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Film Electrode (film + electrode)
Selected AbstractsDetermination of Diazepam, Temazepam and Oxazepam at the Lead Film Electrode by Adsorptive Cathodic Stripping VoltammetryELECTROANALYSIS, Issue 17-18 2010Katarzyna Tyszczuk Abstract The determination of psychoactive 1,4-benzodiazepine drugs is of relevant interest in clinical, biomedical areas. Therefore a highly sensitive and simple voltammetric method for the determination of temazepam, diazepam and oxazepam at an in situ plated lead film electrode was developed. The method was successfully applied to the determination of diazepam and temazepam in pharmaceutical formulations with minimum sample manipulation and oxazepam in human urine samples without any separation steps. The determinations of oxazepam in human urine samples were performed in a flow system. Therefore a previous extraction procedure was not necessary to separate the active compound before its determination. [source] Simultaneous Determination of Trace Zinc(II) and Cadmium(II) by Differential Pulse Anodic Stripping Voltammetry Using a MWCNTs,NaDBS Modified Stannum Film ElectrodeELECTROANALYSIS, Issue 23 2009Qing Tian Abstract A multiwalled carbon nanotubes,sodium dodecyl benzene sulfonate (MWCNTs,NaDBS) modified stannum film electrode was employed for the determination of cadmium(II) and zinc(II). The Sn/MWCNTs-NaDBS film electrode was prepared by applying MWCNTs,NaDBS suspension to the surface of the GCE, while the Sn film was plated in situ simultaneously with the target metal ions. Under optimal conditions, linear calibration curves were obtained in a range of 5.0 ,100.0,,g L,1 with detection limits of 0.9,,g L,1 for zinc(II) and 0.8,,g L,1 for cadmium(II), respectively. This film electrode was successfully applied to the determination of Zn(II) and Cd(II) in tap water sample. [source] Properties of Poly(sodium 4-styrenesulfonate)-Ionic Liquid Composite Film and Its Application in the Determination of Trace Metals Combined with Bismuth Film ElectrodeELECTROANALYSIS, Issue 5 2008Jianbo Jia Abstract A new kind of bismuth film modified electrode to sensitively detect trace metal ions based on incorporating highly conductive ionic liquids 1-butyl-3-methyl-imidazolium hexafluorophosphate (BMIMPF6) in solid matrices at glassy carbon (GC) was investigated. Poly(sodium 4-styrenesulfonate) (PSS), silica, and Nafion were selected as the solid matrices. The electrochemical properties of the mixed films modified GC were evaluated. The electron transfer rate of Fe(CN)64,/Fe(CN)63, can be effectively improved at the PSS-BMIMPF6 modified GC. The bismuth modified PSS-BMIMPF6 composite film electrodes (GC/PSS-BMIMPF6/BiFEs) displayed high mechanical stability and sensitive stripping voltammetric performances for the determination of trace metal cations. The GC/PSS-BMIMPF6/BiFE exhibited well linear response to both Cd(II) and Pb(II) over a concentration range from 1.0 to 50,,g L,1. And the detection limits were 0.07,,g L,1 for Cd(II) and 0.09,,g L,1 for Pb(II) based on three times the standard deviation of the baseline with a preconcentration time of 120,s, respectively. Finally, the GC/PSS-BMIMPF6/BiFEs were successfully applied to the determination of Cd(II) and Pb(II) in real sample, and the results of present method agreed well with those of atomic absorption spectroscopy. [source] A Cobalt Film Electrode for Nitrite Determination in Natural WaterELECTROANALYSIS, Issue 24 2007Koïkoï Soropogui Abstract In this study a cobalt film electrodeposited on a copper disk (Ø=3.1,mm) was tested as electrode to measure nitrite ions in raw water. This electrode was able to determine the nitrite ions concentration in nondeaerated synthetic media and in natural water. The electrode reached a detection limit of 0.2,,mol L,1 and has a linear concentration range of 0.4 to 2,,mol L,1 NO2,. The influence of several ions such as NO3,, Cl,, SO42,, Mg2+, HCO3, and NH4+ was also tested. The electrode was used to determine the concentration of nitrite ions in a real sample. [source] Voltammetric Determination of Mercury(II) at Poly(3-hexylthiophene) Film Electrode.ELECTROANALYSIS, Issue 24 2007Effect of Halide Ions Abstract The well-known method for the determination of mercury(II), which is based on the anodic stripping voltammetry of mercury(II), has been adapted for applications at the thin film poly(3-hexylthiophene) polymer electrode. Halide ions have been