methods in an Electrode Kinetic Study of the Pathologically Variable [Fe(CN) 6 ] 3–/4– Process by AC Voltammetry

KAUST Repository

Morris, Graham P.; Simonov, Alexandr N.; Mashkina, Elena A.; Bordas, Rafel; Gillow, Kathryn; Baker, Ruth E.; Gavaghan, David J.; Bond, Alan M.

2013-01-01

Fully automated and computer assisted heuristic data analysis approaches have been applied to a series of AC voltammetric experiments undertaken on the [Fe(CN)6]3-/4- process at a glassy carbon electrode in 3 M KCl aqueous electrolyte. The recovered

Electrochemistry of Hemin on Single-Crystal Au(111)-electrode Surfaces

DEFF Research Database (Denmark)

Zhang, Ling; Ulstrup, Jens; Zhang, Jingdong

adsorption on well-defined single-crystal Au(111)-electrode surfaces using electrochemistry combined with scanning tunnelling microscopy under electrochemical control. Hemin gives two voltammetric peaks assigned to adsorbed monomers and dimmers (Fig. 1B). In situ STM shows that hemin self...

Depletive stripping chronopotentiometry : a major step forward in electrochemical stripping techniques for metal ion speciation analysis

NARCIS (Netherlands)

Town, R.M.; Leeuwen, van H.P.

2004-01-01

A comparative evaluation of the utility of the various modes of stripping chronopotentiometry (SCP) for trace metal speciation analysis is presented in the broad context of stripping voltammetric techniques. The remarkable fundamental advantages of depletive SCP at scanned deposition potential

Characterisation of material behaviour in high temperature aqueous environments by means of electrochemical techniques

International Nuclear Information System (INIS)

Bojinov, M.; Laitinen, T.; Maekelae, K.; Sirkiae, P.; Beverskog, B.

1998-01-01

Electrochemical measurements in solutions simulating power plant coolants are complicated by the low conductivity of the water, especially in the case of boiling water reactor (BWR) environments. To be able to obtain useful information also in BWR conditions, electrochemical techniques based on a thin-layer electrode arrangement are introduced. This arrangement makes it possible to perform voltammetric and electrochemical impedance measurements in high-temperature water with a room temperature conductivity (κ) as low as 0.1 μScm -1 . A combination of these results with those obtained by means of measuring the resistance of the surface film using the contact electric resistance (CER) technique facilitates versatile characterisation of oxide film behaviour. Examples are given on impedance and CER measurements of the oxide films formed on AISI 316 stainless steel in high temperature high purity (κ -1 ) water and on OX18H10T stainless steel in VVER water. Correlations between temperature, hydrogen and oxygen content of the solution and the oxide behaviour are discussed. (author)

Ultramicrosensors based on transition metal hexacyanoferrates for scanning electrochemical microscopy

Directory of Open Access Journals (Sweden)

Maria A. Komkova

2013-10-01

Full Text Available We report here a way for improving the stability of ultramicroelectrodes (UME based on hexacyanoferrate-modified metals for the detection of hydrogen peroxide. The most stable sensors were obtained by electrochemical deposition of six layers of hexacyanoferrates (HCF, more specifically, an alternating pattern of three layers of Prussian Blue and three layers of Ni–HCF. The microelectrodes modified with mixed layers were continuously monitored in 1 mM hydrogen peroxide and proved to be stable for more than 5 h under these conditions. The mixed layer microelectrodes exhibited a stability which is five times as high as the stability of conventional Prussian Blue-modified UMEs. The sensitivity of the mixed layer sensor was 0.32 A·M−1·cm−2, and the detection limit was 10 µM. The mixed layer-based UMEs were used as sensors in scanning electrochemical microscopy (SECM experiments for imaging of hydrogen peroxide evolution.

Revisited: the conception of lability of metal complexes

NARCIS (Netherlands)

Leeuwen, van H.P.

2001-01-01

Starting from the original reaction layer concept, the voltammetric properties of electroinactive metal complexes are critically reviewed in terms of their finite rates of dissociation into electroactive free metal ions. The limiting conditions for the reaction layer-based flux expressions are made

Reduction of NO adlayers on Pt(110) and Pt(111) in acidic media: evidence for adsorption site-specific reduction

NARCIS (Netherlands)

Rosca, V.; Beltramo, G.L.; Koper, M.T.M.

2005-01-01

We present a combined in situ Fourier transform infrared reflection-absorption spectroscopy and voltammetric study of the reduction of saturated and subsaturated NO adlayers on Pt(111) and Pt(110) single-crystal surfaces in acidic media. The stripping voltammetry experiments and the associated

Lability criteria for metal complexes in micro-electrode voltammetry

NARCIS (Netherlands)

Leeuwen, van H.P.; Pinheiro, J.P.

1999-01-01

Theoretical expressions are derived for the voltammetric lability criteria of metal complexes in the micro-electrode regime. The treatment includes three limiting situations: (i) the macro-electrode limit, where both the diffusion layer and the dissociation reaction layer are linear; (ii) an

Assembling gold nanorods on a poly-cysteine modified glassy carbon electrode strongly enhance the electrochemical response to tetrabromobisphenol A

International Nuclear Information System (INIS)

Wang, Yanying; Liu, Guishen; Hou, Xiaodong; Huang, Yina; Li, Chunya; Wu, Kangbing

2016-01-01

Cysteine (Cys) was electrochemically deposited on a glassy carbon electrode (GCE) by cyclic voltammetry. The poly-Cys modified electrode was placed in a solution of gold nanorods (GNRs) to induced self-assembly of the GNRs. The GNRs/poly-Cys/GCEs were characterized by scanning electron microscopy and electrochemical impedance spectroscopy. A voltammetric study on tetrabromobisphenol A (TBBPA) with this GCE showed the current response to be enhanced by a factor of 11 compared to a non-modified GCE. Based on these findings, a square wave voltammetric assay was worked out. Under optimized conditions, a linear relationship between the oxidation peak current and TBBPA is found for the 10 nM to 10 μM concentration range. The detection limit is 3.2 nM (at an S/N ratio of 3). The electrode was successfully applied to the determination of TBBPA in spiked tap water and lake water samples. (author)

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

Science.gov (United States)

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.

Microgravimetric Studies of Selenium Electrodeposition Onto Different Substrates

Directory of Open Access Journals (Sweden)

Kowalik R.

2014-10-01

Full Text Available The mechanism of selenium electrodeposition from sulfuric acid solution on different substrates was studied with the electrochemical techniques. The cyclic voltammetry was combined with the quartz crystal microbalance technique to analyze selenium deposition process. The electrochemical reduction of selenous acid on gold, silver and copper electrodes was investigated. It was found that reduction of selenous acid is a very complex process and it strongly depends from the applied substrate. The voltammetric measurements indicate the range of potentials in which the process of reduction of selenous acids on the applied substrate is possible. Additionally, the microgravimetric data confirm the deposition of selenium and they reveal the mechanism of the deposition process.

Cholesterol biosensor based on rf sputtered zinc oxide nanoporous thin film

International Nuclear Information System (INIS)

Singh, S. P.; Arya, Sunil K.; Pandey, Pratibha; Malhotra, B. D.; Saha, Shibu; Sreenivas, K.; Gupta, Vinay

2007-01-01

Cholesterol oxidase (ChOx) has been immobilized onto zinc oxide (ZnO) nanoporous thin films grown on gold surface. A preferred c-axis oriented ZnO thin film with porous surface morphology has been fabricated by rf sputtering under high pressure. Optical studies and cyclic voltammetric measurements show that the ChOx/ZnO/Au bioelectrode is sensitive to the detection of cholesterol in 25-400 mg/dl range. A relatively low value of enzyme's kinetic parameter (Michaelis-Menten constant) ∼2.1 mM indicates enhanced enzyme affinity of ChOx to cholesterol. The observed results show promising application of nanoporous ZnO thin film for biosensing application without any functionalization

Preparation of glasses and glass ceramics of heavy metal oxides containing silver: optical, structural and electrochemical properties; Preparacao de vidros e vitroceramicas de oxidos de metais pesados contendo prata: propriedades opticas, estruturais e eletroquimicas

Energy Technology Data Exchange (ETDEWEB)

Bregadiolli, Bruna A. [Departamento de Fisica, Faculdade de Ciencias, Universidade Estadual Paulista, Bauru - SP (Brazil); Souza, Ernesto R.; Sigoli, Fernando A. [Instituto de Quimica, Universidade Estadual de Campinas, Campinas - SP (Brazil); Caiut, Jose M.A. [Departamento de Quimica, Faculdade de Filosofia Ciencias e Letras de Ribeirao Preto, Universidade de Sao Paulo, Ribeirao Preto - SP (Brazil); Alencar, Monica A.S.; Benedetti, Assis V. [Instituto de Quimica, Universidade Estadual Paulista, Araraquara - SP (Brazil); Nalin, Marcelo, E-mail: mnalin@ufscar.br [Departamento de Quimica, Universidade Federal de Sao Carlos, SP, (Brazil)

2012-07-01

Silver containing heavy metal oxide glasses and glass ceramics of the system WO{sub 3}-SbPO{sub 4} -PbO-AgCl with different AgCl contents have been prepared and their thermal, structural and optical properties characterized. Glass ceramics containing metallic silver nanoparticles have been prepared by annealing glass samples at temperatures above the glass transition and analyzed by transmission electron microscopy and energy dispersive X-ray microanalysis. The presence of the metallic clusters has been also confirmed by the observation of a surface plasmon resonance band in the visible range. Cyclic voltammetric measurements indicated the presence of metallic silver into the glasses, even before to perform the thermal treatment. (author)

South African Journal of Chemistry - Vol 54 (2001)

African Journals Online (AJOL)

Determination of Phthalate Esters in the Aquatic Environment · EMAIL FREE FULL TEXT EMAIL FREE FULL TEXT ... Chemical Speciation of Chromium in Various Matrices in South African Terrestrial Water Using an Optimised Adsorptive Stripping Voltammetric Procedure · EMAIL FREE FULL TEXT EMAIL FREE FULL ...

Electrochemical behaviour of alkaline copper complexes

Indian Academy of Sciences (India)

Abstract. A search for non-cyanide plating baths for copper resulted in the development of alkaline copper complex baths containing trisodium citrate [TSC] and triethanolamine [TEA]. Voltammetric studies were carried out on platinum to understand the electrochemical behaviour of these complexes. In TSC solutions, the.

Improvement in the assessment of direct and facilitated ion transfers by electrochemically induced redox transformations of common molecular probes

DEFF Research Database (Denmark)

Zhou, Min; Gan, Shiyu; Zhong, Lijie

2012-01-01

A new strategy based on a thick organic film modified electrode allowed us, for the first time, to explore the voltammetric processes for a series of hydrophilic ions by electrochemically induced redox transformations of common molecular probes. During the limited time available for voltammetry, ...

Dynamic Structures of DNA Heptamers with Different Central Trinucleotide Sequences Studied by Electrochemical and Spectral Methods

Czech Academy of Sciences Publication Activity Database

Pilarová, I.; Kejnovská, Iva; Vorlíčková, Michaela; Trnková, L.

2014-01-01

Roč. 26, č. 10 (2014), s. 2118-2128 ISSN 1040-0397 R&D Projects: GA ČR(CZ) GAP205/12/0466 Institutional support: RVO:68081707 Keywords : DNA heptamers * Voltammetry * Elimination voltammetric procedure Subject RIV: BO - Biophysics Impact factor: 2.138, year: 2014

Enhancement of catalytic activity of platinum-based nanoparticles towards electrooxidation of ethanol through interfacial modification with heteropolymolybdates

Energy Technology Data Exchange (ETDEWEB)

Barczuk, Piotr J.; Lewera, Adam; Miecznikowski, Krzysztof; Zurowski, Artur; Kulesza, Pawel J. [Department of Chemistry, University of Warsaw, Pasteura 1, PL-02-093 Warsaw (Poland)

2010-05-01

As evidenced from the increase of electrocatalytic currents measured under voltammetric and chronoamperometric conditions, the activity of bimetallic Pt-Ru and Pt-Sn nanoparticles towards oxidation of ethanol is increased by modification of their surfaces with ultra-thin films of phosphododecamolybdic acid (H{sub 3}PMo{sub 12}O{sub 40}). The enhancement effect has been most pronounced in a case of heteropolymolybdate-modified carbon-supported Pt-Sn catalysts. Independent high-resolution XPS measurements indicate the ability of heteropolymolybdates to stabilize tin (in bimetallic Pt-Sn particles) at higher oxidation states (presumably as tin oxo species). The overall activation effect may also be ascribed to changes in the morphology of catalytic films following modification with heteropolymolybdates. Presence of the polyoxometallate is also likely to increase of the interfacial population of reactive oxo groups in the vicinity of platinum centers. (author)

Enhancement of catalytic activity of platinum-based nanoparticles towards electrooxidation of ethanol through interfacial modification with heteropolymolybdates

Science.gov (United States)

Barczuk, Piotr J.; Lewera, Adam; Miecznikowski, Krzysztof; Zurowski, Artur; Kulesza, Pawel J.

As evidenced from the increase of electrocatalytic currents measured under voltammetric and chronoamperometric conditions, the activity of bimetallic Pt-Ru and Pt-Sn nanoparticles towards oxidation of ethanol is increased by modification of their surfaces with ultra-thin films of phosphododecamolybdic acid (H 3PMo 12O 40). The enhancement effect has been most pronounced in a case of heteropolymolybdate-modified carbon-supported Pt-Sn catalysts. Independent high-resolution XPS measurements indicate the ability of heteropolymolybdates to stabilize tin (in bimetallic Pt-Sn particles) at higher oxidation states (presumably as tin oxo species). The overall activation effect may also be ascribed to changes in the morphology of catalytic films following modification with heteropolymolybdates. Presence of the polyoxometallate is also likely to increase of the interfacial population of reactive oxo groups in the vicinity of platinum centers.

Synthesis, characterization and performance of CoxNi1−xS compounds for application in lithium batteries

Directory of Open Access Journals (Sweden)

Atef Y. Shenouda

2017-06-01

Full Text Available This study reports a process to prepare CoxNi1−xS (x = 0, 0.25, 0.5, 0.75 and 1 samples by hydrothermal process at 250 °C using stoichiometric weight ratios of raw materials. The prepared powder samples were annealed in Ar atmosphere at 450 °C for 3 h. The crystal structure of prepared annealed CoxNi1−xS samples was characterized by XRD. SEM investigations were carried out explaining the morphology of these samples. Electrochemical impedance spectra (EIS measurements, Cyclic voltammetric (CV and galvanostatic measurements were carried out. The life cycle performance was carried out for the cells and Li/Co0.25Ni0.75S cell gave specific discharge capacities of about 330 mA h g−1.

Electrochemically fabricated polyaniline nanowire-modified electrode for voltammetric detection of DNA hybridization

International Nuclear Information System (INIS)

Zhu Ningning; Chang Zhu; He Pingang; Fang Yuzhi

2006-01-01

A novel and sensitive electrochemical DNA biosensor based on electrochemically fabricated polyaniline nanowire and methylene blue for DNA hybridization detection is presented. Nanowires of conducting polymers were directly synthesized through a three-step electrochemical deposition procedure in an aniline-containing electrolyte solution, by using the glassy carbon electrode (GCE) as the working electrode. The morphology of the polyaniline films was examined using a field emission scanning electron microscope (SEM). The diameters of the nanowires range from 80 to 100 nm. The polyaniline nanowires-coated electrode exhibited very good electrochemical conductivity. Oligonucleotides with phosphate groups at the 5' end were covalently linked onto the amino groups of polyaniline nanowires on the electrode. The hybridization events were monitored with differential pulse voltammetry (DPV) measurement using methylene blue (MB) as an indicator. The approach described here can effectively discriminate complementary from non-complementary DNA sequence, with a detection limit of 1.0 x 10 -12 mol l -1 of complementary target, suggesting that the polyaniline nanowires hold great promises for sensitive electrochemical biosensor applications

Recent progress in electrochemical sensors and assays for DNA damage and repair

Czech Academy of Sciences Publication Activity Database

Fojta, Miroslav; Daňhel, Aleš; Havran, Luděk; Vyskočil, V.

2016-01-01

Roč. 79, MAY2016 (2016), s. 160-167 ISSN 0165-9936 R&D Projects: GA ČR GBP206/12/G151 Institutional support: RVO:68081707 Keywords : in-situ evaluation * carbon-paste electrode * voltammetric detection Subject RIV: BO - Biophysics Impact factor: 8.442, year: 2016

Journal of Chemical Sciences | Indian Academy of Sciences

Indian Academy of Sciences (India)

Voltammetric sensor for D-penicillamine determination based on its electrocatalytic oxidation at the surface of ferrocenes modified carbon paste electrodes · Jahan-Bakhsh Raoof Reza Ojani Fereshteh Chekin · More Details Abstract Fulltext PDF. Electrocatalytic oxidation of D-penicillamine (D-PA) at the surface of ferrocene ...

