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Accumulation Time (accumulation + time)
Selected AbstractsElectroanalysis of Bisphenol A at a Multiwalled Carbon Nanotubes-gold Nanoparticles Modified Glassy Carbon ElectrodeELECTROANALYSIS, Issue 22 2009Xinman Tu Abstract A sensitive electrochemical method was developed for the determination of bisphenol A (BPA) at a glassy carbon electrode (GCE) modified with a multiwalled carbon nanotubes (MWCNTs)-gold nanoparticles (GNPs) hybrid film, which was prepared based on the electrostatic interaction between positively charged cetyltrimethylammonium bromide (CTAB) and negatively charged MWCNTs and GNPs. The MWCNT-GNPs/GCE exhibited an enhanced electroactivity for BPA oxidation versus unmodified GCE and MWCNTs/GCE. The experimental parameters, including the amounts of modified MWCNTs and GNPs, the pH of the supporting electrolyte, scan rate and accumulation time, were examined and optimized. Under the optimal conditions, the differential pulse voltammetric anodic peak current of BPA was linear with the BPA concentration from 2.0×10,8 to 2×10,5 mol L,1, with a limit of detection of 7.5,nmol L,1. The proposed procedure was applied to determine BPA leached from real plastic samples with satisfactory results. [source] Renewable Ceramic (TiN) Ring Electrode in Stripping Voltammetry.ELECTROANALYSIS, Issue 16 2009Determination of Pb(II) Without Removal of Oxygen Abstract Characteristic features of the process of Pb(II) reduction and oxidation at a renewable ceramic ring electrode (RCRE) were studied by stripping voltammetry. The main constituents of the RCRE are: a specially constructed TiN ring electrode, a silver sheet used as silver counter/quasi-reference electrode and a silicon O-ring are fastened together in a polypropylene body. The renovation of this electrode is carried out through mechanical removal of solid contaminants and electrochemical activation in the electrolyte which fills the RCRE body. The optimal measurement conditions, composition of supporting electrolyte and procedures of the electrode activation were selected. The measurements were carried out from nondeaerated solutions. As shown on selected examples, RCRE exhibits good performance in underpotential deposition stripping voltammetry (UPD-SV) applied for the determination of lead(II) in synthetic solutions with and without surfactants and in certified reference materials. The peak current is proportional to the concentration of lead(II) over the range 2×10,9,1×10,7,mol L,1, with a 3, detection limit of 1×10,9,mol L,1 with an accumulation time of 30,s. The obtained results showed good reproducibility, (RSD=2,5%; n=5) and reliability. [source] Voltammetric Detection of Lead(II) Using Amide-Cyclam- Functionalized Silica-Modified Carbon Paste ElectrodesELECTROANALYSIS, Issue 15 2009Stéphanie Goubert-Renaudin Abstract 2-(4,8,11-Triscarbamoylmethyl-1,4,8,11-tetraazacyclotetradec-1-yl)acetamide (TETAM) derivatives bearing 1, 2, or 4 silylated arms have been synthesized and grafted to the surface of silica gel and ordered mesoporous silica samples. The resulting organic-inorganic hybrids have been incorporated into carbon paste electrodes and applied to the preconcentration electroanalysis of Pb(II). The attractive recognition properties of these cyclam derivatives functionalized with amide pendent groups toward Pb(II) species and the highly porous structure of the adsorbents can be exploited for the selective and sensitive detection of the target analyte. Various parameters affecting the preconcentration and detection steps have been discussed with respect to the composition and pH of both accumulation and detection media, the nature of the adsorbent (number of silylated groups linking the macrocycle to silica, texture of materials), the accumulation time, and the presence of interfering cations. Under optimal conditions and for 2,min accumulation at open-circuit, the voltammetric response increased linearly with the Pb(II) concentration in a range extending from 2×10,7 to 10,5,M, while a longer accumulation time of 15,min afforded a linear calibration curve between 10,8 and 10,7,M with a detection limit of 2.7×10,9,M which is well below the European regulatory limit of lead in consumption water. [source] Voltammetric Reduction of a 4-Nitroimidazole Derivative on a Multiwalled Carbon Nanotubes Modified Glassy Carbon ElectrodeELECTROANALYSIS, Issue 13 2008P. Jara-Ulloa Abstract We report the electrochemical behavior of a 4-nitroimidazole derivative, 1-methyl-4-nitro-2-hydroxymethylimidazole (4-NImMeOH), on glassy carbon electrode (GCE) modified with multiwalled carbon nanotubes (MWCNT). As dispersing agents, dimethylformamide (DMF) and water