found to increase the sensitivity of the mercury response and shift it more positive potentials. This behavior is explained by formation of mercuric halide which can be easily deposited and stripped from the polymer electrode surface. The procedure was optimized for mercury determination. For 120,s accumulation time, detection limit of 5,ng mL,1 mercury(II) has been observed. The relative standard deviation is 1.3% at 40,ng mL,1 mercury(II). The performance of the polymer film studied in this work was evaluated in the presence of surfactants and some potential interfering metal ions such as cadmium, lead, copper and nickel. [source] Electrocatalytic Reduction of Nitrite Ion on a Toluidine Blue Sol-Gel Thin Film Electrode Derived from 3-Aminopropyl Trimethoxy SilaneELECTROANALYSIS, Issue 22 2007K. Thenmozhi Abstract An organically modified sol-gel electrode using 3-aminopropyltrimethoxy silane for covalent immobilization of a redox mediator namely toluidine blue has been reported. Cyclic voltammetric characterization of the modified electrode in the potential range of 0.2,V to ,0.6,V exhibited stable voltammetric behavior in aqueous supporting electrolyte with a formal potential of ,0.265,V vs. SCE, corresponding to immobilized toluidine blue. The electrocatalytic activity of the modified electrode when tested towards nitrite ion exhibited a favorable response with the electrocatalytic reduction of nitrite occurring at a reduced potential of ,0.34,V. A good linear working range from 2.94×10,6,M to 2.11×10,3,M with a detection limit of 1.76×10,6,M and quantification limit of 5.87×10,6,M was obtained for nitrite determination. The stable and quick response (4,s) of the modified electrode towards nitrite under hydrodynamic conditions shows the feasibility of using the present sensor in flow systems. Significant improvements in the operational stability by overcoming the leachability problem and repeatability with a relative standard deviation of 1.8% of the TB thin film sensor have been obtained by the strategy of immobilization of the mediator in the sol-gel matrix. [source] Bismuth Film Electrode as an Alternative for Mercury Electrodes: Determination of Azo Dyes and Application for Detection in Food StuffsELECTROANALYSIS, Issue 21 2007Benoît Claux Abstract Bismuth electrodes were investigated and exhibit electrochemical properties similar to mercury electrodes but with much lower toxicity. An electrochemical application of bismuth film modified glassy carbon electrode for azo dyes determination was investigated. The plating step was optimized in order to achieve its analytical efficiency. A plating potential of ,0.9,V in a solution of 200,mg/L Bi(NO3)3, 0.5,M HNO3 for 100,s yields to a suitable electrode (in terms of stability and detection). Azo dyes such as azorubine (i.e., carmoisine, E122), amaranth (E123), ponceau 4R (i.e., new coccine, E124) and allura red (E129) were determined by differential pulse voltammetry in a NaCl solution in the concentration range of few ppm to 100 ppm. The reproducibility of the signal, characterized by the relative standard deviation, was found to be less than 5%, the detection and quantification limits were few mg/L. The influence of other food components on the signal was studied and the applicability was tested on real beverages samples. [source] Silver Amalgam Film Electrode of Prolonged Application in Stripping ChronopotentiometryELECTROANALYSIS, Issue 18 2007Kapturski Abstract The utility of the cylindrical silver-based mercury film electrode of prolonged analytical application in stripping chronopotentiometry (SCP) was examined. This electrode allowed us to obtain good reproducibility of results owing to the special electrode design, which enables regeneration of the thin layer before each measurement cycle. The accessible potential window in KNO3 (pH,2), acetate and ammonia buffers was defined, and the optimal conditions (i.e., stripping current, deposition potential and deposition time) for the determination of Cd and Pb traces were selected. The detection limits, obtained for an accumulation time of 60,s, were 0.023,,g/L for Cd and 0.075,,g/L for Pb. The response increases linearly with Cd, Pb and Zn concentration, up to at least 100,,g/L. It was also shown that the proposed procedure ensures excellent separation of the In and Tl, Pb and Tl or the In and Cd signals. The method was tested with dolomite and lake sediment samples, and good agreement with