Electrokinetic and impedimetric dynamics of FeCo-nanoparticles on glassy carbon electrode

CSIR Research Space (South Africa)

Ikpo, CO

2013-01-01

Full Text Available voltammetric experiments revealed a diffusion-controlled electron transfer process on the GCE/FeCo electrode surface. Further interrogation on the electrochemical properties of the FeCo nanoelectrode in an oxygen saturated 1 M LiClO4 containing 1:1 v/v ethylene...

Journal of Chemical Sciences | Indian Academy of Sciences

Indian Academy of Sciences (India)

The complex bis (carbo/thiocabohydrazide) Zn(II) chloride was also subjected to voltammetric analysis in order to understand the reactivity both in free and metal bound states. The reaction conditions were optimized for the determination of above compounds in micrograms quantities by differential pulse voltammetry, ...

APPLICATION OF ο-TOLIDINE AS SUBSTRATE FOR THE ...

African Journals Online (AJOL)

tolidine (OT) with H2O2. The oxidative product of OT with H2O2 was an azo substrate, which was electroactive and had a sensitive linear sweep voltammetric reductive peak at -0.52 V (vs. SCE) on hanging mercury drop working electrode ...

Simultaneous electrochemical detection of dopamine and uric acid over ceria supported three dimensional gold nanoclusters

Science.gov (United States)

Palanisamy, Sivakumar

2014-12-01

CeO2 is well known for being an active material to support the growth of Au nanoclusters (Au NCs). In this work, three dimensional (3D) Au NCs were deposited on three different shaped CeO2 nanostructures such as nanoparticles (NPs), nanorod arrays (NRAs) and nanoflowers (NFs) modified Ti substrate for electrochemical simultaneous detection of dopamine (DA) and uric acid (UA). The electrodeposition of 3D Au NCs were carried out via cyclic voltammetric (CV) method at over-potential, while CeO2 nanostructures were deposited by galvanostatic constant current method under the optimized conditions. The morphology and elemental composition analysis of 3D Au NCs with CeO2 nanostructures were characterized by SEM, XRD, XPS and EDAX measurements. The electrocatalytic activity of 3D Au NCs on different CeO2 supports were thoroughly investigated by using voltammetric and amperometric techniques. According to the obtained results, CeO2 NPs supported 3D Au NCs (3D Au NCs@CeO2 NPs) displayed strong signal for DA as compared to that of CeO2 NRAs (3D Au NCs@CeO2 NRAs) and CeO2 NFs supported 3D Au NCs (3D Au NCs@CeO2 NFs). In addition, the 3D Au NCs@CeO2 NPs electrode resulted in more sensitive and simultaneous detection of DA in the presence of excess UA. Thus, the 3D Au NCs@CeO2 NPs electrode can practically be applied for the detection of DA using biological samples.

Molecularly imprinted photo-sensitive polyglutamic acid nanoparticles for electrochemical sensing of hemoglobin

International Nuclear Information System (INIS)

Zhang, Rongli; Xu, Sheng; Luo, Jing; Liu, Xiaoya

2015-01-01

A voltammetric sensor for hemoglobin (Hb) was prepared from molecularly imprinted polymer nanoparticles (MINPs) via electrophoretic deposition. A photo-sensitive copolymer composed of poly-γ-glutamic grafted with the fluorophore 7-amino-4-methylcoumarin was converted into nanoparticles that were imprinted with Hb. The resultant MINPs were then placed on a glassy carbon electrode (GCE) via electrophoretic deposition. Subsequent photo-crosslinking locks the recognition sites. The template was removed by extraction with a mixture of acetic acid and methanol at a ratio of 1:9 (v:v) to obtain a voltammetric sensor for Hb. The current response of the sensor at a working voltage of −260 mV is linearly related to the concentration of Hb in the range from 5 to 100 μg mL −1 , and recoveries range from 98.7 to 102.3 %. Compared to the respective non-imprinted nanoparticles, the sensor displays high recognition capability and affinity for Hb. (author)

Selective electrochemical detection of dopamine in a microfluidic channel on carbon nanoparticulate electrodes.

Science.gov (United States)

Rozniecka, Ewa; Jonsson-Niedziolka, Martin; Celebanska, Anna; Niedziolka-Jonsson, Joanna; Opallo, Marcin

2014-06-07

There is a continuous need for the construction of detection systems in microfluidic devices. In particular, electrochemical detection allows the separation of signals from the analyte and interfering substances in the potential domain. Here, a simple microfluidic device for the sensitive and selective determination of dopamine in the presence of interfering substances was constructed and tested. It employs a carbon nanoparticulate electrode allowing the separation of voltammetric signals of dopamine and common interfering substances (ascorbic acid and acetaminophen) both in quiescent conditions and in flow due to the electrocatalytic effect. These voltammograms were also successfully simulated. The limit of detection of dopamine detected by square wave voltammetry in 1 mM solutions of interfering substances in phosphate buffered saline is about 100 nM. In human serum a clear voltammetric signal could be seen for a 200 nM solution, sufficient to detect dopamine in the cerebral fluid. Flow injection analysis allows a decrease in the limit of detection down to 3.5 nM.

Nanomolar detection of methylparaben by a cost-effective hemoglobin-based biosensor.

Science.gov (United States)

Hajian, A; Ghodsi, J; Afraz, A; Yurchenko, O; Urban, G

2016-12-01

This work describes the development of a new biosensor for methylparaben determination using electrocatalytic properties of hemoglobin in the presence of hydrogen peroxide. The voltammetric oxidation of methylparaben by the proposed biosensor in phosphate buffer (pH=7.0), a physiological pH, was studied and it was confirmed that methylparaben undergoes a one electron-one proton reaction in a diffusion-controlled process. The biosensor was fabricated by carbon paste electrode modified with hemoglobin and multiwalled carbon nanotube. Based on the excellent electrochemical properties of the modified electrode, a sensitive voltammetric method was used for determination of methylparaben within a linear range from 0.1 to 13μmolL(-1) and detection limit of 25nmolL(-1). The developed biosensor possessed accurate and rapid response to methylparaben and showed good sensitivity, stability, and repeatability. Finally, the applicability of the proposed biosensor was verified by methylparaben evaluation in various real samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Flavonoid-surfactant interactions: A detailed physicochemical study

Science.gov (United States)

Singh, Onkar; Kaur, Rajwinder; Mahajan, Rakesh Kumar

2017-01-01

The aim of this article is to study the interactions between flavonoids and surfactants with attention of finding the probable location of flavonoids in micellar media that can be used for controlling their antioxidant behavior. In present study, the micellar and interfacial behavior of twin tailed anionic surfactants viz. sodium bis(2-ethylhexyl)sulfosuccinate (AOT) and sodium bis(2-ethylhexyl)phosphate (NaDEHP) in the presence of two flavonoids, namely quercetin (QUE) and kaempferol (KFL) have been studied by surface tension measurements. UV-visible, fluorescence and differential pulse voltammetric (DPV) measurements have been employed to predict the probable location of flavonoids (QUE/KFL) within surfactant (AOT/NaDEHP) aggregates. Dynamic light scattering (DLS) measurements further confirmed the solubilization of QUE/KFL in AOT/NaDEHP aggregates deduced from increased hydrodynamic diameter (Dh) of aggregates in the presence of flavonoids. Both radical scavenging activity (RSA) and degradation rate constant (k) of flavonoids are found to be higher in NaDEHP micelles as compared to AOT micelles.

Voltammetric and chronopotentiometric protein structure-sensitive analysis

Czech Academy of Sciences Publication Activity Database

Černocká, Hana; Paleček, Emil

2017-01-01

Roč. 224, JAN2017 (2017), s. 211-219 ISSN 0013-4686 R&D Projects: GA ČR(CZ) GA15-15479S Institutional support: RVO:68081707 Keywords : circular-dichroism spectroscopy * catalytic hydrogen evolution * mercury-electrodes Subject RIV: BO - Biophysics Impact factor: 4.798, year: 2016

Voltammetric Determination of Thiodiglycolic Acid in Urine

Czech Academy of Sciences Publication Activity Database

Dlasková, Z.; Navrátil, Tomáš; Heyrovský, Michael; Pelclová, D.; Novotný, Ladislav

2003-01-01

Roč. 375, - (2003), s. 164-168 ISSN 1618-2642 Institutional research plan: CEZ:AV0Z4040901 Keywords : urine * thioglycolic acid * voltammetry Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 1.715, year: 2003

Voltammetric Determination of a Benzimidazole Anthelmintic Mixture ...

African Journals Online (AJOL)

2002-10-17

Oct 17, 2002 ... Electrochemistry, square-wave voltammetry, benzimidazole anthelmintics, ... potential application, cathodic reduction/anodic oxidation, the type of the electrode ... benzimidazole anthelmintic in 10 cm3 of methanol-formic acid.

SQUARE WAVE VOLTAMMETRIC DETERMINATION OF LEAD IN ...

African Journals Online (AJOL)

2011-12-31

Dec 31, 2011 ... contamination of several kohl samples purchased from Algeria retail ... [7,8], atomic emission spectrometry [9] high performance liquid chromatography [10], inductively coupled plasma-mass ..... Metal Ions in Water and Food by Microcolumn High-Performance Liquid ... Applications, Kluwer, Dordrecht, 139.

Journal of Chemical Sciences | Indian Academy of Sciences

Indian Academy of Sciences (India)

propanol in 0.5 M H2SO4 were investigated with Pt and PtRu electrodes. Tafel slope and apparent activation energy were evaluated from the cyclic voltammetric data in the low potential region (0.3-0.5 V vs SHE). The CV results provided Tafel ...

Methanol oxidation on stepped Pt[n(111) x (110)] electrodes: a chronoamperometric study

NARCIS (Netherlands)

Housmans, T.H.M.; Koper, M.T.M.

2003-01-01

The methanol oxidation reaction has been studied on Pt[n(111) × (110)]-type electrodes in a 0.5 M sulfuric acid and 0.025 M methanol solution, using cyclic voltammetry and chronoamperometry. The voltammetric behavior of methanol on the three electrodes under investigation [Pt(111), Pt(554), and

Theoretical Analysis of the Relative Significance of Thermodynamic and Kinetic Dispersion in the dc and ac Voltammetry of Surface-Confined Molecules

KAUST Repository

Morris, Graham P.; Baker, Ruth E.; Gillow, Kathryn; Davis, Jason J.; Gavaghan, David J.; Bond, Alan M.

2015-01-01

© 2015 American Chemical Society. Commonly, significant discrepancies are reported in theoretical and experimental comparisons of dc voltammograms derived from a monolayer or close to monolayer coverage of redox-active surface-confined molecules. For example, broader-than-predicted voltammetric wave shapes are attributed to the thermodynamic or kinetic dispersion derived from distributions in reversible potentials (E⁰) and electrode kinetics (k⁰), respectively. The recent availability of experimentally estimated distributions of E⁰ and k⁰ values derived from the analysis of data for small numbers of surface-confined modified azurin metalloprotein molecules now allows more realistic modeling to be undertaken, assuming the same distributions apply under conditions of high surface coverage relevant to voltammetric experiments. In this work, modeling based on conventional and stochastic kinetic theory is considered, and the computationally far more efficient conventional model is shown to be equivalent to the stochastic one when large numbers of molecules are present. Perhaps unexpectedly, when experimentally determined distributions of E⁰ and k⁰ are input into the model, thermodynamic dispersion is found to be unimportant and only kinetic dispersion contributes significantly to the broadening of dc voltammograms. Simulations of ac voltammetric experiments lead to the conclusion that the ac method, particularly when the analysis of kinetically very sensitive higher-order harmonics is undertaken, are far more sensitive to kinetic dispersion than the dc method. ac methods are therefore concluded to provide a potentially superior strategy for addressing the inverse problem of determining the k⁰ distribution that could give rise to the apparent anomalies in surface-confined voltammetry.

Theoretical Analysis of the Relative Significance of Thermodynamic and Kinetic Dispersion in the dc and ac Voltammetry of Surface-Confined Molecules

KAUST Repository

Morris, Graham P.

2015-05-05

© 2015 American Chemical Society. Commonly, significant discrepancies are reported in theoretical and experimental comparisons of dc voltammograms derived from a monolayer or close to monolayer coverage of redox-active surface-confined molecules. For example, broader-than-predicted voltammetric wave shapes are attributed to the thermodynamic or kinetic dispersion derived from distributions in reversible potentials (E⁰) and electrode kinetics (k⁰), respectively. The recent availability of experimentally estimated distributions of E⁰ and k⁰ values derived from the analysis of data for small numbers of surface-confined modified azurin metalloprotein molecules now allows more realistic modeling to be undertaken, assuming the same distributions apply under conditions of high surface coverage relevant to voltammetric experiments. In this work, modeling based on conventional and stochastic kinetic theory is considered, and the computationally far more efficient conventional model is shown to be equivalent to the stochastic one when large numbers of molecules are present. Perhaps unexpectedly, when experimentally determined distributions of E⁰ and k⁰ are input into the model, thermodynamic dispersion is found to be unimportant and only kinetic dispersion contributes significantly to the broadening of dc voltammograms. Simulations of ac voltammetric experiments lead to the conclusion that the ac method, particularly when the analysis of kinetically very sensitive higher-order harmonics is undertaken, are far more sensitive to kinetic dispersion than the dc method. ac methods are therefore concluded to provide a potentially superior strategy for addressing the inverse problem of determining the k⁰ distribution that could give rise to the apparent anomalies in surface-confined voltammetry.

Electrochemical/chemical oxidation of bisphenol A in a four-electron/two-proton process in aprotic organic solvents

International Nuclear Information System (INIS)

Chan, Ya Yun; Yue, Yanni; Li, Yongxin; Webster, Richard D.

2013-01-01

Graphical abstract: - Highlights: • Bisphenol A undergoes a chemically irreversible voltammetric oxidation process. • Chemical oxidation was performed to overcome adsorption effects that cause electrode fouling. • A new product was isolated from chemical oxidation with 4 mol equiv. of the one-electron oxidant, NO + . • The oxidative mechanism was proposed to be a four-electron/two-proton process. - Abstract: The electrochemical behavior of bisphenol A (BPA) was examined using cyclic voltammetry, bulk electrolysis and chemical oxidation in aprotic organic solvents. It was found that BPA undergoes a chemically irreversible voltammetric oxidation process to form compounds that cannot be electrochemically converted back to the starting materials on the voltammetric timescale. To overcome the effects of electrode fouling during controlled potential electrolysis experiments, NO + was used as a one-electron chemical oxidant. A new product, hydroxylated bisdienone was isolated from the chemical oxidation of BPA with 4 mol equiv of NO + SbF 6 − in low water content CH 3 CN. The structure of the cation intermediate species was deduced and it was proposed that BPA is oxidized in a four-electron/two-proton process to form a relatively unstable dication which reacts quickly in the presence of water in acetonitrile (in a mechanism that is similar to phenols in general). However, as the water content of the solvent increased it was found that the chemical oxidation mechanism produced a nitration product in high yield. The findings from this study provide useful insights into the reactions that can occur during oxidative metabolism of BPA and highlight the possibility of the role of a bisdienone cation as a reactive metabolite in biological systems

Porphyrin–anthraquinone dyads: Synthesis, spectroscopy and ...

Indian Academy of Sciences (India)

Unknown

and characterized by mass (FAB), IR, UV–visible, 1H NMR and ESR spectroscopic techniques and also by cyclic and differential pulse voltammetric methods. Analysis of the data reveals that the spectral and electrochemical properties of the individual chromophoric entities are retained and that there is no specific π–.