were used. The electrochemical response of the resulting electrodes was evaluated using linear sweep, cyclic and square-wave voltammetry (LSV, CV and SWV). Several parameters such as medium pH, nature and concentration of the CNTs dispersion and accumulation time were tested. The optimal conditions determined for obtain better response were: pH,2, dispersion concentration=4,mg/mL of CNT in water, accumulation time=7,min. The MWCNT-modified GCE exhibited attractive electrochemical properties producing enhanced currents with a significant reduction in the overpotential and good signal-to-noise characteristics, in comparison with the bare GCE. The modified electrode is highly repeatable for consecutive measurements, reaching a variation coefficient of 2.9% for ten consecutive runs. [source] Simultaneous Determination of Nickel and Cadmium by Adsorptive Stripping VoltammetryELECTROANALYSIS, Issue 12 2008B. Gholivand Abstract A sensitive and fast method for the simultaneous determination of trace amounts of nickel and cadmium in real samples has been described using differential pulse adsorptive stripping voltammetry (DPASV) by adsorptive accumulation of the N,N,-bis(salicylaldehydo)4-carboxyphenylenediamine (BSCPDA),complex on the hanging mercury drop electrode (HMDE). As supporting electrolyte 0.02,mol L,1 ammonia buffers containing ligand has been used. Optimal analytical conditions were found to be: BSCPDA concentration of 42,,M, pH,9.6 and adsorption potential at ,50,mV versus Ag/AgCl. With an accumulation time of 20,s, the peaks current are proportional to the concentration of nickel and cadmium over the 1,180, and 0.5,200,ng mL,1 with detection limits of 0.06 and 0.03,ng mL,1 respectively. The sensitivity of method for determination of nickel and cadmium were obtained 0.54 and 0.98,nA mL ng,1, respectively. The procedure was applied to simultaneous determination of nickel and cadmium in some real and synthetic artificial samples with satisfactory results. [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] Study of Factors Affecting the Performance of Voltammetric Copper Sensors Based on Gly-Gly-His Modified Glassy Carbon and Gold ElectrodesELECTROANALYSIS, Issue 12 2006Guozhen Liu Abstract This paper reports a study of the factors affecting the analytical performance of gold and glassy carbon electrodes modified with the tripeptide Gly-Gly-His for the detection of copper ions. Gly-Gly-His is attached to a glassy carbon (GC) surface modified with 4-carboxyphenyl moieties or a gold surface modified with 3-mercaptopropionic acid by the reaction of the N-terminal amine group of the peptide with the carboxylic acid groups of the monolayer via carbodiimide activation. X-ray photoelectron spectroscopy was used to characterize the steps in the biosensor fabrication. It was found that the analytical performance of a sensor prepared with Gly-Gly-His on a GC electrode was similar to that on a gold electrode under the same conditions. The performance was greatly enhanced at higher temperature, no added salt during copper accumulation and longer accumulation time within a pH range of 7,9. Interference studies and investigations of stability of the Gly-Gly-His sensor are reported. Analysis of natural water samples show that the sensors measure only copper ions that can complex at the sensor surface. Strongly complexed copper in natural water is not measured. Despite greater stability of diazonium salt derived monolayers on carbon surfaces compared with alkanethiols self-assembled monolayers on gold, the stability of the sensors was essentially the same regardless of the modification procedure. [source] Catalytic Adsorptive Stripping Voltammetric Procedure for Determination of Total Chromium in Environmental MaterialsELECTROANALYSIS, Issue 12 2006gorzata Grabarczyk Abstract A sensitive catalytic adsorptive stripping voltammetric procedure for determination of traces of total chromium in environmental samples is reported. The method is based on the preconcentration of a Cr(III)H2DTPA complex by adsorption at the HMDE from an acetate buffer solution at the potential ,1.0,V vs. Ag/AgCl. Total chromium was determined as Cr(III) after reduction of Cr(VI) to Cr(III) by NaHSO3. In order to stabilize the signal of Cr(III) the measurements were performed at 5,°C. The calibration graph for chromium for an accumulation time of 60,s was linear in the range from 5×10,10 to 5×10,8,mol L,1. The relative standard deviation for a chromium concentration of 1×10,8,mol L,1 was 3.9% (n=5). The detection limit for accumulation time of 60,s was about 8×10,11,mol L,1. The validation of the procedure was performed by the analysis of the certified reference materials. [source] Highly