reference values was achieved. The obtained results showed good reproducibility (RSD=5,6%) and reliability. [source] Fast Simultaneous Adsorptive Stripping Voltammetric Determination of Ni(II) and Co(II) at Lead Film Electrode Plated on Gold SubstrateELECTROANALYSIS, Issue 14 2007Katarzyna Tyszczuk Abstract A fast adsorptive stripping voltammetric procedure for simultaneous determination of Ni(II) and Co(II) in the presence of nioxime as a complexing agent at an in situ plated lead film electrode was described. The time of determination of these ions was shortened due to the application of gold as a substrate for lead film. At gold substrate lead film formation and accumulation of Ni(II) and Co(II) complexes with nioxime proceeds simultaneously. To obtain a stable signals for both ions a simple procedure of activation of the electrode was proposed. Calibration graphs for an accumulation time of 20,s were linear from 5×10,9 to 1×10,7 mol L,1 and from 5×10,10 to 1×10,8 mol L,1 for Ni(II) and Co(II), respectively. The procedure with the application of a lead film electrode on a gold substrate was validated in the course of Ni(II) and Co(II) determination in certified reference materials. [source] DNA Determination in the Presence of Copper in Diluted Alkaline Electrolyte by Adsorptive Stripping Voltammetry at the Mercury Film ElectrodeELECTROANALYSIS, Issue 11 2007Augusto, Mardini Farias, Percio Abstract A stripping method for the determination of single-stranded DNA in presence of copper at the submicromolar concentration levels is described. The method is based on controlled adsorptive accumulation of adenine (from acid-treated DNA) at thin-film mercury electrode followed by linear scan voltammetry measurement of the surface species. Optimum experimental conditions were found to be the use of a 5.0×10,3,M NaOH solution, an accumulation potential of ,0.40,V and a scan rate of 200,mV s,1. The response of adenine,copper is linear over the concentration range 50,250,ppb. For an accumulation time of 15,minutes, the detection limit was found to be 4,ppb. The more convenient relation to measuring the ssDNA in presence of metals and nitrogenated bases were also investigated. The utility of the method is demonstrated by the presence of adenosine-triphosphate (ATP) and amino acids. [source] Enhanced Resolution of Copper and Bismuth by Addition of Gallium in Anodic Stripping Voltammetry with the Bismuth Film ElectrodeELECTROANALYSIS, Issue 24 2006Chad Prior Abstract This paper presents the enhanced analysis of copper on a bismuth electrode upon addition of gallium(III). The presence of gallium alleviates the problems of overlapping stripping signals usually observed between copper and bismuth when using the Bismuth Film Electrode. In addition, it has been found that the presence of gallium improves the reproducibility of the bismuth stripping signal. Simultaneous deposition of copper and bismuth at ,1500,mV for 2,minutes in a supporting electrolyte composed of 0.1,M pH,4.75 acetate buffer with 250,,g L,1 gallium yields well resolved copper and bismuth signals when analyzed with square-wave anodic stripping voltammetry. Simultaneous analysis of copper and lead yielded linear calibration plots in the range 10 to 100,,g L,1 with regression coefficients of 0.997 and 0.994 respectively. The theoretical detection limit for copper was calculated to be 4.98,,g L,1 utilizing a 2,minutes deposition time. The relative standard deviation for a copper concentration of 50,,g L,1 was 1.6% (n=10). [source] Electrochemical Deposition and Properties of Nanometer-structure Ce-doped Lead Dioxide Film ElectrodeCHINESE JOURNAL OF CHEMISTRY, Issue 1 2005Shi-Yun Al Abstract The effect of Ce(III) on the morphology and structure of deposited film of lead dioxide was studied by cyclic voltammetry (CV), X-ray diffractometry (XRD) and scanning tunneling microscopy (STM). The results indicated that the Ce-doped PbO2 film consisted of a mixture of , - and , -phase of PbO2. Ce doping changed the size of PbO2 crystal grains and made the crystallite size on the electrode surface in the nanometer range. Owing to the formation of nanometer-structured grains, the specific surface areas and activity sites of the electrode surface were increased, hence the catalytic activity of Ce-doped PbO2 electrode was evidently higher than that of undoped PbO2 electrode. [source] Directly Heated Bismuth Film Electrodes Based on Gold MicrowiresELECTROANALYSIS, Issue 