Immunoassays of chemically modified polysaccharides, glycans in glycoproteins and ribose in nucleic acids

Czech Academy of Sciences Publication Activity Database

Strmečki, S.; Trefulka, Mojmír; Zatloukalová, P.; Durech, M.; Vojtěšek, B.; Paleček, Emil

2017-01-01

Roč. 955, FEB2017 (2017), s. 108-115 ISSN 0003-2670 R&D Projects: GA ČR(CZ) GA15-15479S Institutional support: RVO:68081707 Keywords : structural-characterization * voltammetric determination * electrochemical detection Subject RIV: CB - Analytical Chemistry, Separation OBOR OECD: Analytical chemistry Impact factor: 4.950, year: 2016

Carboxylated dithiafulvenes and tetrathiafulvalene vinylogues: synthesis, electronic properties, and complexation with zinc ions

Directory of Open Access Journals (Sweden)

Yunfei Wang

2015-06-01

Full Text Available A class of carboxyl and carboxylate ester-substituted dithiafulvene (DTF derivatives and tetrathiafulvalene vinylogues (TTFVs has been synthesized and their electronic and electrochemical redox properties were characterized by UV–vis spectroscopic and cyclic voltammetric analyses. The carboxyl-TTFV was applied as a redox-active ligand to complex with Zn(II ions, forming a stable Zn-TTFV coordination polymer. The structural, electrochemical, and thermal properties of the coordination polymer were investigated by infrared spectroscopy, cyclic voltammetry, powder X-ray diffraction, and differential scanning calorimetric analyses. Furthermore, the microscopic porosity and surface area of the Zn-TTFV coordination polymer were measured by nitrogen gas adsorption analysis, showing a BET surface of 148.2 m2 g−1 and an average pore diameter of 10.2 nm.

Structural and cyclic volta metric investigations on BIPBVOX solid electrolyte synthesized by ethylene glycol–citric acid sol–gel route

Energy Technology Data Exchange (ETDEWEB)

Naqvi, Faria K.; Beg, Saba, E-mail: profsababeg@gmail.com [Solid-State Chemistry Lab, Physical Chemistry Division, Department of Chemistry, Aligarh Muslim University, Aligarh, 202002 INDIA (India); Al-Areqi, Niyazi A. S. [Department of Chemistry, Faculty of Applied Science, Taiz University, Taiz, Republic of Yemen (Yemen)

2016-05-06

Samples of BIPBVOX.x (Bi{sub 2}V{sub 1–x}Pb{sub x}O{sub 5.5–x/2}) in the composition range 0.05 ≤ x ≤ 0.20 were prepared by ethylene glycol– citric acid sol–gel synthesis route. Structural investigations were carried out by X–ray diffraction, DTA. The highly conducting γ′– phase was effectively stabilized at room temperature for compositions with x ≥ 0.17. Cyclic voltammetric measurements showed reversible redox reactions of vanadium and irreversible redox reaction of Bi{sup 3+} in the BIPBVOX system during the first cathodic and anodic sweep. However, a higher stability against the reduction of Bi{sup 3+} to metallic bismuth was seen for x=0.20.

Brain Tissue Oxygen: In Vivo Monitoring with Carbon Paste Electrodes

Directory of Open Access Journals (Sweden)

John P. Lowry

2005-11-01

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

Influence of silver on the anodic corrosion and gas evolution of Pb-Sb-As-Se alloys as positive grids in lead acid batteries

International Nuclear Information System (INIS)

Tizpar, A.; Ghasemi, Z.

2006-01-01

The influence of silver addition in the range 0.01-0.09 wt.% on the anodic corrosion and gas evolution of Pb-Sb-As-Se alloy in 1.28 sp.gr. H 2 SO 4 solution at 25 deg. C was studied using linear sweep voltammetry, cyclic voltammetry, weight loss measurements and scanning electron microscopy. The results drawn from different techniques are comparable. The effect of different concentration of silver on the corrosion behavior of Pb-Sb-As-Se was investigated. The experimental results show that the silver added to Pb-Sb-As-Se alloy inhibits the growth of anodic corrosion layer. A decrease in the oxygen evolution overpotential and an increase in the hydrogen evolution overpotential with the addition of Ag were also observed during the experiments. Cyclic voltammetric measurements provided information on the effect of Ag on the oxidation of PbSO 4 to PbO 2

Journal of Chemical Sciences | Indian Academy of Sciences

Indian Academy of Sciences (India)

Cupronickels offer enhanced corrosion protection in marine environments by the formation of passive films on the surface. Cyclic voltammetric studies were carried on cupronickels in chloride solutions at H 6.3 to understand the role of chloride ions in passive film formation. Increase in nickel content of the alloy and of ...

Electrochemical behavior of boron in LiF-NaF-KF- melts

DEFF Research Database (Denmark)

Polyakova, L.P.; Bukatova, G.A.; Polyakova, E.G.

1996-01-01

The electrochemical reduction of B(III) to B(0) in KBF4-LiF-NaF-KF melts has been studied by voltammetric and chronopotentiometric methods, Glassy carbon, Pt, and Ag were used as working electrode materials. Only in the case of Ag was the reduction not complicated by interaction between boron...

Journal of Fundamental and Applied Sciences - Vol 3, No 2 (2011)

African Journals Online (AJOL)

Square wave voltammetric determination of lead in commercial kohl using a glassy carbon electrode · EMAIL FREE FULL TEXT EMAIL FREE FULL TEXT DOWNLOAD FULL TEXT DOWNLOAD FULL TEXT. MA Saha, M Alia, A Rebiai, T Lanez, 155-164. http://dx.doi.org/10.4314/jfas.v3i2.4 ...

Journal of Chemical Sciences | Indian Academy of Sciences

Indian Academy of Sciences (India)

Electrochemical behaviour of platinum at polymer-modified glassy carbon electrodes · Carmem L P S Zanta C A Martínez-Huitle · More Details Abstract Fulltext PDF. In this paper, the preparations and voltammetric characteristics of chitosan-modified glassy carbon (Ct-MGC) and platinum electrodes are studied. Ct-MGC can ...

Study of colored anodized aluminum with calcon in sulfuric acidic solution using cyclic voltammetry and impedance measurement methods

Energy Technology Data Exchange (ETDEWEB)

Norouzi, P.; Ganjali, M.R.; Golmohamaddi, M.; Mousavi, S. [Department of Chemistry, Faculty of Science, University of Tehran, Tehran (Iran); Vatankhah, G. [Iranian Organization for Science and Technology (IROST), Isfahan Center, A5 Ghezelbash Avenue, Tohid Street, Isfahan 8173954541 (Iran)

2003-04-01

The effect of coloring condition of Al with Calcon (sodium 2,2'-dihydroxy-azonaphthalene-4-sulfonate), on the corrosion resistance of Al in 0.1 M sulfuric acid solution was studied, using cyclic voltammetry and measurement of impedance noise methods. The changes in the corrosion resistance of colored aluminum electrodes were evaluated by measuring the magnitude of impedance and cyclic voltammetric responses of anodized and colored electrodes. An irreversible corrosion response was observed at the cyclic voltammogram of the colored aluminum electrode. The current and threshold potential of corrosion responses strongly depends on the applied conditions during anodizing, coloring and sealing stages. In addition, significant changes in impedance at the ac voltammogram and noise level at some ac frequencies were observed, when the electrodes were colored under various conditions. In this regard, the surface of the electrode was studied by Scanning Electron Microscopy (SEM). Comparison of SEM images of the colored and uncolored aluminum specimens showed that the colored surface contained a significant numbers of pits. The results indicated that coloring aluminum with Calcon could reduce corrosion resistance of aluminum and increase roughness of the oxide film. (Abstract Copyright [2003], Wiley Periodicals, Inc.) [German] Mit Hilfe zyklischer Voltammetrie und Messungen mit Impedanzrauschmethoden wurde der Einfluss der Faerbungsbedingungen von Aluminium mit Calcon (Natrium 2,2'-Dihydroxyazonaphthalen-4-Sulfonat) auf den Korrosionswiderstand von Aluminium in 0,1 M Schwefelsaeure untersucht. Die Veraenderungen des Korrosionswiderstandes von gefaerbten Aluminiumelektroden wurden durch Messungen der Hoehe der Impedanzreaktion bzw. der Reaktion bei der zyklischen Voltammetrie von anodisierten und gefaerbten Elektroden beurteilt. Eine irreversible Korrosionsreaktion wurde beim zyklischen Voltammogramm der gefaerbten Aluminiumelektrode beobachtet. Der Strom und das

A novel tin-bismuth alloy electrode for anodic stripping voltammetric determination of zinc

International Nuclear Information System (INIS)

Pan, D.; Yin, T.; Qin, W.; Zhang, L.; Zhuang, J.

2012-01-01

We report on a novel tin-bismuth alloy electrode (SnBiE) for the determination of trace concentrations of zinc ions by square-wave anodic stripping voltammetry without deoxygenation. The SnBiE has the advantages of easy fabrication and low cost, and does not require a pre-treatment (in terms of modification) prior to measurements. A study on the potential window of the electrode revealed a high hydrogen overvoltage though a limited anodic range due to the oxidation of tin. The effects of pH value, accumulation potential, and accumulation time were optimized with respect to the determination of trace zinc(II) at pH 5. 0. The response of the SnBiE to zinc(II) ion is linear in the 0.5-25 μM concentration range. The detection limit is 50 nM (after 60 s of accumulation). The SnBiE was applied to the determination of zinc(II) in wines and honeys, and the results were consistent with those of AAS. (author)

Electrochemistry of cations in diopsidic melt - Determining diffusion rates and redox potentials from voltammetric curves

Science.gov (United States)

Colson, Russell O.; Haskin, Larry A.; Crane, Daniel

1990-01-01

Results are presented on determinations of reduction potentials and their temperature dependence of selected ions in diopsidic melt, by using linear sweep voltammetry. Diffusion coefficients were measured for cations of Eu, Mn, Cr, and In. Enthalpies and entropies of reduction were determined for the cations V(V), Cr(3+), Mn(2+), Mn(3+), Fe(2+), Cu(2+), Mo(VI), Sn(IV), and Eu(3+). Reduction potentials were used to study the structural state of cations in the melt.

physico-chemical studies on DNA-drugs interaction and their analytical applications

International Nuclear Information System (INIS)

Kandil, S.A

2003-01-01

The present thesis is devoted to study the interaction of some antibacterial agents i.e. fluoroquinolones . these agents include ciprofloxacin, norfloxacin , ofloxacin , pefloxacin and levofloxacin with DNA. voltammetric and spectrophotometric methods were used to carry out this study. Also the interaction of the suggested drugs with DNA at the surface of carbon electrode by cyclic voltammetry and differential pulse techniques is examined. The work comprises three chapters: (1) includes an introduction of voltammetry , differential pulse, drug-DNA interaction and fluoroquinoline- DNA interaction and literature survey on fluoroquinolones.Chapter (II) includes preparation of the solutions and instruments which were used for the measurements using the different techniques.Chapter(III) comprises three parts; (1) deals with the interaction of fluoroquinolones (ciprofloxacin, norfloxacin, ofloxacin, pefloxacin and levofloxacin) with DNA in solution have been investigated by means of voltammetry and spectroscopy . the results show that the values of binding constant of fluoroquinolne drugs with DNA obtained through the changes of the anodic peak current, and their values are, 30900,31000,32300,32000 and 32500 M -1 respectively. or changes of absorption and values are, 36000,30200.38300,36500 and 34400 M -1 receptively.(II) includes voltammetric behavior of fluoroquinolones on DNA-modified carbon paste electrode. (III)includes analytical application for proposed method for the determination of levofloxacin as a typical example for fluoroquinolones. Concentration in the range 5.0x10 -7 ∼ 5.0x10 -6 mol/L , with a detection limit of 1.0x10 -7 mol/L. direct and simple determination of levofloxacin in urine was established with no manipulation of urine sample other than dilution 1:10

Improved Bi Film Wrapped Single Walled Carbon Nanotubes for Ultrasensitive Electrochemical Detection of Trace Cr(VI)

Science.gov (United States)

Zhou, Shilin; Xue, Zi-Ling; Xu, Lina; Gu, Yingying; Miao, Yuqing

2014-01-01

We report here the successful fabrication of an improved Bi film wrapped single walled carbon nanotubes modified glassy carbon electrode (Bi/SWNTs/GCE) as a highly sensitive platform for ultratrace Cr(VI) detection through catalytic adsorptive cathodic stripping voltammetry (AdCSV). The introduction of negatively charged SWNTs extraordinarily decreased the size of Bi particles to nanoscale due to electrostatic interaction which made Bi(III) cations easily attracted onto the surface of SWNTs in good order, leading to higher quality of Bi film deposition. The obtained Bi/SWNTs composite was well characterized with electrochemical impedance spectroscopy (EIS), scanning electron microscopy (SEM), the static water contact angle and the voltammetric measurements. The results demonstrates the improvements in the quality of Bi film deposited on the surface of SWNTs such as faster speed of electron transfer, more uniform and smoother morphology, better hydrophilicity and higher stripping signal. Using diethylene triaminepentaacetic acid (DTPA) as complexing ligand, the fabricated electrode displays a well-defined and highly sensitive peak for the reduction of Cr(III)-DTPA complex at −1.06 V (vs. Ag/AgCl) with a linear concentration range of 0–25 nM and a fairly low detection limit of 0.036 nM. No interference was found in the presence of coexisting ions, and good recoveries were achieved for the analysis of a river sample. In comparison to previous approaches using Bi film modified GCE, the newly designed electrode exhibits better reproducibility and repeatability towards aqueous detection of trace Cr(VI) and appears to be very promising as the basis of a highly sensitive and selective voltammetric procedure for Cr(VI) detection at trace level in real samples. PMID:24771881

Preparation of poly(3,4-ethylenedioxythiophene) nanofibers modified pencil graphite electrode and investigation of over-oxidation conditions for the selective and sensitive determination of uric acid in body fluids

Energy Technology Data Exchange (ETDEWEB)

Özcan, Ali, E-mail: aozcan3@anadolu.edu.tr; İlkbaş, Salih

2015-09-03

In this study, we have performed the preparation of over-oxidized poly(3,4-ethylenedioxythiophene) nanofibers modified pencil graphite electrode (Ox-PEDOT-nf/PGE) to develop a selective and sensitive voltammetric uric acid (UA) sensor. It was noted that the over-oxidation potential and time had a prominent effect on the UA response of the Ox-PEDOT-nf/PGE. Characterizations of PEDOT-nf/PGE and Ox-PEDOT-nf/PGE have been performed by cyclic voltammetry, electrochemical impedance spectroscopy, scanning electron microscopy, Fourier transform infrared spectroscopy and Raman spectroscopy. The highest voltammetric response of UA was obtained at pH 2.0. A linear relationship between the concentration of UA and oxidation peak currents was observed in the concentration range of 0.01–20.0 μM. The detection limit (1.3 nM according to S/N = 3) and reproducibility (RSD: 4.6 % for N:10) have also been determined. The effects of different substances on the determination of UA have been investigated. A very high peak separation value of 423 mV was obtained between UA and ascorbic acid which is the major interfering substance for UA. The use of Ox-PEDOT-nf/PGE has been successfully tested in the determination of UA in human blood serum and urine samples for the first time in the literature. - Highlights: • Modification of pencil graphite with over-oxidized PEDOT nanofibers was performed. • The prepared electrodes were used in the voltammetric determination of uric acid. • The over-oxidation potential and time has a prominent effect on the responses. • A very high peak separation (463 mV) was obtained between ascorbic and uric acids. • Analytical application of the electrodes was successfully tested in real samples.

Preparation of poly(3,4-ethylenedioxythiophene) nanofibers modified pencil graphite electrode and investigation of over-oxidation conditions for the selective and sensitive determination of uric acid in body fluids

International Nuclear Information System (INIS)

Özcan, Ali; İlkbaş, Salih

2015-01-01

In this study, we have performed the preparation of over-oxidized poly(3,4-ethylenedioxythiophene) nanofibers modified pencil graphite electrode (Ox-PEDOT-nf/PGE) to develop a selective and sensitive voltammetric uric acid (UA) sensor. It was noted that the over-oxidation potential and time had a prominent effect on the UA response of the Ox-PEDOT-nf/PGE. Characterizations of PEDOT-nf/PGE and Ox-PEDOT-nf/PGE have been performed by cyclic voltammetry, electrochemical impedance spectroscopy, scanning electron microscopy, Fourier transform infrared spectroscopy and Raman spectroscopy. The highest voltammetric response of UA was obtained at pH 2.0. A linear relationship between the concentration of UA and oxidation peak currents was observed in the concentration range of 0.01–20.0 μM. The detection limit (1.3 nM according to S/N = 3) and reproducibility (RSD: 4.6 % for N:10) have also been determined. The effects of different substances on the determination of UA have been investigated. A very high peak separation value of 423 mV was obtained between UA and ascorbic acid which is the major interfering substance for UA. The use of Ox-PEDOT-nf/PGE has been successfully tested in the determination of UA in human blood serum and urine samples for the first time in the literature. - Highlights: • Modification of pencil graphite with over-oxidized PEDOT nanofibers was performed. • The prepared electrodes were used in the voltammetric determination of uric acid. • The over-oxidation potential and time has a prominent effect on the responses. • A very high peak separation (463 mV) was obtained between ascorbic and uric acids. • Analytical application of the electrodes was successfully tested in real samples.