13 2010Martin Jacobsen Abstract As a nontoxic substitute for mercury electrodes, bismuth electrodes attained a lot of attention during the last years. In this report we describe for the first time the preparation of two different directly heatable bismuth-modified microwire electrodes. We characterized the electrochemical behaviour using cyclic voltammetry in acetate buffer and alkaline tartrate solution. The bismuth electrodes show a significantly wider potential window compared with bare gold wires. In the presence of picric acid as one example for the detection of explosives, the bismuth electrodes deliver higher signals. By applying heat during the measurements, the signals can be enhanced further. We used the temperature pulse amperometry (TPA) technique to improve the electrochemical response at the different types of electrodes. In this preliminary study, we were able to detect 3,ppm traces of picric acid. [source] Electrocatalytic Reduction and Determination of Iodate and Periodate at Silicomolybdate-Incorporated-Glutaraldehyde- Cross-Linked Poly- L -lysine Film ElectrodesELECTROANALYSIS, Issue 10 2010Yu-Ching Pan Abstract The present work describes reduction of iodate (IO3,), and periodate (IO4,) at silicomolybdate-doped-glutaraldehyde-cross-linked poly- L -lysine (PLL-GA-SiMo) film coated glassy carbon electrode in 0.1,M H2SO4. In our previous study, we were able to prepare the PLL-GA-SiMo film modified electrode by means of electrostatically trapping SiMo12O404, mediator in the cationic film of PLL-GA, and the voltammetric investigation in pure supporting indicated that the charge transport through the film was fast. Here, the electrocatalytic activity of PLL-GA-SiMo film electrode towards iodate and periodate was tested and subsequently used for analytical determination of these analytes by amperometry. The two electron reduced species of SiMo12O404, anion was responsible for the electrocatalytic reduction of IO3, at PLL-GA-SiMo film electrode while two and six electron reduced species were showed electrocatalytic activity towards IO4, reduction. Under optimized experimental conditions of amperometry, the linear concentration range and sensitivity are 2.5×10,6 to 1.1×10,2,M and 18.47,,A mM,1 for iodate, and 5×10,6 to 1.43×10,4,M and 1014.7,,A mM,1 for periodate, respectively. [source] Renewable Copper and Silver Amalgam Film Electrodes of Prolonged Application for the Determination of Elemental Sulfur Using Stripping VoltammetryELECTROANALYSIS, Issue 7 2008Robert Piech Abstract New, renewable copper (Hg(Cu)FE) and silver (Hg(Ag)FE) based amalgam film electrodes applied for the determination of elemental sulfur using differential pulse cathodic stripping voltammetry are presented. With surface areas adjustable from 1 to 12,mm2, both electrodes are characterized by very good surface reproducibility (,2%) and long-term stability (a few thousand measurement cycles). The mechanical refreshing of the amalgam film takes about 1,2 seconds. The effects of various factors such as instrumental parameters and the supporting electrolyte composition were optimized. Interferences from sulfides are easily removed by the addition of acid, and bubbling with argon, for Hg(Ag)FE. In the case of Hg(Cu)FE, sulfides did not interfere. The calibration graph is linear within the studied range from 16,ng L,1 to 4.8,,g L,1 for Hg(Cu)FE, and up to 6.4,,g L,1 for Hg(Ag)FE (tacc=15,s). The correlation coefficients for the two electrodes were at least 0.997. The detection limits for a low concentration of S(0) and tacc=60,s are as low as 14,ng L,1 for Hg(Cu)FE and 4,ng L,1 for Hg(Ag)FE. The proposed method was successfully applied and validated by studying the recovery of S(0) from spiked river water. [source] Development of Novel Glucose and Pyruvate Biosensors at Poly(Neutral Red) Modified Carbon Film Electrodes.ELECTROANALYSIS, Issue 8 2006Application to Natural Samples Abstract Amperometric biosensors based on the corresponding oxidase enzyme with poly(neutral red) redox mediator have been developed for the determination of glucose and pyruvate. The enzymes have been immobilized on top of poly(neutral red) modified carbon film electrodes with glutaraldehyde as the cross-linking agent. The biosensors were characterized by cyclic voltammetry and by electrochemical impedance spectroscopy. The glucose biosensor exhibited a linear response in the range 90,,M to 1.8,mM with a detection limit of 22,,M and the pyruvate biosensor in the range 90 to 600,,M with a detection limit of 34,,M. The relative standard deviations were found to be 2.1% (n=3) and 2.8% (n=4) respectively. The interference effects of various compounds were also studied. The glucose content of several types of wine and the amount of pyruvate in onion and garlic were determined and the results were compared with those obtained by standard spectrophotometric methods. [source] Trace Determination of Chromium by Square-Wave Adsorptive Stripping Voltammetry on Bismuth Film ElectrodesELECTROANALYSIS, Issue 21 2004Eleni Chatzitheodorou Abstract This works reports the use of adsorptive stripping voltammetry (AdSV) for the trace determination of chromium on a rotating-disk bismuth-film electrode (BFE). During the reductive accumulation step, all the chromium species in the sample were reduced to Cr(III) which was complexed with cupferron and the complex was accumulated by adsorption on the surface of a preplated BFE. The stripping step was carried out by using a square-wave (SW) potential-time voltammetric signal. Electrochemical cleaning of the bismuth film was employed, enabling the same bismuth film to be used for a series of measurements in the presence of dissolved oxygen. The experimental variables as well as potential interferences were investigated and the figures of merit of the method were established. Using the selected conditions, the 3, limit of detection for chromium was 100,ng L,1 (for 120,s of preconcentration) and the relative standard deviation was 3.6% at the 2,,g L,1 level (n=8). Finally, the method was applied to the determination of chromium in real samples with satisfactory results. [source] Electrodeposition of Lead at Boron-Doped Diamond Film Electrodes: Effect of TemperatureELECTROANALYSIS, Issue 12 2003César Prado Abstract The electrodeposition of lead on boron-doped diamond has been studied with a view to identifying the fundamental parameters controlling the sensitivity and lower detection limit in anodic stripping voltammetry. Chronoamperometric transients are used to explore the deposition, indicating a progressive growth mechanism confirmed by ex situ AFM images. Linear sweep ASV experiments show a threshold concentration of ca 10,6,M below which no lead is detected; this is attributed to the need for nucleation of the solid phase on the electrode. Experiments with variable temperature show that this threshold can be usefully lowered at elevated temperatures. [source] Nanodiamond Thin Film Electrodes: Metal Electro-Deposition and Stripping ProcessesELECTROANALYSIS, Issue 3 2003Hian, Lau Chi Abstract The properties of a nanodiamond thin film deposit formed on titanium substrates in a microwave-plasma enhanced CVD process, are investigated for applications in electroanalysis. The nanodiamond deposit consists of intergrown nano-sized platelets of diamond with a high sp2 carbon content giving it high electrical conductivity and electrochemical reactivity. Nanodiamond thin film electrodes (of approximately 2,,m thickness) are characterized by electron microscopy and electrochemical methods. First, for a reversible one electron redox system, Ru(NH3)63+/2+, nanodiamond is shown to give well-defined diffusion controlled voltammetric responses. Next, metal deposition processes are shown to proceed on nanodiamond with high reversibility and high efficiency compared to processes reported on boron-doped diamond. The nucleation of gold is shown to be facile at edge sites, which are abundant on the nanodiamond surface. For the deposition and stripping of both gold and copper, a stripping efficiency (the ratio of electro-dissolution charge to electro-deposition charge) of close to unity is detected even at low concentrations of analyte. The effect of thermal annealing in air is shown to drastically modify the electrode characteristics probably due to interfacial oxidation, loss of active sp2 sites, and loss of conductivity. [source] Enhancement of Anodic Response for DMSO at Ruthenium Oxide Film Electrodes as a Result of Doping with Iron(III)ELECTROANALYSIS, Issue 2 2003Brett Abstract The oxidation of dimethyl sulfoxide (DMSO) to dimethyl sulfone (DMSO2) is representative of numerous anodic oxygen-transfer reactions of organosulfur compounds that suffer from slow kinetics at noble metal electrodes. Anodic voltammetric data for DMSO are examined at various RuO2 -film electrodes prepared by thermal deposition on titanium substrates. The