A novel composite electrode based on tungsten oxide nanoparticles and carbon nanotubes for the electrochemical determination of paracetamol

International Nuclear Information System (INIS)

Baytak, Aysegul Kutluay; Duzmen, Sehriban; Teker, Tugce; Aslanoglu, Mehmet

2015-01-01

An electrochemical sensor was prepared by the modification of a glassy carbon electrode (GCE) with a composite of nanoparticles of tungsten oxide (WO 3 ) and carbon nanotubes (CNTs) for the quantification of paracetamol (PR). Energy dispersive X-ray analysis (EDX) and scanning electron microscopy (SEM) were performed for the characterization of the nanocomposite layer. Compared with a bare GCE and a GCE modified with CNTs, the proposed electrode (WO 3 NPs/CNTs/GCE) exhibited a well-defined redox couple for PR and a marked enhancement of the current response. The experimental results also showed that ascorbic acid (AA) did not interfere with the selective determination of PR. The proposed electrode was used for the determination of PR in 0.1 M phosphate buffer solution (PBS) at pH 7.0 using square wave voltammetry (SWV). The peak current increased linearly with the concentration of PR in the range of 1.0 × 10 −9 –2.0 × 10 −7 M. The detection limit (LOD) was 5.54 × 10 −11 M (based on 3 S b /m). The proposed voltammetric sensor provided long-time stability, improved voltammetric behavior and good reproducibility for PR. The selective, accurate and precise determination of PR makes the proposed electrode of great interest for monitoring its therapeutic use. - Highlights: • A voltammetric nanosensor was prepared using nanoparticles of WO 3 and CNTs. • A selective quantification of paracetamol was carried out in the presence of AA. • A linear plot was obtained for current responses versus concentrations over the range from 1.0 × 10 −9 to 2.0 × 10 −7 M. • A detection limit of 554 pM was obtained for paracetamol using the proposed nanosensor. • An accurate quantification makes the proposed nanosensor of great interest for public health

Journal of Chemical Sciences | Indian Academy of Sciences

Indian Academy of Sciences (India)

Electrochemical reduction of hydrogen peroxide is studied on a sand-blasted stainless steel (SSS) electrode in an aqueous solution of NaClO4. The cyclic voltammetric reduction of H2O2 at low concentrations is characterized by a cathodic peak at -0.40 V versus standard calomel electrode (SCE). Cyclic voltammetry is ...

cobalt(II), nickel(II)

Indian Academy of Sciences (India)

Unknown

procedures. The supporting electrolyte, NaClO4 used in the voltammetric experiment was purchased from. Sigma. IR spectra were recorded in KBr medium on .... (13⋅6). L = Schiff base ligand form of one broad band envelope. The electronic spectra of Co(II) complex showed two spin-allowed transitions at 17856 and ...

Ferrocene-Functionalized Graphene Oxide Nanosheets: Efficient Electronic Communication between Ferrocene Centers across Graphene Nanosheets

International Nuclear Information System (INIS)

Lu, Yizhong; Jiang, Yuanyuan; Wu, Haibin; Chen, Wei

2015-01-01

Highlights: • Graphene oxide (GO) nanosheets functionalized with ferrocenyl moieties (GO-Fc) are fabricated. • GO-Fc shows efficient electronic communication between ferrocene centers. • GO-Fc exhibits two pairs of voltammetric peaks with a large potential spacing of 0.515 V. • GO-Fc shows a broad absorption peak in the near-infrared range (∼ 1428 nm) at mixed valence. - Abstract: Graphene oxide (GO) nanosheets functionalized with ferrocenyl moieties (GO-Fc) were fabricated through strong covalent C−C bonds. The resulting hybrid showed efficient electronic communication between ferrocene centers due to the strong electron delocalization facilitated by the large pi-pi conjugated structure of graphene sheets. The obtained hybrid exhibited two pairs of voltammetric peaks with a large potential spacing of 0.515 V and a broad absorption peak in the near-infrared range (∼ 1428 nm) at mixed valence. The electrochemical and near IR spectroscopic features suggested a Class II/III behavior of the intervalence charge transfer. This work indicates clearly that strong electronic coupling between ferrocene centers can be easily realized across graphene nanosheets with sp 2 -hybridized carbon

VALIDAÇÃO INTRALABORATORIAL DA DETERMINAÇÃO DE METILTESTOSTERONA EM ÁGUAS NATURAIS POR VOLTAMETRIA USANDO ELETRODO DE GOTA PENDENTE DE MERCÚRIO

Directory of Open Access Journals (Sweden)

Luciane Miranda

2015-03-01

Full Text Available 17α-methyltestosterone (17α-MT is a hormone used in medicine and aquaculture which can be found in natural waters. It is considered an emerging organic pollutant and its accurate and precise analysis is required. Therefore, this study presents the in-house validation of a new voltammetric methodology for 17α-MT analysis in natural waters. A hanging mercury drop electrode and NaOH 5.0×10-3 mol L-1 solution as the electrolyte were employed in the voltammetric determinations. To confirm the presence of 17α-MT in water samples quantitative analysis was performed by ESI-MS/MS. The methodology exhibited good selectivity, linearity, accuracy (recovery of between 100.4 and 108.8% and precision (RSDs for repeatability of 2.85% and for intermediate precision of 14.10%, with n = 5, respectively. LOD and LOQ were 3.07 µg L-1 and 10.78 µg L-1, respectively. The methodology was suitable for determination of 17α-MT in natural waters due to low-cost, good performance and no sample pre-treatment required.

Immobilization of phenylalanine-dehydrogenase on nano-sized polytaurine: a new platform for application of nano-polymeric materials on enzymatic biosensing technology.

Science.gov (United States)

Omidinia, Eskandar; Shadjou, Nasrin; Hasanzadeh, Mohammad

2014-09-01

A strategy of phenylalanine-dehydrogenase (PheDH) entrapment within the polytaurine matrix is demonstrated to probe the direct electrochemistry of phenylalanine (Pha). It was found that PheDH has been stably immobilized on glassy carbon electrode modified by polytaurine based on simple technique. Cyclic voltammetric study indicated that the oxidation process is irreversible and diffusion controlled. The number of exchanged electrons in the electro-oxidation process was obtained, and the data indicated that Pha is oxidized via one-electron steps. The results revealed that Pha promotes the rate of oxidation by increasing the peak current. The diffusion coefficient and electron-transfer coefficient of Pha were found to be 0.2×10(-6)cm(2)s(-1) and 0.467, respectively. A sensitive, simple and time-saving differential-pulse voltammetric procedure was developed for the analysis of Pha. The results show that by using the proposed method, Pha can be determined with a detection limit of 9 nM. Copyright © 2014 Elsevier B.V. All rights reserved.

Modified glassy carbon electrodes based on carbon nanostructures for ultrasensitive electrochemical determination of furazolidone.

Science.gov (United States)

Shahrokhian, Saeed; Naderi, Leila; Ghalkhani, Masoumeh

2016-04-01

The electrochemical behavior of Furazolidone (Fu) was investigated on the surface of the glassy carbon electrode modified with different carbon nanomaterials, including carbon nanotubes (CNTs), carbon nanoparticles (CNPs), nanodiamond-graphite (NDG), graphene oxide (GO), reduced graphene oxide (RGO) and RGO-CNT hybrids (various ratios) using linear sweep voltammetry (LSV). The results of voltammetric studies exhibited a considerable increase in the cathodic peak current of Fu at the RGO modified GCE, compared to other modified electrodes and also bare GCE. The surface morphology and nature of the RGO film was thoroughly characterized by scanning electron microscopy (SEM), atomic force microscopy (AFM), electrochemical impedance spectroscopy (EIS) and cyclic voltammetry (CV) techniques. The modified electrode showed two linear dynamic ranges of 0.001-2.0 μM and 2.0-10.0 μM with a detection limit of 0.3 nM for the voltammetric determination of Fu. This sensor was used successfully for Fu determination in pharmaceutical and clinical preparations. Copyright © 2016 Elsevier B.V. All rights reserved.

Development of an alcohol dehydrogenase biosensor for ethanol determination with toluidine blue O covalently attached to a cellulose acetate modified electrode.

Science.gov (United States)

Alpat, Senol; Telefoncu, Azmi

2010-01-01

In this work, a novel voltammetric ethanol biosensor was constructed using alcohol dehydrogenase (ADH). Firstly, alcohol dehydrogenase was immobilized on the surface of a glassy carbon electrode modified by cellulose acetate (CA) bonded to toluidine blue O (TBO). Secondly, the surface was covered by a glutaraldehyde/bovine serum albumin (BSA) cross-linking procedure to provide a new voltammetric sensor for the ethanol determination. In order to fabricate the biosensor, a new electrode matrix containing insoluble Toluidine Blue O (TBO) was obtained from the process, and enzyme/coenzyme was combined on the biosensor surface. The influence of various experimental conditions was examined for the characterization of the optimum analytical performance. The developed biosensor exhibited sensitive and selective determination of ethanol and showed a linear response between 1 × 10(-5) M and 4 × 10(-4) M ethanol. A detection limit calculated as three times the signal-to-noise ratio was 5.0 × 10(-6) M. At the end of the 20(th) day, the biosensor still retained 50% of its initial activity.

Development of an Alcohol Dehydrogenase Biosensor for Ethanol Determination with Toluidine Blue O Covalently Attached to a Cellulose Acetate Modified Electrode

Directory of Open Access Journals (Sweden)

Azmi Telefoncu

2010-01-01

Full Text Available In this work, a novel voltammetric ethanol biosensor was constructed using alcohol dehydrogenase (ADH. Firstly, alcohol dehydrogenase was immobilized on the surface of a glassy carbon electrode modified by cellulose acetate (CA bonded to toluidine blue O (TBO. Secondly, the surface was covered by a glutaraldehyde/bovine serum albumin (BSA cross-linking procedure to provide a new voltammetric sensor for the ethanol determination. In order to fabricate the biosensor, a new electrode matrix containing insoluble Toluidine Blue O (TBO was obtained from the process, and enzyme/coenzyme was combined on the biosensor surface. The influence of various experimental conditions was examined for the characterization of the optimum analytical performance. The developed biosensor exhibited sensitive and selective determination of ethanol and showed a linear response between 1 × 10−5 M and 4 × 10−4 M ethanol. A detection limit calculated as three times the signal-to-noise ratio was 5.0 × 10−6 M. At the end of the 20th day, the biosensor still retained 50% of its initial activity.

Determination of Mercury (II Ion on Aryl Amide-Type Podand-Modified Glassy Carbon Electrode

Directory of Open Access Journals (Sweden)

Sevgi Güney

2011-01-01

Full Text Available A new voltammetric sensor based on an aryl amide type podand, 1,8-bis(o-amidophenoxy-3,6-dioxaoctane, (AAP modified glassy carbon electrode, was described for the determination of trace level of mercury (II ion by cyclic voltammetry (CV and differential pulse voltammetry (DPV. A well-defined anodic peak corresponding to the oxidation of mercury on proposed electrode was obtained at 0.2 V versus Ag/AgCl reference electrode. The effect of experimental parameters on differential voltammetric peak currents was investigated in acetate buffer solution of pH 7.0 containing 1 × 10−1 mol L−1 NaCl. Mercury (II ion was preconcentrated at the modified electrode by forming complex with AAP under proper conditions and then reduced on the surface of the electrode. Interferences of Cu2+, Pb2+, Fe3+, Cd2+, and Zn2+ ions were also studied at two different concentration ratios with respect to mercury (II ions. The modified electrode was applied to the determination of mercury (II ions in seawater sample.

Electrochemical studies of nevirapine, an anti-HIV drug, and its assay in tablets and biological samples

Directory of Open Access Journals (Sweden)

JALDAPPAGARI SEETHARAMAPPA

2012-06-01

Full Text Available The electrochemical oxidation of nevirapine, an anti-HIV drug, at a glassy carbon electrode has been studied by voltammetric techniques. Nevirapine showed one well defined irreversible oxidation peak with a potential of 0.749 V in phosphate buffer at pH 10. The effects of different electrolytes, pH and scan rate on the electrochemical behaviour of nevira¬pine were examined to determine the optimum reaction conditions. The oxidation peak current was found to vary linearly with the concentration of nevirapine in the range of 5.0 – 350 µM. The limit of detection and limit of quantification values were calculated and found to be 1.026 µM and 3.420 µM, respectively. The low relative standard deviation values of inter-day and intra-day assays highlighted the good reproducibility of the proposed m¬ethod for assay of nevirapine. Further, a sensitive and accurate differential pulse voltammetric method was developed for the determination of nevirapine concentrations in pharma¬ceutical formulations.

Electrochemical sensor based on graphene and mesoporous TiO2 for the simultaneous determination of trace colourants in food.

Science.gov (United States)

Gan, Tian; Sun, Junyong; Meng, Wen; Song, Li; Zhang, Yuxia

2013-12-15

Currently, synthetic colourants draw much attention as food additives. This paper investigated the simultaneous electrocatalytic oxidation of sunset yellow and tartrazine, two yellow colourants commonly present in food together, with a novel voltammetric sensor based on graphene and mesoporous TiO2 modified carbon paste electrode. Due to the high accumulation effect and great catalytic capability of graphene and mesoporous TiO2, the developed sensor exhibited well-defined and separate square wave voltammetric peaks (i.e., 272 mV) for sunset yellow tartrazine. The peak currents of sunset yellow and tartrazine increased linearly with their concentration in the ranges of 0.02-2.05 μM and 0.02-1.18 μM, respectively. And the detection limit was 6.0 and 8.0 nM for sunset yellow and tartrazine, respectively. This new sensor was applied to determine sunset yellow and tartrazine in several food sample extracts. Results suggested that the proposed sensor was sensitive, rapid and reliable. Copyright © 2013 Elsevier Ltd. All rights reserved.

Determination of Zalcitabine in Medicaments by Differential Pulse Voltammetry

Directory of Open Access Journals (Sweden)

Katia Christina Leandro

2013-01-01

Full Text Available The zalcitabine (ddC has been extensively used in the treatment of HIV patients due to its antiretroviral activity. The quality control of this active principle in medications is of outstanding importance to public health. The principal objective of the current study was the development of an alternative analytical methodology for the zalcitabine determination using a voltammetric process. The zalcitabine gives a reduction peak (at -1.22 V versus Ag/AgCl at the hanging mercury drop electrode (HMDE. The differential pulse voltammetric response is evaluated with respect to the scan rate (20 mV/s, pulse amplitude (50 mV, support electrolyte (Clark-Lubs buffer, pH (2.0, and other variables. The response is linear over the 10.0 to 28.0 mg/L (47 to 133 μM concentration range, and the detection limit is 2.08 mg/L. The validation of this method was realized using a governmental Brazilian document (Inmetro, 2007 and the results are reported for medication drugs.

Growth of anodic films on compound semiconductor electrodes: InP in aqueous (NH sub 4) sub 2 S

CERN Document Server

Buckley, D N

2002-01-01

Film formation on compound semiconductors under anodic conditions is discussed. The surface properties of InP electrodes were examined following anodization in a (NH sub 4) sub 2 S electrolyte. The observation of a current peak in the cyclic voltammetric curve was attributed to selective etching of the substrate and a film formation process. AFM images of samples anodized in the sulfide solution revealed surface pitting. Thicker films formed at higher potentials exhibited extensive cracking as observed by optical and electron microscopy, and this was explicitly demonstrated to occur ex situ rather than during the electrochemical treatment. The composition of the thick film was identified as In sub 2 S sub 3 by EDX and XPS. The measured film thickness varies linearly with the charge passed, and comparison between experimental thickness measurements and theoretical estimates for the thickness indicate a porosity of over 70 %. Cracking is attributed to shrinkage during drying of the highly porous film and does n...

Simulation of square wave voltammetry of three electrode reactions coupled by two reversible chemical reactions

OpenAIRE

Lovrić, Milivoj

2017-01-01

Three fast and reversible electrode reactions that are connected by two reversible chemical reactions that are permanently in the equilibrium are analysed theoretically for square wave voltammetry. The dependence of peak potentials on the dimensionless equilibrium constants of chemical reactions is calculated. The influence of the basic thermodynamic parameters on the square wave voltammetric responses is analysed.

A cell for the controllable thermal treatment and electrochemical characterisation of single crystal alloy electrodes

DEFF Research Database (Denmark)

Bondarenko, Alexander S.; Stephens, Ifan E.L.; Chorkendorff, Ib

2012-01-01

be performed in this cell. These include preparation and basic voltammetric characterisation of Cu/Pt(111) near-surface and surface alloys where monolayer amounts of Cu are located in the 1st and 2nd layers, respectively. The cell can also be useful for “electrochemical atomic layer epitaxy” to assemble...... multilayers using repetitive underpotential deposition....