response for DMSO is slightly larger at RuO2 films prepared in a flame as compared with films prepared in a furnace; however, temperature is more easily controlled in the furnace. Doping of the RuO2 films with Fe(III) further improves the sensitivity of anodic response for DMSO. Optimal response is obtained at an Fe(III)-doped RuO2 -film electrode prepared using a deposition solution of 50,mM RuCl3 and 10,mM FeCl3 in a 1,:,1 mixture of isopropanol and 12,M HCl at an annealing temperature of 450,°C. The Levich plot (i vs. ,1/2) and Koutecky-Levich plot (1/i vs. 1/,1/2) of amperometric data for the oxidation of DMSO at an Fe(III)-doped RuO2 -film electrode configured as a rotated disk are consistent with an anodic response controlled by mass-transport processes at low rotational velocities. Flow injection data demonstrate that Fe(III)-doped RuO2 -film electrodes exhibit detection capability for methionine and cysteine in addition to DMSO. Detection limits for 100-,L injections of the three compounds are ca. 3.2×10,4,mM, i.e., ca. 32,pmol. [source] Determination of Diazepam, Temazepam and Oxazepam at the Lead Film Electrode by Adsorptive Cathodic Stripping VoltammetryELECTROANALYSIS, Issue 17-18 2010Katarzyna Tyszczuk Abstract The determination of psychoactive 1,4-benzodiazepine drugs is of relevant interest in clinical, biomedical areas. Therefore a highly sensitive and simple voltammetric method for the determination of temazepam, diazepam and oxazepam at an in situ plated lead film electrode was developed. The method was successfully applied to the determination of diazepam and temazepam in pharmaceutical formulations with minimum sample manipulation and oxazepam in human urine samples without any separation steps. The determinations of oxazepam in human urine samples were performed in a flow system. Therefore a previous extraction procedure was not necessary to separate the active compound before its determination. [source] Electrocatalytic Reduction and Determination of Iodate and Periodate at Silicomolybdate-Incorporated-Glutaraldehyde- Cross-Linked Poly- L -lysine Film ElectrodesELECTROANALYSIS, Issue 10 2010Yu-Ching Pan Abstract The present work describes reduction of iodate (IO3,), and periodate (IO4,) at silicomolybdate-doped-glutaraldehyde-cross-linked poly- L -lysine (PLL-GA-SiMo) film coated glassy carbon electrode in 0.1,M H2SO4. In our previous study, we were able to prepare the PLL-GA-SiMo film modified electrode by means of electrostatically trapping SiMo12O404, mediator in the cationic film of PLL-GA, and the voltammetric investigation in pure supporting indicated that the charge transport through the film was fast. Here, the electrocatalytic activity of PLL-GA-SiMo film electrode towards iodate and periodate was tested and subsequently used for analytical determination of these analytes by amperometry. The two electron reduced species of SiMo12O404, anion was responsible for the electrocatalytic reduction of IO3, at PLL-GA-SiMo film electrode while two and six electron reduced species were showed electrocatalytic activity towards IO4, reduction. Under optimized experimental conditions of amperometry, the linear concentration range and sensitivity are 2.5×10,6 to 1.1×10,2,M and 18.47,,A mM,1 for iodate, and 5×10,6 to 1.43×10,4,M and 1014.7,,A mM,1 for periodate, respectively. [source] Simultaneous Determination of Trace Zinc(II) and Cadmium(II) by Differential Pulse Anodic Stripping Voltammetry Using a MWCNTs,NaDBS Modified Stannum Film ElectrodeELECTROANALYSIS, Issue 23 2009Qing Tian Abstract A multiwalled carbon nanotubes,sodium dodecyl benzene sulfonate (MWCNTs,NaDBS) modified stannum film electrode was employed for the determination of cadmium(II) and zinc(II). The Sn/MWCNTs-NaDBS film electrode was prepared by applying MWCNTs,NaDBS suspension to the surface of the GCE, while the Sn film was plated in situ simultaneously with the target metal ions. Under optimal conditions, linear calibration curves were obtained in a range of 5.0 ,100.0,,g L,1 with detection limits of 0.9,,g L,1 for zinc(II) and 0.8,,g L,1 for cadmium(II), respectively. This film electrode was successfully applied to the determination of Zn(II) and Cd(II) in tap water sample. [source] A New Indirect Electroanalytical Method to Monitor the Contamination of Natural Waters with 4-Nitrophenol Using Multiwall Carbon NanotubesELECTROANALYSIS, Issue 9 2009Cruz Moraes, Fernando Abstract The electrochemical detection of