Poly(brilliant green) and poly(thionine) modified carbon nanotube coated carbon film electrodes for glucose and uric acid biosensors.

Science.gov (United States)

Ghica, M Emilia; Brett, Christopher M A

2014-12-01

Poly(brilliant green) (PBG) and poly(thionine) (PTH) films have been formed on carbon film electrodes (CFEs) modified with carbon nanotubes (CNT) by electropolymerisation using potential cycling. Voltammetric and electrochemical impedance characterisation were performed. Glucose oxidase and uricase, as model enzymes, were immobilised on top of PBG/CNT/CFE and PTH/CNT/CFE for glucose and uric acid (UA) biosensing. Amperometric determination of glucose and UA was carried out in phosphate buffer pH 7.0 at -0.20 and +0.30 V vs. SCE, respectively, and the results were compared with other similarly modified electrodes existing in the literature. An interference study and recovery measurements in natural samples were successfully performed, indicating these architectures to be good and promising biosensor platforms. Copyright © 2014 Elsevier B.V. All rights reserved.

Single molecular switch based on thiol tethered iron(II)clathrochelate on gold

Energy Technology Data Exchange (ETDEWEB)

Viswanathan, Subramanian [Institute of Animal Reproduction and Food Research of the Polish Academy of Sciences, Tuwima 10, 10-747 Olsztyn (Poland); Voloshin, Yan Z. [Nesmeyanov Institute of Organoelement Compounds of the Russian Academy of Sciences, 119991 Moscow (Russian Federation); Radecka, Hanna [Institute of Animal Reproduction and Food Research of the Polish Academy of Sciences, Tuwima 10, 10-747 Olsztyn (Poland); Radecki, Jerzy [Institute of Animal Reproduction and Food Research of the Polish Academy of Sciences, Tuwima 10, 10-747 Olsztyn (Poland)], E-mail: radecki@pan.olsztyn.pl

2009-09-30

Molecular electronics has been associated with high density nano-electronic devices. Developments of molecular electronic devices were based on reversible switching of molecules between the two conductive states. In this paper, self-assembled monolayers of dodecanethiol (DDT) and thiol tethered iron(II)clathrochelate (IC) have been prepared on gold film. The electrochemical and electronic properties of IC molecules inserted into the dodecanethiol monolayer (IC-DDT SAM) were investigated using voltammetric, electrochemical impedance spectroscopy (EIS), scanning tunneling microscopy (STM) and cross-wire tunneling measurements. The voltage triggered switching behaviour of IC molecules on mixed SAM was demonstrated. Deposition of polyaniline on the redox sites of IC-DDT SAM using electrochemical polymerization of aniline was performed in order to confirm that this monolayer acts as nano-patterned semiconducting electrode surface.

Long-range interfacial electron transfer and electrocatalysis of molecular scale Prussian Blue nanoparticles linked to Au(111)-electrode surfaces by different chemical contacting groups

DEFF Research Database (Denmark)

Zhu, Nan; Ulstrup, Jens; Chi, Qijin

2017-01-01

We have explored interfacial electrochemical electron transfer (ET) and electrocatalysis of 5–6 nm Prussian Blue nanoparticles (PBNPs) immobilized on Au(111)-electrode surfaces via molecular wiring with variable-length, and differently functionalized thiol-based self-assembled molecular monolayers...... (SAMs). The SAMs contain positively (−NH3+) or negatively charged (–COO–) terminal group, as well an electrostatically neutral hydrophobic terminal group (–CH3). The surface microscopic structures of the immobilized PBNPs were characterized by high-resolution atomic force microscopy (AFM) directly...... in aqueous electrolyte solution under the same conditions as for electrochemical measurements. The PBNPs displayed fast and reversible interfacial ET on all the surfaces, notably in multi-ET steps as reflected in narrow voltammetric peaks. The ET kinetics can be controlled by adjusting the length of the SAM...

Synthesis, characterization, DNA interaction and antimicrobial screening of isatin-based polypyridyl mixed-ligand Cu(II and Zn(II complexes

Directory of Open Access Journals (Sweden)

NATARAJAN RAMAN

2010-06-01

Full Text Available Several mixed ligand Cu(II/Zn(II complexes using 3-(phenyl-imino-1,3-dihydro-2H-indol-2-one (obtained by the condensation of isatin and aniline as the primary ligand and 1,10-phenanthroline (phen/2,2’-bipyridine (bpy as an additional ligand were synthesized and characterized analytically and spectroscopically by elemental analyses, magnetic susceptibility and molar conductance measurements, as well as by UV–Vis, IR, NMR and FAB mass spectroscopy. The interaction of the complexes with calf thymus (CT DNA was studied using absorption spectra, cyclic voltammetric and viscosity measurements. They exhibit absorption hypochromicity, and the specific viscosity increased during the binding of the complexes to calf thymus DNA. The shifts in the oxidation–reduction potential and changes in peak current on addition of DNA were shown by CV measurements. The Cu(II/Zn(II complexes were found to promote cleavage of pUC19 DNA from the supercoiled form I to the open circular form II and linear form III. The complexes show enhanced antifungal and antibacterial activities compared with the free ligand.

Novel homo- and heterobinuclear ball-type phthalocyanines: synthesis and electrochemical, electrical, EPR and MCD spectral properties.

Science.gov (United States)

Odabaş, Zafer; Dumludağ, Fatih; Ozkaya, Ali Riza; Yamauchi, Seigo; Kobayashi, Nagao; Bekaroğlu, Ozer

2010-09-21

The mononuclear Fe(II) phthalocyanine 2 and ball-type homobinuclear Fe(II)-Fe(II) and Cu(II)-Cu(II) phthalocyanines, 3 and 4 respectively, were synthesized from the corresponding 4,4'-[1,1'-methylenebis-(naphthalene-2,1-diyl)]bis(oxy)diphthalonitrile 1, and then ball-type heterobinuclear Fe(II)-Cu(II) phthalocyanine 5 was synthesized from 2. The novel compounds 4 and 5 have been characterized by elemental analysis, UV/vis, IR and MALDI-TOF mass spectroscopies. Electron paramagnetic resonance and magnetic circular dichroism measurements of 3, 4 and 5 were also examined. The voltammetric measurements of the complexes showed the formation of various electrochemically stable ligand- and metal-based mixed-valence species, due to the intramolecular interactions between the two MPc units, especially in ball-type binuclear iron(II) phthalocyanine. Impedance spectroscopy and d.c. conductivity measurements of 4 and 5 were performed as a function of temperature (295-523 K) and frequency (40-10(5) Hz). While room temperature impedance spectra consist of a curved line, a transformation into a full semicircle with increasing temperature was observed for both compounds.

Exciplex mediated photoinduced electron transfer reactions of phthalocyanine-fullerene dyads.

Science.gov (United States)

Niemi, Marja; Tkachenko, Nikolai V; Efimov, Alexander; Lehtivuori, Heli; Ohkubo, Kei; Fukuzumi, Shunichi; Lemmetyinen, Helge

2008-07-31

Evidences of an intramolecular exciplex intermediate in a photoinduced electron transfer (ET) reaction of double-linked free-base and zinc phthalocyanine-C60 dyads were found. This was the first time for a dyad with phthalocyanine donor. Excitation of the phthalocyanine moiety of the dyads results in rapid ET from phthalocyanine to fullerene via an exciplex state in both polar and nonpolar solvents. Relaxation of the charge-separated (CS) state Pc(*+)-C60(*-) in a polar solvent occurs directly to the ground state in 30-70 ps. In a nonpolar solvent, roughly 20% of the molecules undergo transition from the CS state to phthalocyanine triplet state (3)Pc*-C60 before relaxation to the ground state. Formation of the CS state was confirmed with electron spin resonance measurements at low temperature in both polar and nonpolar solvent. Reaction schemes for the photoinduced ET reactions of the dyads were completed with rate constants obtained from the time-resolved absorption and emission measurements and with state energies obtained from the fluorescence, phosphorescence, and voltammetric measurements.

Voltammetric measurement of the Pt electrode capacity and the determination of the polyvalent ions diffusion coefficients in the glass melt

Czech Academy of Sciences Publication Activity Database

Vondrák, Jiří; Rohanová, D.; Klápště, Břetislav; Velická, Jana

2003-01-01

Roč. 47, č. 2 (2003), s. 51-55 ISSN 0862-5468 R&D Projects: GA AV ČR IAA4032002 Institutional research plan: CEZ:AV0Z4032918; CEZ:MSM 262200010 Keywords : electric capacity of pt electrode * polyvalent ions * Fe3- and Cr3- ions Subject RIV: CA - Inorganic Chemistry Impact factor: 0.449, year: 2003

Electrochemical Quantification of Extracellular Local H2O2 Kinetics Originating from Single Cells.

Science.gov (United States)

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.

Voltammetric behaviour of levodopa and its quantification in ...

Indian Academy of Sciences (India)

Administrator

benzenesulfonic acid) modified glassy carbon electrode (GCE) was developed for the determination of levodopa. ... β-cyclodextrine were prepared in 0⋅2 M KCl at pH. 7⋅4. All other reagents ... through the cell prior to each experiment. All ex-.

Voltammetric determination of wedelolactone, an anti-HIV herbal ...

Indian Academy of Sciences (India)

-wave and cyclic ... ing in charge transfer resistance at the boron-doped diamond electrode as compared to the glassy carbon elec- ... The effect of concentration on the peak currents of ... has low charge carrier activation energy of 0.37 eV,42.

Differential pulse voltammetric determination of theophylline at poly ...

African Journals Online (AJOL)

Bulletin of the Chemical Society of Ethiopia. Journal Home · ABOUT THIS JOURNAL · Advanced Search · Current Issue · Archives · Journal Home > Vol 26, No 1 (2012) >. Log in or Register to get access to full text downloads.

Spectrophotometric and Voltammetric Studies on the Interaction of ...

African Journals Online (AJOL)

0.84V(vs. SCE) also changed correspondingly without change of the peak potential, which also indicated that the binding reaction had taken place. Under the selected conditions a new spectrophotometric analytical method was established for ...

Spectrophotometric and Voltammetric Studies on the Interaction of ...

African Journals Online (AJOL)

NJD

Owing to the formation of the new complex, the maximum absorption wavelength of crystal ... O-sulphate and N-sulphate groups in the structures of heparin completely ... 2.1. Apparatus. A Cary 50 probe spectrophotometer (Varian, Australia) and a ... pH 3.0 by 0.2 mol L–1 aqueous solution of sodium hydroxide. All other ...

Pulse-voltammetric glucose detection at gold junction electrodes.

Science.gov (United States)

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.

differential pulse voltammetric determination of theophylline at poly

African Journals Online (AJOL)

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modified electrodes (PMEs) have received attention in recent years due to their ... alternative; selective, sensitive, simple, environmentally friendly and easily .... Figure 2. (A) CVs of poly(AHNSA)/GCE in PBS (pH 5.0), at scan rates of 20, 40, 60, ...

supp7.doc

Indian Academy of Sciences (India)

(A) Cyclic voltammeric response and (B) impedimetric response of (a) unmodified Au, (b) DTB, (c) PET and (d) DTB-PET electrodes in presence of Fe(CN)63-/4- in 0.1 M PBS (pH 7.2). Figure S2. Cyclic voltammetric response obtained for covalently bound Cyt-c on DTB-PET electrode in the (a) absence and (b) presence of ...

Determination of thorium in the range of low concentrations

International Nuclear Information System (INIS)

Hill, R.; Lieser, K.H.

1992-01-01

Methods for the determination of Th in the range of low concentrations are compiled and discussed. Application of spectrophotometry and voltammetry is investigated. Spectrophotometry is applicable down to concentrations of the order of 0.1 μg/l as long as the ratio U:Th is low. Voltammetric determination of Th is not possible in the presence of Al. (orig.)

Electrooxidation of Indomethacin at Multiwalled Carbon Nanotubes-Modified GCE and Its Determination in Pharmaceutical Dosage Form and Human Biological Fluids

OpenAIRE

Sataraddi, Sanjeevaraddi R.; Patil, Shreekant M.; Bagoji, Atmanand M.; Pattar, Vijay P.; Nandibewoor, Sharanappa T.

2014-01-01

A simple, rapid, selective, and sensitive electrochemical method for the direct determination of indomethacin was developed. The electrochemical behavior of indomethacin was carried at multiwalled carbon nanotube- (MWCNTs-) modified glassy carbon electrode (GCE). The cyclic voltammetric results indicated that MWCNT-modified glassy carbon electrode remarkably enhanced electrocatalytic activity towards the oxidation of indomethacin in slightly acidic solutions. It led to a considerable improvem...

Cobalt phthalocyanine modified electrodes utilised in electroanalysis: nano-structured modified electrodes vs. bulk modified screen-printed electrodes.

Science.gov (United States)

Foster, Christopher W; Pillay, Jeseelan; Metters, Jonathan P; Banks, Craig E

2014-11-19

Cobalt phthalocyanine (CoPC) compounds have been reported to provide electrocatalytic performances towards a substantial number of analytes. In these configurations, electrodes are typically constructed via drop casting the CoPC onto a supporting electrode substrate, while in other cases the CoPC complex is incorporated within the ink of a screen-printed sensor, providing a one-shot economical and disposable electrode configuration. In this paper we critically compare CoPC modified electrodes prepared by drop casting CoPC nanoparticles (nano-CoPC) onto a range of carbon based electrode substrates with that of CoPC bulk modified screen-printed electrodes in the sensing of the model analytes L-ascorbic acid, oxygen and hydrazine. It is found that no "electrocatalysis" is observed towards L-ascorbic acid using either of these CoPC modified electrode configurations and that the bare underlying carbon electrode is the origin of the obtained voltammetric signal, which gives rise to useful electroanalytical signatures, providing new insights into literature reports where "electrocatalysis" has been reported with no clear control experiments undertaken. On the other hand true electrocatalysis is observed towards hydrazine, where no such voltammetric features are witnessed on the bare underlying electrode substrate.

Electrode reactions of iron oxide-hydroxide colloids.

Science.gov (United States)

Mahmoudi, Leila; Kissner, Reinhard

2014-11-07

Small-sized FeO(OH) colloids stabilised by sugars, commercially available for the clinical treatment of iron deficiency, show two waves during cathodic polarographic sweeps, or two current maxima with stationary electrodes, in neutral to slightly alkaline aqueous medium. Similar signals are observed with Fe(III) in alkaline media, pH > 12, containing citrate in excess. Voltammetric and polarographic responses reveal a strong influence of fast adsorption processes on gold and mercury. Visible spontaneous accumulation was also observed on platinum. The voltammetric signal at more positive potential is caused by Fe(III)→Fe(II) reduction, while the one at more negative potential has previously been assigned to Fe(II)→Fe(0) reduction. However, the involvement of adsorption phenomena leads us to the conclusion that the second cathodic current is caused again by Fe(III)→Fe(II), of species deeper inside the particles than those causing the first wave. This is further supported by X-ray photoelectron spectra obtained after FeO(OH) particle adsorption and reduction on a gold electrode surface. The same analysis suggests that sucrose stabilising the colloid is still bound to the adsorbed material, despite dilution and rinsing.

Important parameters affecting the cell voltage of aqueous electrical double-layer capacitors

Science.gov (United States)

Wu, Tzu-Ho; Hsu, Chun-Tsung; Hu, Chi-Chang; Hardwick, Laurence J.

2013-11-01

This study discusses and demonstrates how the open-circuit potential and charges stored in the working potential window on positive and negative electrodes affect the cell voltage of carbon-based electrical double-layer capacitors (EDLCs) in aqueous electrolytes. An EDLC consisting of two activated carbon electrodes is employed as the model system for identifying these key parameters although the potential window of water decomposition can be simply determined by voltammetric methods. First, the capacitive performances of an EDLC with the same charge on positive and negative electrodes are evaluated by cyclic voltammetric, charge-discharge, electrochemical impedance spectroscopic (EIS) analyses, and inductance-capacitance-resistance meter (LCR meter). The principles for obtaining the highest acceptable cell voltage of such symmetric ECs with excellent reversibility and capacitor-like behaviour are proposed. Aqueous charge-balanced EDLCs can be operated as high as 2.0 V with high energy efficiency (about 90%) and only 4% capacitance loss after the 600-cycle stability checking. The necessity of charge balance (but not capacitance balance) for positive and negative electrodes is substantiated from the lower acceptable cell voltage of charge-unbalanced EDLCs.

ELECTROCHEMICAL FINGERPRINT STUDIES OF SELECTED MEDICINAL PLANTS RICH IN FLAVONOIDS.

Science.gov (United States)

Konieczyński, Paweł

2015-01-01

The combination of a size-exclusion column (SEC) with electrochemical (voltammetric) detection at a boron-doped diamond electrode (BDDE) was applied for studying the correlations between electroactive Cu and Fe species with phenolic groups of flavonoids. For comparison with electrochemical results, SEC-HPLC-DAD detection was used. The studied plant material comprised of: Betula verrucosa Ehrh., Equisetun arvense L., Polygonum aviculare L., Viola tricolor L., Crataegus oxyacantha L., Sambucus nigra L. and Helichrysum arenarium (L.) Moench. Based upon the results, high negative correlation was found for the chromatographic peak currents at 45 min with the sum of Cu and Fe for the aqueous extracts of Sambucus, Crataegus and Betula species, and for the peak currents at 65 min of the aqueous extracts of Sambucus, Crataegus, Helichrysum and Betula botanical species. This behavior confirms that it is mainly the flavonoids with easily oxidizable phenolic groups which are strongly influenced by the presence of Cu and Fe. Moreover, the electrochemical profiles obtained thanks to the use of HPLC hyphenated with voltammetric detection can be potentially applied for fingerprint studies of the plant materials used in medicine.

Electrochemical determination of resveratrol in dietary supplements at a boron-doped diamond electrode in the presence of hexadecyltrimethylammonium bromide using square-wave adsorptive stripping voltammetry

Directory of Open Access Journals (Sweden)

Yardim Yavuz

2017-01-01

Full Text Available A sensitive electroanalytical methodology for the determination of resveratrol is presented for the first time using adsorptive stripping voltammetry at a bare boron-doped diamond (BDD electrode. In cyclic voltammetry, resveratrol shows one irreversible and an adsorption-controlled oxidation peak at a BDD electrode. The voltammetric results indicated that in the presence of hexadecyl trimethyl ammonium bromide, the BDD electrode remarkably enhanced the oxidation of resveratrol, which leads to an improvement in the peak current with a shift of the peak potential to more positive values. Using the square-wave stripping mode, the compound yielded a well-defined voltammetric response in 0.1 M nitric acid solution containing 100 μmol L-1 hexadecyl trimethyl ammonium bromide at 0.74 V (vs. Ag/AgCl, after 60 s accumulation at the open-circuit condition. A linear calibration graph was obtained in the concentration range 0.025 to 60.0 μg mL-1, with a detection limit of 0.0063 μg mL-1. The applicability of the proposed method was verified by analysis of resveratrol in commercial dietary supplements.

Electrochemical sensor for ranitidine determination based on carbon paste electrode modified with oxovanadium (IV) salen complex.

Science.gov (United States)

Raymundo-Pereira, Paulo A; Teixeira, Marcos F S; Fatibello-Filho, Orlando; Dockal, Edward R; Bonifácio, Viviane Gomes; Marcolino, Luiz H

2013-10-01

The preparation and electrochemical characterization of a carbon paste electrode modified with the N,N-ethylene-bis(salicyllideneiminato)oxovanadium (IV) complex ([VO(salen)]) as well as its application for ranitidine determination are described. The electrochemical behavior of the modified electrode for the electroreduction of ranitidine was investigated using cyclic voltammetry, and analytical curves were obtained for ranitidine using linear sweep voltammetry (LSV) under optimized conditions. The best voltammetric response was obtained for an electrode composition of 20% (m/m) [VO(salen)] in the paste, 0.10 mol L(-1) of KCl solution (pH 5.5 adjusted with HCl) as supporting electrolyte and scan rate of 25 mV s(-1). A sensitive linear voltammetric response for ranitidine was obtained in the concentration range from 9.9×10(-5) to 1.0×10(-3) mol L(-1), with a detection limit of 6.6×10(-5) mol L(-1) using linear sweep voltammetry. These results demonstrated the viability of this modified electrode as a sensor for determination, quality control and routine analysis of ranitidine in pharmaceutical formulations. Copyright © 2013. Published by Elsevier B.V.

An Electrochemical Sensor Based on Nanostructured Hollandite-type Manganese Oxide for Detection of Potassium Ions

Directory of Open Access Journals (Sweden)

Alex S. Lima

2009-08-01

Full Text Available The participation of cations in redox reactions of manganese oxides provides an opportunity for development of chemical sensors for non-electroactive ions. A sensor based on a nanostructured hollandite-type manganese oxide was investigated for voltammetric detection of potassium ions. The detection is based on the measurement of anodic current generated by oxidation of Mn(III to Mn(IV at the surface of the electrode and the subsequent extraction of the potassium ions into the hollandite structure. In this work, an amperometric procedure at an operating potential of 0.80 V (versus SCE is exploited for amperometric monitoring. The current signals are linearly proportional to potassium ion concentration in the range 4.97 × 10−5 to 9.05 × 10−4 mol L−1, with a correlation coefficient of 0.9997.

Recent Advances in Electrochemical Glycobiosensing

Directory of Open Access Journals (Sweden)

Germarie Sánchez-Pomales

2011-01-01

Full Text Available Biosensors based on electrochemical transduction mechanisms have recently made advances into the field of glycan analysis. These glyco-biosensors offer simple, rapid, sensitive, and economical approaches to the measurement need for rapid glycan analysis for biomarker detection, cancer and disease diagnostics, and bioprocess monitoring of therapeutic glycoproteins. Although the prevalent methods of glycan analysis (high-performance liquid chromatography, mass spectrometry, and nuclear magnetic resonance spectroscopy provide detailed identification and structural analysis of glycan species, there are significantly few low-cost, rapid glycan assays available for diagnostic and screening applications. Here we review instances in which glyco-biosensors have been used for glycan analysis using a variety of electrochemical transduction mechanisms (e.g., amperometric, potentiometric, impedimetric, and voltammetric, selective binding agents (e.g., lectins and antibodies, and redox species (e.g., enzyme substrates, inorganic, and nanomaterial.

Using Poly-L-Histidine Modified Glassy Carbon Electrode to Trace Hydroquinone in the Sewage Water

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Bin Wang

2014-01-01

Full Text Available A sensitive voltammetric method for trace measurements of hydroquinone in the sewage water is described. The poly-L-histidine is prepared to modify the glassy carbon electrode in order to improve the electrochemical catalysis of interesting substances such as hydroquinone. The influence of the base solution, pH value, and scanning speed on the tracing of hydroquinone is discussed, and the experimental procedures and conditions are optimized. The laboratory results show that it is possible to construct a linear calibration curve between the peak current of hydroquinone on modified electrode and its concentration at the level of 0.00001 mol/L. The potential limitation of the method is suggested by a linear peaking shift model as well. The method was successfully applied to the determination of hydroquinone in the actual sample of industrial waste water.

Formation and proof of stable bi-, tri- and tetraradical polyanions during the electrochemical reduction of cone-polynitrocalix[4]arenes. An ESR-UV-vis spectroelectrochemical study

International Nuclear Information System (INIS)

Liška, Alan; Rosenkranz, Marco; Klíma, Jiří; Dunsch, Lothar; Lhoták, Pavel; Ludvík, Jiří

2014-01-01

Graphical abstract: - Abstract: The first intermediates of electrochemical reduction of nitro compounds in nonaqueous DMF are stable radical anions. In the series of mono-, di-, tri- and tetranitro calix[4]arenes each nitro group represents a reduction center, therefore the question about the spin state of intermediary anions arises. In this communication, the voltammetric and coulometric investigation of these compounds is performed together with the spectral measurements (ESR and UV-vis). The in-situ spectroelectrochemical approach proved that during reduction, in all polynitro radicalic intermediates the electrons remain unpaired and thus relatively stable mono-, di-, tri- and tetraradical mono-, di-, tri- and tetraanions, respectively, can be electrochemically generated in aprotic DMF from polynitrocalix[4]arenes. This finding confirms that the nitrophenyl units in polynitrocalix[4]arenes are completely independent and no mutual electronic communication takes place among them

Voltametrické stanovení pesticidů na meniskem modifikované stříbrné pevné amalgamové elektrodě

OpenAIRE

Gajdár, Július

2013-01-01

The aim of this bachelor thesis is to find the optimal conditions for voltammetric determination of pesticides cypermethrin, deltamethrin and difenzoquat on meniscus modified silver solid amalgam electrode using differential pulse voltammetry. Conditions under which cypermethrin and deltamethrin could be determinated were found in previously published works. These conditions were reproduced. Substances were studied in methanol and dimethylformamide solutions. The optimal conditions for determ...

Carbon paste electrodes in electroanalytical chemistry

Directory of Open Access Journals (Sweden)

KAREL VYTŘAS

2009-09-01

Full Text Available An overview is given dealing with the applications of carbon paste electrodes in equilibrium potentiometry as well as in electrochemical stripping analysis using both voltammetric and potentiometric modes. Various modifications of carbon pastes and carbon paste-based biosensors are also mentioned. The main emphasis in this article is directed at summarizing recent results of the authors’ research group during the past few years.

A composite material based on nanoparticles of yttrium (III) oxide for the selective and sensitive electrochemical determination of acetaminophen

International Nuclear Information System (INIS)

Baytak, Aysegul Kutluay; Teker, Tugce; Duzmen, Sehriban; Aslanoglu, Mehmet

2016-01-01

An electrochemical sensor was prepared by modifying a glassy carbon electrode (GCE) with a composite of yttrium (III) oxide nanoparticles (Y_2O_3NPs) and carbon nanotubes (CNTs) for the determination of acetaminophen (ACT). Compared with a bare GCE and CNTs/GCE, the Y_2O_3NPs/CNTs/GCE exhibited a well-defined redox couple for ACT and highly enhanced the current response. The separations in the anodic and cathodic peak potentials (ΔE_p) for ACT were 552 mV, 24 mV and 10 mV at ba4re GCE, CNTs/GCE and Y_2O_3NPs/CNTs/GCE, respectively. The observation of only 10 mV of ΔE_p for ACT at Y_2O_3NPs/CNTs/GCE was a clear indication of a great acceleration of the electrode process compared to bare GCE and GCE modified with CNTs. Also, L-ascorbic acid (L-AA) and L-tyrosine (L-TRY) did not interfere with the selective determination of ACT. Square wave voltammetry (SWV) was performed for the quantification of ACT. A linear plot was obtained for current responses versus the concentrations of ACT over the range from 1.0 × 10"−"1"0 to 1.8 × 10"−"8 M with a detection limit of 3.0 × 10"−"1"1 M (based on 3S_b/m). The proposed composite material provided high electrocatalytic activity, improved voltammetric behavior, good selectivity and good reproducibility. The accurate quantification of ACT makes the proposed electrode of great interest for the public health. - Highlights: • A voltammetric sensor based on yttrium oxide was prepared for the detection of ACT. • The proposed electrode has greatly accelerated the voltammetric process of ACT. • A detection limit of 0.03 nM was obtained for ACT. • The proposed electrode exhibited great selectivity for ACT in the presence of L-AA and L-TRY. • The composite material exhibited high sensitivity, good stability and excellent reproducibility.

A novel composite electrode based on tungsten oxide nanoparticles and carbon nanotubes for the electrochemical determination of paracetamol

Energy Technology Data Exchange (ETDEWEB)

Baytak, Aysegul Kutluay; Duzmen, Sehriban; Teker, Tugce; Aslanoglu, Mehmet, E-mail: maslanoglu@harran.edu.tr

2015-12-01

An electrochemical sensor was prepared by the modification of a glassy carbon electrode (GCE) with a composite of nanoparticles of tungsten oxide (WO{sub 3}) and carbon nanotubes (CNTs) for the quantification of paracetamol (PR). Energy dispersive X-ray analysis (EDX) and scanning electron microscopy (SEM) were performed for the characterization of the nanocomposite layer. Compared with a bare GCE and a GCE modified with CNTs, the proposed electrode (WO{sub 3}NPs/CNTs/GCE) exhibited a well-defined redox couple for PR and a marked enhancement of the current response. The experimental results also showed that ascorbic acid (AA) did not interfere with the selective determination of PR. The proposed electrode was used for the determination of PR in 0.1 M phosphate buffer solution (PBS) at pH 7.0 using square wave voltammetry (SWV). The peak current increased linearly with the concentration of PR in the range of 1.0 × 10{sup −9}–2.0 × 10{sup −7} M. The detection limit (LOD) was 5.54 × 10{sup −11} M (based on 3 S{sub b}/m). The proposed voltammetric sensor provided long-time stability, improved voltammetric behavior and good reproducibility for PR. The selective, accurate and precise determination of PR makes the proposed electrode of great interest for monitoring its therapeutic use. - Highlights: • A voltammetric nanosensor was prepared using nanoparticles of WO{sub 3} and CNTs. • A selective quantification of paracetamol was carried out in the presence of AA. • A linear plot was obtained for current responses versus concentrations over the range from 1.0 × 10{sup −9} to 2.0 × 10{sup −7} M. • A detection limit of 554 pM was obtained for paracetamol using the proposed nanosensor. • An accurate quantification makes the proposed nanosensor of great interest for public health.

Fabrification of electroreduced graphene oxide–bentonite sodium composite modified electrode and its sensing application for linezolid

International Nuclear Information System (INIS)

Prashanth, S.N.; Teradal, Nagappa L.; Seetharamappa, J.; Satpati, Ashis K.; Reddy, A.V.R.

2014-01-01

Graphene and its composites have attracted considerable attention in synthesis and electrochemical applications. In the present work, we have synthesized and characterized graphene oxide-bentonite composite (GO-BEN) and utilized it to fabricate an electrochemical sensor. For this, the solution of GO-BEN cast on glassy carbon electrode (GCE) was reduced electrochemically in phosphate buffer solution of pH 6 to obtain electrochemically reduced graphene oxide-bentonite composite (ERGO-BEN-GCE). This ERGO-BEN film was used for electrochemical investigation of an oxazolidinone class of antibiotic, linezolid (LIN) for the first time. The electrochemical sensor showed excellent enhancement and adsorptive ability towards the electrooxidation of LIN. LIN exhibited two each of oxidation and reduction peaks on ERGO-BEN film in phosphate buffer of pH 7.0. Effects of accumulation time, pH of solution and scan rate were studied and various electrochemical parameters were evaluated. The plot of pH versus E p gave a slope of 26.2 mV/pH in the pH range of 4.2-8.0 indicating the participation of two electrons and one proton in the electrode process. An adsorptive stripping differential pulse voltammetric method (AdSDPV) was developed for the determination of LIN in bulk, pharmaceutical formulations and urine samples. Adsorptive stripping linear sweep voltammetric (AdSLSV) and differential pulse voltammetric (DPV) methods were also developed and the results were compared. LIN showed linear relationship between the current density and concentration in the range of 0.25 - 31.25 μM with a LOD of 0.0337 μM in AdSDPV method; 0.5 - 31.25 μM with a LOD of 0.100 μM in DPV method and 1.25 - 37.5 μM with a LOD of 0.5461 μM in AdSLSV method respectively. The proposed AdSDPV method was observed to be simple, fast and inexpensive and hence, could be readily adopted for quality control in pharmaceutical products

One at a time: counting single-nanoparticle/electrode collisions for accurate particle sizing by overcoming the instability of gold nanoparticles under electrolytic conditions

International Nuclear Information System (INIS)

Qiu, Danfeng; Wang, Song; Zheng, Yuanqin; Deng, Zhaoxiang

2013-01-01

In response to an increasing demand for understanding electrochemical processes on the nanometer scale, it now becomes possible to monitor electron transfer reactions at the single-nanoparticle level, namely particle collision electrochemistry. This technique has great potential in the development of research tools towards single-particle electrocatalysis and selective and multiplexed particle sizing. However, one existing problem that may discourage these applications is the relatively weak colloidal stability of nanoparticles in an electrolytic solution. Here we report on a facile but efficient way to achieve a good stability of gold nanoparticles in an acidic media so that ‘zero-aggregation’ collisions can be achieved at a carbon ultramicroelectrode. This allows us to obtain anodic dissolution currents from individual nanoparticles in a ‘one particle at a time’ manner, based on which accurate particle sizing with a resolution of 1–2 nm can be achieved. Our work strongly suggests that to maintain a well dispersed nanoparticle solution during a particle impact electrochemical experiment is critically important for accurate particle sizing, as well as other applications that require information to be extracted from individual nanoparticles (not their aggregates). (paper)

Graphene–platinum nanocomposite as a sensitive and selective voltammetric sensor for trace level arsenic quantification

Directory of Open Access Journals (Sweden)

R. Kempegowda

2014-01-01

Full Text Available A simple protocol for the chemical modification of graphene with platinum nanoparticles and its subsequent electroanalytical application toward sensitive and selective determination of arsenic has been described. Chemical modification was carried out by the simultaneous and sequential chemical reduction of graphene oxide and hexachloroplatinic acid in the presence of ethylene glycol as a mild reducing agent. The synthesized graphene–platinum nanocomposite (Gr–nPt has been characterized through infrared spectroscopy, x-ray diffraction study, field emission scanning electron microscopy and cyclic voltammetry (CV techniques. CV and square-wave anodic stripping voltammetry have been used to quantify arsenic. The proposed nanostructure showed linearity in the concentration range 10–100 nM with a detection limit of 1.1 nM. The proposed sensor has been successfully applied to measure trace levels of arsenic present in natural sample matrices like borewell water, polluted lake water, agricultural soil, tomato and spinach leaves.