the hazardous pollutant 4-nitrophenol (4-NP) at low potentials, in order to avoid matrix interferences, is an important research challenge. This study describes the development, electrochemical characterization and utilization of a multiwall carbon nanotube (MWCNT) film electrode for the quantitative determination of 4-NP in natural water. Electrochemical impedance spectroscopy measurements showed that the modified surface exhibits a decrease of ca. 13 times in the charge transfer resistance when compared with a bare glassy carbon (GC) surface. Voltammetric experiments showed the possibility to oxidize a hydroxylamine layer (produced by the electrochemical reduction of 4-NP on the GC/MWNCT surface) in a potential region which is approximately 700,mV less positive than that needed to oxidize 4-NP, thus minimizing the interference of matrix components. The limit of detection for 4-NP obtained using square-wave voltammetry (0.12,,mol L,1) was lower than the value advised by EPA. A natural water sample from a dam located in São Carlos (Brazil) was spiked with 4-NP and analyzed by the standard addition method using the GC/MWCNT electrode, without any further purification step. The recovery procedure yielded a value of 96.5% for such sample, thus confirming the suitability of the developed method to determine 4-NP in natural water samples. The electrochemical determination was compared with that obtained by HPLC with UV-vis detection. [source] Electrochemical Properties of Ordered Mesoporous Carbon Film Adsorbed onto a Self-Assembled Alkanethiol Monolayer on Gold ElectrodeELECTROANALYSIS, Issue 2 2009Dan Zheng Abstract A stable ordered mesoporous carbon (OMC) film electrode was successfully constructed by adsorbing OMC onto a self-assembled monolayer (SAM) of C18H37SH chemisorbed on the Au electrode. Transmission electron microscopy (TEM), atomic force microscopy (AFM), and electrochemical methods were used to characterize the properties of the OMC film electrode. The adsorbed OMC can restore the heterogeneous electron transfer almost totally blocked by the alkanethiol monolayer. Nyquist plots show a sharply decrease of the charge transfer resistance (Rct) of the Fe(CN) couple at the OMC film electrode. Furthermore, the OMC film electrode is found to possess a significantly reduced interfacial capacitance and largely enhanced current response of hydrogen peroxide. This novel approach to the fabrication of stable OMC film electrode with excellent electrochemical properties is believed to be very attractive for electrochemical studies and electroanalytical applications. [source] Preparation of Nanogapped Gold Nanoparticle Array for DNA DetectionELECTROANALYSIS, Issue 4 2008Shiho Tokonami Abstract A novel DNA detection technique using a gold nanoparticle array film electrode has been reported here. The gold nanoparticles molecularly linked with binder molecule (1,10-decanedithiol) were separated 1.3,nm from each other, and the DNA conductivity change from single to double strand was measured by monitoring a voltage drop across the particles, between which a probe of a 12-mer oligonucleotide was immobilized. In adding a complementary oligonucleotide on the nanoparticle film chip, an immediate decrease in the film resistance (ca. 1.4 ,) due to a hybridization event occurred in a reproducible manner with this simple setup. In the paper, we have an interest in the primary sensing properties; effect of the film resistance on the sensor response, dependence of the resistance change on the DNA concentration, and the performance of the system for DNA detection including single nucleotide polymorphisms were described. [source] Silver Amalgam Film Electrode of Prolonged Application in Stripping ChronopotentiometryELECTROANALYSIS, Issue 18 2007Kapturski Abstract The utility of the cylindrical silver-based mercury film electrode of prolonged analytical application in stripping chronopotentiometry (SCP) was examined. This electrode allowed us to obtain good reproducibility of results owing to the special electrode design, which enables regeneration of the thin layer before each measurement cycle. The accessible potential window in KNO3 (pH,2), acetate and ammonia buffers was defined, and the optimal conditions (i.e., stripping current, deposition potential and deposition time) for the determination of Cd and Pb traces were selected. The detection limits, obtained for an accumulation time of 60,s, were 0.023,,g/L for