[Development and application of electroanalytical methods in biomedical fields].

Science.gov (United States)

Kusu, Fumiyo

2015-01-01

To summarize our electroanalytical research in the biomedical field over the past 43 years, this review describes studies on specular reflection measurement, redox potential determination, amperometric acid sensing, HPLC with electrochemical detection, and potential oscillation across a liquid membrane. The specular reflection method was used for clarifying the adsorption of neurotransmitters and their related drugs onto a gold electrode and the interaction between dental alloys and compound iodine glycerin. A voltammetric screening test using a redox potential for the antioxidative effect of flavonoids was proposed. Amperometric acid sensing based on the measurement of the reduction prepeak current of 2-methyl-1,4-naphthoquinone (VK3) or 3,5-di-tert-buty1-1,2-benzoquinone (DBBQ) was applied to determine acid values of fats and oils, titrable acidity of coffee, and enzyme activity of lipase, free fatty acids (FFAs) in serum, short-chain fatty acids in feces, etc. The electrode reactions of phenothiazines, catechins, and cholesterol were applied to biomedical analysis using HPLC with electrochemical detection. A three-channel electrochemical detection system was utilized for the sensitive determination of redox compounds in Chinese herbal medicines. The behavior of barbituric acid derivatives was examined based on potential oscillation measurements.

Metal ion analysis in contaminated water samples using anodic stripping voltammetry and a nanocrystalline diamond thin-film electrode

International Nuclear Information System (INIS)

Sonthalia, Prerna; McGaw, Elizabeth; Show, Yoshiyuki; Swain, Greg M.

2004-01-01

Boron-doped nanocrystalline diamond thin-film electrodes were employed for the detection and quantification of Ag (I), Cu (II), Pb (II), Cd (II), and Zn (II) in several contaminated water samples using anodic stripping voltammetric (ASV). Diamond is an alternate electrode that possesses many of the same attributes as Hg and, therefore, appears to be a viable material for this electroanalytical measurement. The nanocrystalline form has been found to perform slightly better than the more conventional microcrystalline form of diamond in this application. Differential pulse voltammetry (DPASV) was used to detect these metal ions in lake water, well water, tap water, wastewater treatment sludge, and soil. The electrochemical results were compared with data from inductively coupled plasma mass spectrometric (ICP-MS) and or atomic absorption spectrometric (AAS) measurements of the same samples. Diamond is shown to function well in this electroanalytical application, providing a wide linear dynamic range, a low limit of quantitation, excellent response precision, and good response accuracy. For the analysis of Pb (II), bare diamond provided a response nearly identical to that obtained with a Hg-coated glassy carbon electrode

Stripping voltammetry of technetium using a TOA modified carbon paste electrode

International Nuclear Information System (INIS)

Ruf, H.; Schorb, K.

1989-10-01

Low concentrations of technetium have been measured DP-stripping-voltammetrically using a carbon paste electrode modified with tri-n-octylamine (TOA-CPE). Preconcentration of the metal ion on the electrode surface accomplished by dipping of the latter in the sample solution which is 2M in HCl, relies on the chemical reaction with the amine acting as a liquid anion exchanger. Both, Tc-IV occurring as the TcCl 6 2- ion in chloride solutions as well as Tc-VII hereby are deposited. Measurements following deposition yield voltammograms of essentially different shapes for the two Tc species. With Tc-IV a characteristic curve with a prominent current signal at -280 mV (vs. Ag/AgCl) is obtained which can be evaluated for Tc quantitation. However, starting from Tc-VII, complex voltammograms are registered not allowing direct technetium assays. Nevertheless, after reduction to Tc-IV, e.g. by means of ascorbic acid, also Tc-VII can be quantified reliably by the method described, the lower detection limit for both oxidation states being about 4x10 -8 M. (orig.) [de

On the purity assessment of solid sodium borohydride

Science.gov (United States)

Botasini, Santiago; Méndez, Eduardo

2012-01-01

Since sodium borohydride has become extensively used as chemical hydrogen storage material in fuel cells, many techniques have been proposed to assess the purity of this substance. However, all of them are developed in aqueous media, where the reagent is unstable. In addition, its hygroscopic nature was difficults in any attempt to make precise quantifications. The present work compares three different methods, namely, voltammetric, titrimetric, and Fourier transformed infrared spectroscopy (FTIR) in order to assess the purity of sodium borohydride, using an expired and a new sodium borohydride samples as references. Our results show that only the FTIR measurements provide a simple and semi-quantitative means to assess the purity of sodium borohydride due to the fact that it is the only one that measures the sample in the solid state. A comparison between the experimental data and theoretical calculation reveals the identification of the absorption bands at 1437 cm-1 of sodium metaborate and 2291 cm-1 of sodium borohydride which represent a good fingerprint for the qualitative assessment of the sample quality.

Activation of glassy carbon electrodes by photocatalytic pretreatment

Energy Technology Data Exchange (ETDEWEB)

Dumanli, Onur [Department of Chemistry, Faculty of Science and Art, Ondokuz Mayis University, Kurupelit, 55139 Samsun (Turkey); Onar, A. Nur [Department of Chemistry, Faculty of Science and Art, Ondokuz Mayis University, Kurupelit, 55139 Samsun (Turkey)], E-mail: nonar@omu.edu.tr

2009-11-01

This paper describes a simple and rapid photocatalytic pretreatment procedure that removes contaminants from glassy carbon (GC) surfaces. The effectiveness of TiO{sub 2} mediated photocatalytic pretreatment procedure was compared to commonly used alumina polishing procedure. Cyclic voltammetric and chronocoulometric measurements were carried out to assess the changes in electrode reactivity by using four redox systems. Electrochemical measurements obtained on photocatalytically treated GC electrodes showed a more active surface relative to polished GC. In cyclic voltammograms of epinephrine, Fe(CN){sub 6}{sup 3-/4-} and ferrocene redox systems, higher oxidation and reduction currents were observed. The heterogeneous electron transfer rate constants (k{sup o}) were calculated for Fe(CN){sub 6}{sup 3-/4-} and ferrocene which were greater for photocatalytic pretreatment. Chronocoulometry was performed in order to find the amount of adsorbed methylene blue onto the electrode and was calculated as 0.34 pmol cm{sup -2} for photocatalytically pretreated GC. The proposed photocatalytic GC electrode cleansing and activating pretreatment procedure was more effective than classical alumina polishing.

Voltammetric assay of extremely low technetium concentrations following enrichment at the HMDE after reaction with Thiocyanate

International Nuclear Information System (INIS)

Friedrich, M.; Ruf, H.

1984-12-01

It is known that in sulfuric acid solution pertechnetate is reduced by thiocyanate to form thiocyanate complexes. After this reaction the technetium acquires the capability of being adsorbed at the hanging mercury drop electrode (HMDE) provided that a potential of -0,40 V (vs. Ag/AgCl) has been applied to the electrode. If, by application of the differential pulse voltammetry after the phase of deposition the potential at the electrode is scanned cathodically, traces of technetium can be determined very sensitively by evaluation of the peak current recorded at minus 1,27 V (Ag/AgCl). The effect is still being enhanced by the presence of not interfering small perrhenate amounts. The reproducibility of the measured values is excellent. (orig.) [de

Electrochemical and spectroscopic characterisation of amphetamine-like drugs: Application to the screening of 3,4-methylenedioxymethamphetamine (MDMA) and its synthetic precursors

OpenAIRE

Milhazes, Nuno; Martins, Pedro; Uriarte, Eugenio; Garrido, Jorge; Calheiros, Rita; Marques, M. Paula M.; Borges, Fernanda

2007-01-01

A complete physicochemical characterisation of MDMA and its synthetic precursors MDA, 3,4-methylenedioxybenzaldehyde (piperonal) and 3,4-methylenedioxy-beta-methyl-beta-nitrostyrene was carried out through voltammetric assays and Raman spectroscopy combined with theoretical (DFT) calculations. The former provided important analytical redox data, concluding that the oxidative mechanism of the N-demethylation of MDMA involves the removal of an electron from the amino-nitrogen atom, leading to t...

Electrochemical analysis of Os(VI)-modified glycoproteins and label-free glycoprotein detection eluted from lectin capillary column

Czech Academy of Sciences Publication Activity Database

Trefulka, Mojmír; Dorčák, Vlastimil; Křenková, Jana; Foret, František; Paleček, Emil

2017-01-01

Roč. 239, JUN 2017 (2017), s. 10-15 ISSN 0013-4686 R&D Projects: GA ČR(CZ) GA15-15479S Institutional support: RVO:68081707 ; RVO:68081715 Keywords : voltammetric determination * modified electrodes * high-sensitivity * concanavalin-a Subject RIV: CG - Electrochemistry; CB - Analytical Chemistry, Separation (UIACH-O) OBOR OECD: Electrochemistry (dry cells, batteries, fuel cells, corrosion metals, electrolysis); Analytical chemistry (UIACH-O) Impact factor: 4.798, year: 2016

Combination of {sup 13}C/{sup 113}Cd NMR, potentiometry, and voltammetry in characterizing the interactions between Cd and two models of the main components of soil organic matter

Energy Technology Data Exchange (ETDEWEB)

Lenoble, V. [IFRE PMSE 112, CEREGE (UMR 6635 CNRS/Universite Paul Cezanne), Aix-en-Provence (France); Universite du Sud Toulon Var, Laboratoire PROTEE, La Garde Cedex (France); Garnier, C. [Universite du Sud Toulon Var, Laboratoire PROTEE, La Garde Cedex (France); Universite Bordeaux I, ISM-LPTC (UMR CNRS 5255), Talence (France); Masion, A.; Garnier, J.M. [IFRE PMSE 112, CEREGE (UMR 6635 CNRS/Universite Paul Cezanne), Aix-en-Provence (France); Ziarelli, F. [CNRS, Federation des Sciences Chimiques de Marseille, Spectropole, Marseille cedex 20 (France)

2008-01-15

This work allowed the characterization of the Cd-binding sites of two compounds taken as models for exudates, the main components of soil organic matter (SOM). The studied compounds were exopolysaccharides (EPS), specifically exudates of roots (polygalacturonic acid) and of soil bacteria (Phytagel). Potentiometric acid-base titrations were performed and fitting of the obtained results indicated the presence of two main classes of acidic sites, defined by their pK{sub a} values, for both EPS but of a different nature when comparing the two compounds. The two studied exopolysaccharides presented different acidic/basic site ratios: 0.15 for Phytagel and 0.76 for polygalacturonic acid. Spectroscopic techniques ({sup 13}C/{sup 113}Cd NMR, FTIR) distinguished different Cd surroundings for each of the studied EPS, which is in agreement with the titration results. Furthermore, these analyses indicated the presence of -COOH and -OH groups in various proportions for each exopolysaccharide, which should be linked to their reactivity towards cadmium. Cadmium titrations (voltammetric measurements) also differentiated different binding sites for each compound and allowed the determination of the strength of the Cd-binding site of the EPS. Fitting of the results of such voltammetric measurements was performed using PROSECE (Programme d'Optimisation et de Speciation Chimique dans l'Environnement), a software coupling chemical speciation calculation and binding parameter optimization. The fitting, taking into account the Cd{sup 2+}/H{sup +} competition towards exopolysaccharides, confirmed the acid-base titrations and spectroscopic analyses by revealing two classes of binding sites: (i) one defined as a strong complexant regarding its Cd{sup 2+}-EPS association (logK = 9-10.4) and with basic functionality regarding H{sup +}-EPS association (pK{sub a} = 11.3-11.7), and (ii) one defined as a weak complexant (logK = 7.1-8.2) and with acidic functionality (pK{sub a} = 3

Electrochemical oxidation of chlorpheniramine at polytyramine film doped with ruthenium (II) complex: Measurement, kinetic and thermodynamic studies

International Nuclear Information System (INIS)

Khudaish, Emad A.; Al-Hinaai, Mohammed; Al-Harthy, Salim; Laxman, Karthik

2014-01-01

Highlights: • XPS data confirm doping of ruthenium onto the polytyramine moiety. • Doping of Ru decreases the Pty resistivity and increases the electron transfer kinetics. • The resulting sensor is stable for a large range of CPM concentration. • Estimated values of thermodynamic and kinetic parameters were comparable. • Application to commercial dosage forms was excellent and satisfactory. - Abstract: A solid-state sensor based on polytyramine film deposited at glassy carbon electrode doped with tris(2,2′-bipyridyl)Ru(II) complex (Ru/Pty/GCE) was constructed electrochemically. A redox property represented by [Ru(bpy) 3 ] 3+/2+ couple immobilized at the Pty moiety was characterized using typical voltammetric techniques. The XPS data and AFM images confirm the grafting of Ru species on the top of Pty while the electrochemical impedance spectroscopy (EIS) data supports the immobilization of both surface modifiers onto the GCE. The constructed sensor exhibits a substantial reactivity, stability and high sensitivity to chlorpheniramine maleate (CPM) oxidation. The detection limit (S/N = 3) was brought down to 338 nM using differential pulse voltammetry method. Thermodynamic and kinetic parameters were evaluated using hydrodynamic method. The apparent diffusion coefficient and the heterogeneous electron transfer rate constant for the CPM oxidation were 2.67 × 10 −5 cm 2 s −1 and 3.21 × 10 −3 cm s −1 , respectively. Interference studies and real sample analysis were conducted with excellent performance and satisfactory results

Mechanisms and kinetics of electrodeposition of alkali metals on solid and liquid mercury electrodes

Energy Technology Data Exchange (ETDEWEB)

Lu, Wenzhe.

1993-01-01

Electroreduction of alkali metal ions at mercury is an important area in electrochemistry related to the battery industry. In this work, four major topics were considered: alkali metal/mercury interactions; electrosorption of alkali metal ions on solid mercury; electroreduction of alkali metal/crown ether complexes; and ammonium amalgam formation. The formation of alkali metal-mercury intermetallic compounds was studied on liquid and frozen thin layer mercury electrodes. The stoichiometry of the compounds produced under these conditions was determined using cyclic voltammetry. As expected, formation of a new phase was preceded by nucleation phenomena, which were particularly easy to monitor at solid Hg electrodes. The nucleation kinetics were studied using the chronoamperometric method. At very low temperatures, when the mobility of mercury atoms was restricted, the electrosorption of alkali metal ions on solid mercury electrodes was noted. Subsequent study allowed determination of the electrosorption parameters. The free energy of electrosorption is discussed in terms of interactions between alkali metals and mercury. The effect of crown ethers on the kinetics of alkali metal ion reduction was studied at both standard size and ultramicro-mercury electrodes in nonaqueous solutions using ultrafast cyclic voltammetry and ac voltammetry. The usefulness of ultrafast cyclic voltammetry with ultramicroelectrodes in measurements of the kinetics of amalgam formation was verified in a brief study of cadmium ion reduction. The mechanism of the complex reduction at mercury was analyzed based on the free energy changes before and after the activation state. In addition, the stoichiometry and formation constants of the crown ether/alkali metal complexes were determined using cyclic voltammetry. The mechanism of electroreduction of ammonium ions at mercury electrodes in non-aqueous media was analyzed.

Spectroelectrochemical study of polyphenylene by in situ external reflection FT-IR spectroscopy. Pt. 2

International Nuclear Information System (INIS)

Kvarnstroem, C.; Ivaska, A.

1994-01-01

In situ external reflection FT-IR measurements are performed during cyclic voltammetric scans on electrochemically polymerized polyphenylene films. The films are polymerized either in 0.1 or 0.8 M biphenyl in 0.1 M TBABF 4 in acetonitrile. Changes in the IR spectrum of films of different thicknesses are studied when the films are potentially cycled from the neutral to the oxidized states of the polymer. No differences between films made in high or low dimer concentration can be observed in the spectra. The potential-dependent insertion and expulsion of solvent, residual water, anions and cations in and out of the film have different behaviour in films of different thicknesses. Changes in the structure of the segments in the film, from the benzenoid form into the quinoid form, can be followed. Differences between the first and subsequent cyclic potential scans are observed. (orig.)

Electrochemical investigation of mineral electrodes in phosphate-buffered alkaline solution

Directory of Open Access Journals (Sweden)

D Erdenechimeg

2014-12-01

Full Text Available Cyclic voltammetric methods have been applied to study the electrochemical behavior of the sulfide minerals in phosphate-buffered alkaline solution. The redox process of electrodes of sulfide ores was investigated using silicone-impregnated graphite electrode. The cathodic and anodic reaction products in alkaline solution were determined within the potential range of -2V to +2V (vs. Ag/AgCl. The several successive measurement cycles’ voltammograms leads to the appearance of a new anodic peak at E = 450mV, which is absent in the first cycle and curves, as well as other features that appear in cycling, can probably be explained by secondary electrochemical transformations of the products formed by the oxidation of the original pyrite at the interface between the electrode material.DOI: http://doi.dx.org/10.5564/mjc.v15i0.318 Mongolian Journal of Chemistry 15 (41, 2014, p33-35

Potential toxicity of phthalic acid esters plasticizer: interaction of dimethyl phthalate with trypsin in vitro.

Science.gov (United States)

Wang, Yaping; Zhang, Guowen; Wang, Langhong

2015-01-14

Dimethyl phthalate (DMP) is widely used as a plasticizer in industrial processes and has been reported to possess potential toxicity to the human body. In this study, the interaction between DMP and trypsin in vitro was investigated. The results of fluorescence, UV–vis, circular dichroism, and Fourier transform infrared spectra along with cyclic voltammetric measurements indicated that the remarkable fluorescence quenching and conformational changes of trypsin resulted from the formation of a DMP–trypsin complex, which was driven mainly by hydrophobic interactions. The molecular docking and trypsin activity assay showed that DMP primarily interacted with the catalytic triad of trypsin and led to the inhibition of trypsin activity. The dimensions of the individual trypsin molecules were found to become larger after binding with DMP by atomic force microscopy imaging. This study offers a comprehensive picture of DMP–trypsin interaction, which is expected to provide insights into the toxicological effect of DMP.

Effect of substrate nature on the electrochemical deposition of calcium-deficient hydroxyapatites

Science.gov (United States)

Gualdrón-Reyes, A. F.; Domínguez-Vélez, V.; Morales-Morales, J. A.; Cabanzo, R.; Meléndez, A. M.

2017-01-01

Calcium phosphates were obtained by reducing nitrate ions to produce hydroxide ions on TiO2/stainless steel and TiO2/titanium electrodes. TiO2 coatings on metallic substrates were prepared by sol-gel dip-coating method. The morphology of deposits was observed by FESEM. Chemical nature of calcium phosphate deposits was identified by Raman micro-spectroscopy and FESEM/EDS microanalysis. Electrochemical behavior of nitrate and nitrite reduction on stainless steel and titanium electrodes was studied by linear sweep voltammetry. In addition, voltammetric study of the calcium phosphate electrodeposition on both electrodes was performed. From these measurements was selected the potential to form a calcium phosphate. A catalytic current associated to nitrate reduction reaction was obtained for stainless steel electrode, leading to significant deposition of calcium phosphate. Ca/P ratio for both substrates was less than 1.67. The formation of calcium deficient hydroxyapatite was confirmed by Raman spectroscopy.

Voltammetric determination of heparin based on its interaction with ...

African Journals Online (AJOL)

... with the linear regression equation as ∆ip″ (nA) = 360.19 C (mg/L) + 178.88 (n = 15, γ = 0.998) and the detection limit as 0.28 mg/L (3σ). The effects of coexisting substances such as metal ions, amino acids on the determination of heparin were investigated and the results showed that this method had good selectivity.

Voltammetric Determination of Azidothymidine Using Silver Solid Amalgam Electrodes

Czech Academy of Sciences Publication Activity Database

Pecková, K.; Navrátil, Tomáš; Josypčuk, Bohdan; Moreira, J. C.; Leandro, K. Ch.; Barek, J.

2009-01-01

Roč. 21, č. 15 (2009), s. 1750-1757 ISSN 1040-0397 R&D Projects: GA ČR GA203/07/1195; GA AV ČR IAA400400806; GA MŠk(CZ) LC06035 Institutional research plan: CEZ:AV0Z40400503 Keywords : azidothymidine * Zidovudine * Silver solid amalgam electrode * Differential pulse voltammetry Subject RIV: CG - Electrochemistry Impact factor: 2.630, year: 2009

Speciation of cadmium in seawater - a direct voltammetric approach

International Nuclear Information System (INIS)

Helmers, E.

1994-01-01

The present report deals with differential pulse anodic stripping voltammetry (DPASV) applied for the analysis of cadmium in open ocean seawater. Evaluation of different Cd species can generate information about distribution and speciation of Cd in the open ocean. Distribution of Cd was investigated in surface waters of the Atlantic Ocean over a wide geographical range as well as in the water column. Surface water sampling on board the research vessel Polarstern was performed from the bow boom of the ship as well as with a snorkel system which allowed continuous sample-taking. Two different Cd species could be differentiated in the voltammograms. UV-irradiation experiments allowed the identification of an inorganic and organic Cd form, the latter caused by the association between Cd and organic matter as e.g. humic substances (HS). Atlantic ocean surface seawater normally contains between 2 and 4 ng organically complexed Cd/kg and no detectable inorganic Cd. Some areas however showed readings of up to 14 ng inorganic Cd/kg in addition. Water column samples exhibited an enrichment of inorganic Cd by depth. Occurrence of inorganic Cd at the surface could be related to specific oceanographical conditions. Together with analytical results of trace metal contents in the particulate phases of surface seawater, new aspects could be established about the biogeochemical cycling of Cd in the sea. (orig.)

Voltammetric determination of theophylline at a Nafion/multi-wall ...

Indian Academy of Sciences (India)

Administrator

tive anodic peak at around 1180 mV (vs SCE) in 0⋅01 mol/L H2SO4 medium (pH 1⋅8). In contrast with the bare ..... more than that of hydrogen ions participating in the electrode reaction. .... the peak current is just 15⋅0%, indicating good dura- bility of the .... Sadik O A, Land W H and Wang J 2003 Electroana- lysis. 15 1149.

Voltammetric Quantification of Paraquat and Glyphosate in Surface Waters

Directory of Open Access Journals (Sweden)

William Roberto Alza-Camacho

2016-09-01

Full Text Available The indiscriminate use of pesticides on crops has a negative environmental impact that affects organisms, soil and water resources, essential for life. Therefore, it is necessary to evaluate the residual effect of these substances in water sources. A simple, affordable and accessible electrochemical method for Paraquat and Glyphosate quantification in water was developed. The study was conducted using as supporting electrolyte Britton-Robinson buffer solution, working electrode of glassy carbon, Ag/AgCl as the reference electrode, and platinum as auxiliary electrode. Differential pulse voltammetry (VDP method for both compounds were validated. Linearity of the methods presented a correlation coefficient of 0.9949 and 0.9919 and the limits of detection and quantification were 130 and 190 mg/L for Paraquat and 40 and 50 mg/L for glyphosate. Comparison with the reference method showed that the electrochemical method provides superior results in quantification of analytes. Of the samples tested, a value of Paraquat was between 0,011 to 1,572 mg/L and for glyphosate it was between 0.201 to 2.777 mg/L, indicating that these compounds are present in water sources and that those may be causing serious problems to human health.

Voltammetric determination of leucovorin using silver solid amalgam electrode

Czech Academy of Sciences Publication Activity Database

Šelešovská, R.; Bandžuchová, L.; Navrátil, Tomáš; Chýlková, J.

2012-01-01

Roč. 60, JAN 2012 (2012), s. 375-383 ISSN 0013-4686 R&D Projects: GA AV ČR IAA400400806; GA ČR GAP206/11/1638 Institutional research plan: CEZ:AV0Z40400503 Keywords : leucovorin * voltammetry * amalgam electrode Subject RIV: CG - Electrochemistry Impact factor: 3.777, year: 2012

Drop amalgam voltammetric study of lead complexation by natural ...

African Journals Online (AJOL)

A study of inorganic complexation of lead using drop amalgam voltammetry is described. The study has been carried out in simulated salt lake water and at ionic strength of 7.35 M, the predetermined ionic strength of Lake Katwe. The complexation of lead with the simple ligands (Cl-, CO32-) created anodic waves and the ...

Electrochemical mechanism and kinetics studies of haloperidol and its assay in commercial formulations

International Nuclear Information System (INIS)

Ribeiro, Francisco W.P.; Soares, Janete E.S.; Becker, Helena; De Souza, Djenaine; Lima-Neto, Pedro de; Correia, Adriana N.

2011-01-01

The kinetics and mechanism for electrochemical reduction of haloperidol, a psychotherapeutic drug used in the treatment of schizophrenia, were studied using square wave and cyclic voltammetries allied to a hanging mercury drop electrode. The experimental and voltammetric parameters were optimized at 0.04 mol L -1 Brinton-Robinson buffer (pH 10), with a pulse potential frequency of 100 s -1 , a pulse amplitude of 30 mV and scan increment of 2 mV. Two well-defined peaks were observed, which exhibited properties of fast electron transfer with a strong adsorption process of reactants and products on the electrode surface. The first peak was related to a fast and reversible anion-radical formation originating from the reduction of the carbonyl group, and the second was related to the irreversible reduction of the anion-radical previously formed. Analytical parameters such as: linearity range, equation of the analytical curves, correlation coefficients, detection and quantification limits, recovery efficiency, and relative standard deviation for intraday and interday were compared to similar results obtained by use of the UV-vis spectrophotometry technique, and the analytical results obtained in commercial formulations show that the voltammetric procedure using a hanging mercury drop electrode is suitable for analyzing haloperidol in complex commercial formulation samples.

Extending the capability of forensic electrochemistry to the novel psychoactive substance benzylpiperazine

Directory of Open Access Journals (Sweden)

S.A. Waddell

2017-04-01

Full Text Available Benzylpiperazine (BZP is a novel psychoactive substance that is commonly abused in tablet form as an “ecstasy-type” drug. Electroanalysis offers genuine potential for field testing of bulk drug samples. This research is the first to investigate the viability of voltammetric analysis of BZP. Initial cyclic voltammetry in 0.1 M KCl showed an oxidative peak at a glassy carbon electrode for BZP at approximately 0.8 V (scan rate 205 mV s−1. Next an optimised electrode/electrolyte combination (viz. 80:20 W:W glassy carbon beads:nujol and pH 9.5, 40 mM, Britton-Robinson buffer was developed using K3Fe(CN6 to test the electrode material. The oxidation of BZP involves two electrons and two protons and a mechanism has been proposed. An anodic stripping square wave voltammetric method was optimised by factorial design with the conditions of deposition: −0.8 V for 135 s, and stripping: step height 10 mV, amplitude 50 mV and frequency 13 Hz. A limit of detection of 6 μM was achieved. The resolution against 3,4-methylenedioxymethylamphetamine (MDMA was also verified. Keywords: Voltammetry, Forensic, Controlled drugs, Benzylpiperazine, Ecstasy

Nanomolar simultaneous determination of tryptophan and melatonin by a new ionic liquid carbon paste electrode modified with SnO2-Co3O4@rGO nanocomposite.

Science.gov (United States)

Zeinali, Homa; Bagheri, Hasan; Monsef-Khoshhesab, Zahra; Khoshsafar, Hosein; Hajian, Ali

2017-02-01

This work describes the development of a new sensor for simultaneous determination of tryptophan and melatonin. The proposed sensor was an ionic liquid carbon paste electrode modified with reduced graphene oxides decorated with SnO 2 -Co 3 O 4 nanoparticles. The voltammetric oxidation of the analytes by the proposed sensor confirmed that the electrooxidation process undergoes a two-electron/one-proton reaction for melatonin and a two-electron/two-proton reaction for tryptophan in diffusion-controlled processes. Moreover, based on the excellent electrochemical properties of the modified electrode, a sensitive voltammetric method was used for individual and simultaneous determination of melatonin and tryptophan in the aqueous solutions. Under the optimized experimental conditions, a linear response obtained in the range of 0.02 to 6.00μmolL -1 with detection limits of 4.1 and 3.2nmolL -1 for melatonin and tryptophan, respectively. The prepared sensor possessed accurate and rapid response toward melatonin and tryptophan with a good sensitivity, selectivity, stability, and repeatability. Finally, the applicability of the proposed sensor was verified by evaluation of melatonin and tryptophan in various real samples including human serum and tablet samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Performance of electrodes synthesized with polyacrylonitrile-based carbon nanofibers for application in electrochemical sensors and biosensors

Energy Technology Data Exchange (ETDEWEB)

Adabi, Mahdi [Department of Medical Nanotechnology, School of Advanced Technologies in Medicine, Tehran University of Medical Sciences, Tehran (Iran, Islamic Republic of); Saber, Reza [Department of Medical Nanotechnology, School of Advanced Technologies in Medicine, Tehran University of Medical Sciences, Tehran (Iran, Islamic Republic of); Center of Excellence in Electrochemistry, Faculty of Chemistry, University of Tehran, Tehran (Iran, Islamic Republic of); Faridi-Majidi, Reza, E-mail: refaridi@sina.tums.ac.ir [Department of Medical Nanotechnology, School of Advanced Technologies in Medicine, Tehran University of Medical Sciences, Tehran (Iran, Islamic Republic of); Center of Excellence in Electrochemistry, Faculty of Chemistry, University of Tehran, Tehran (Iran, Islamic Republic of); Faridbod, Farnoush [Science and Technology in Medicine (RCSTIM), Tehran University of Medical Sciences, Tehran, Iran. (Iran, Islamic Republic of)

2015-03-01

The purpose of this work was to investigate the performance of electrodes synthesized with Polyacrylonitrile-based carbon nanofibers (PAN-based CNFs). The homogenous PAN solutions with different concentrations were prepared and electrospun to acquire PAN nanofibers and then CNFs were fabricated by heat treatment. The effective parameters for the production of electrospun CNF electrode were investigated. Scanning electron microscopy (SEM) was used to characterize electrospun nanofibers. Cyclic voltammetry was applied to investigate the changes of behavior of electrospun CNF electrodes with different diameters. The structure of CNFs was also evaluated via X-ray diffraction (XRD) and Raman spectroscopy. The results exhibited that diameter of nanofibers reduced with decreasing polymer concentration and applied voltage and increasing tip-to-collector distance, while feeding rate did not have significant effect on nanofiber diameter. The investigations of electrochemical behavior also demonstrated that cyclic voltammetric response improved as diameter of CNFs electrode decreased. - Highlights: • Electrospun CNFs can be directly used as working electrode. • Cyclic voltammetric response improved as diameter of CNFs electrode decreased. • The diameter of nanofibers reduced with decreasing polymer concentration. • The diameter of nanofibers reduced with decreasing applied voltage. • The diameter of nanofibers reduced with increasing tip-to-collector distance.

Performance of electrodes synthesized with polyacrylonitrile-based carbon nanofibers for application in electrochemical sensors and biosensors

International Nuclear Information System (INIS)

Adabi, Mahdi; Saber, Reza; Faridi-Majidi, Reza; Faridbod, Farnoush

2015-01-01

The purpose of this work was to investigate the performance of electrodes synthesized with Polyacrylonitrile-based carbon nanofibers (PAN-based CNFs). The homogenous PAN solutions with different concentrations were prepared and electrospun to acquire PAN nanofibers and then CNFs were fabricated by heat treatment. The effective parameters for the production of electrospun CNF electrode were investigated. Scanning electron microscopy (SEM) was used to characterize electrospun nanofibers. Cyclic voltammetry was applied to investigate the changes of behavior of electrospun CNF electrodes with different diameters. The structure of CNFs was also evaluated via X-ray diffraction (XRD) and Raman spectroscopy. The results exhibited that diameter of nanofibers reduced with decreasing polymer concentration and applied voltage and increasing tip-to-collector distance, while feeding rate did not have significant effect on nanofiber diameter. The investigations of electrochemical behavior also demonstrated that cyclic voltammetric response improved as diameter of CNFs electrode decreased. - Highlights: • Electrospun CNFs can be directly used as working electrode. • Cyclic voltammetric response improved as diameter of CNFs electrode decreased. • The diameter of nanofibers reduced with decreasing polymer concentration. • The diameter of nanofibers reduced with decreasing applied voltage. • The diameter of nanofibers reduced with increasing tip-to-collector distance