Cd and 0.075,,g/L for Pb. The response increases linearly with Cd, Pb and Zn concentration, up to at least 100,,g/L. It was also shown that the proposed procedure ensures excellent separation of the In and Tl, Pb and Tl or the In and Cd signals. The method was tested with dolomite and lake sediment samples, and good agreement with reference values was achieved. The obtained results showed good reproducibility (RSD=5,6%) and reliability. [source] Electrochemical Preparation of Poly(Malachite Green) Film Modified Nafion-Coated Glassy Carbon Electrode and Its Electrocatalytic Behavior Towards NADH, Dopamine and Ascorbic AcidELECTROANALYSIS, Issue 14 2007Shen-Ming Chen Abstract Poly(malachite green) film modified Nafion-coated glassy carbon electrodes have been prepared by potentiodynamic cycling in malachite green solution. The pH of polymerisation solution has only minor effect on film formation. Electrochemical quartz crystal microbalance (EQCM) was used to monitor the growth of the poly(malachite green) film. Cyclic voltammogram of the poly(malachite green) film shows a redox couple with well-defined peaks. The redox response of the modified electrode was found to be depending on the pH of the contacting solution. The peak potentials were shifted to a less positive region with increasing pH and the dependence of the peak potential was found to be 56,mV per pH unit. The electrocatalytic behavior of poly(malachite green) film modified Nafion-coated glassy carbon electrodes was tested towards oxidation of NADH, dopamine, and ascorbic acid. The oxidation of dopamine and ascorbic acid occurred at less positive potential on poly(malachite green) film compared to bare glassy carbon electrode. In the case of NADH, the overpotential was reduced substantially on modified electrode. Finally, the feasibility of utilizing poly(malachite green) film electrode in analytical estimation of ascorbic acid was demonstrated in flow injection analysis. [source] Fast Simultaneous Adsorptive Stripping Voltammetric Determination of Ni(II) and Co(II) at Lead Film Electrode Plated on Gold SubstrateELECTROANALYSIS, Issue 14 2007Katarzyna Tyszczuk Abstract A fast adsorptive stripping voltammetric procedure for simultaneous determination of Ni(II) and Co(II) in the presence of nioxime as a complexing agent at an in situ plated lead film electrode was described. The time of determination of these ions was shortened due to the application of gold as a substrate for lead film. At gold substrate lead film formation and accumulation of Ni(II) and Co(II) complexes with nioxime proceeds simultaneously. To obtain a stable signals for both ions a simple procedure of activation of the electrode was proposed. Calibration graphs for an accumulation time of 20,s were linear from 5×10,9 to 1×10,7 mol L,1 and from 5×10,10 to 1×10,8 mol L,1 for Ni(II) and Co(II), respectively. The procedure with the application of a lead film electrode on a gold substrate was validated in the course of Ni(II) and Co(II) determination in certified reference materials. [source] Preparation, Characterization and Electrocatalytic Studies on Copper Complex Dye Film Modified ElectrodesELECTROANALYSIS, Issue 13 2007Shen-Ming Chen Abstract Copper complex dye (C.I. Direct Blue 200) film modified electrodes have been prepared by multiple scan cyclic voltammetry. The effect of solution pH and nature of electrode material on film formation was investigated. The optimum pH for copper complex film formation on glassy carbon was found to be 1.5. The mechanism of film formation on ITO seems to be similar to that on GC surface but completely different mechanism followed with gold electrode. Cyclic voltammetric features of our modified electrodes are in consistent with a surface-confined redox process. The voltammetric response of modified electrode was found to be depending on pH of the contacting solution. UV-visible spectra show that the nature of copper complex dye is identical in both solution phase and after forming film on electrode. The electrocatalytic behavior of copper complex dye film modified electrode towards oxidation of dopamine, ascorbic acid and reduction of SO52, was investigated. The oxidation of dopamine and ascorbic acid occurred at less positive potential on film electrode compared to bare glassy carbon electrode. Feasibility of utilizing our modified electrode in analytical estimation of dopamine, ascorbic acid was also demonstrated. [source] | ||||||||||