Sensitive and Selective Measurement of Bismuth in Seawater and Drug with 1,2-Phenylenedioxydiacetic Acid by Cathodic Adsorptive Stripping VoltammetryELECTROANALYSIS, Issue 7 2006B. Gholivand Abstract A new method is presented for determination of bismuth based on cathodic adsorptive stripping of complex bismuth with 1,2-phenylenedioxydiacetic acid (PDA) at a hanging mercury drop electrode (HMDE). The effect of various parameters such as pH, concentration of ligand, accumulation potential and accumulation time on the selectivity and sensitivity were studied. The optimum conditions for determination of bismuth include nitric acid concentration 0.01,M, 8.0×10,4,M PDA and accumulation time 120,s, accumulation potential of ,200,mV. The limits of detection are 0.25 and 0.05,nM, and responses are linear 1,1000 and 0.1,400,nM at tacc of 60 and 120,s, respectively. Many common anions and cations do not interfere in the determination of bismuth. The method was applied to the determination of bismuth in some real samples such as sea , and spring water and drug. [source] Simultaneous Determination of Copper and Bismuth by Anodic Stripping Voltammetry Using H-Point Standard Addition Method with Simultaneous Addition of AnalytesELECTROANALYSIS, Issue 17 2005Esmaeil Shams Abstract Simultaneous determination of bismuth and copper by anodic stripping voltammetry using H-point standard addition method (HPSAM) with simultaneous addition of analytes is described. The effect of various parameters including acid concentration, accumulation time, accumulation potential and concentration ratio of analytes in the standard solution on the sensitivity and accuracy of method were investigated. The results of applying the H-point standard addition method showed that Cu2+ and Bi3+ could be determined simultaneously with the concentration ratios of Cu2+ to Bi3+ varying from 1,:,15 to 16,:,1 in the mixed sample. The method was successfully applied to the simultaneous determination of copper and bismuth in some synthetic mixtures. [source] Determination of Platinum with Thiosemicarbazide by Catalytic Adsorptive Stripping Voltammetry (AdSV)ELECTROANALYSIS, Issue 4 2005Sylwester Huszal Abstract This work describes a very sensitive and selective voltammetric procedure for the determination of platinum. Instead of commonly used hydrazine, thiosemicarbazide as a component of supporting electrolyte was applied. The method is based on adsorption of platinum-thiosemicarbazone complex, formed in situ in voltammetric cell from thiosemicarbazide and formaldehyde, coupled with a hydrogen catalytic reaction at a hanging mercury drop electrode. The linear relation between platinum concentration and height of analytical signal was observed up to 1.5×10,9,mol,L,1 with the detection limit calculated as 1.5×10,13,mol,L,1 (3,s of the blank) after 50,s of accumulation time. The effect of various interferences from other ions was studied. Described method was applied for platinum determination in hydroponically cultivated plants after microwave decomposition. [source] Electrochemical Biosensor for the Detection of Interaction Between Arsenic Trioxide and DNA Based on Guanine SignalELECTROANALYSIS, Issue 7 2003Mehmet Ozsoz Abstract The interaction of arsenic trioxide (As2O3) with calf thymus double-stranded DNA (dsDNA), calf thymus single-stranded DNA (ssDNA) and also 17-mer short oligonucleotide (Probe,A) was studied electrochemically by using differential pulse voltammetry (DPV) with carbon paste electrode (CPE) at the surface and also in solution. Potentiometric stripping analysis (PSA) was employed to monitor the interaction of As2O3 with dsDNA in solution phase by using a renewable pencil graphite electrode (PGE). The changes in the experimental parameters such as the concentration of As2O3, and the accumulation time of As2O3 were studied by using DPV; in addition, the reproducibility data for the interaction between DNA and As2O3 was determined by using both electrochemical techniques. After the interaction of As2O3 with dsDNA, the DPV signal of guanine was found to be decreasing when the accumulation time and the concentration of As2O3 were increased. Similar DPV results were also found with ssDNA and oligonucleotide. PSA results observed at a low DNA concentration such as 1,ppm and a different working electrode such as PGE showed that there could be damage to guanine bases. The partition coefficients of As2O3 after interaction with dsDNA and ssDNA in solution by using CPE were calculated. Similarly, the partition coefficients (PC) of As2O3 after interaction with dsDNA in solution was also calculated by PSA at PGE. The features of this proposed method for the detection of DNA damage by As2O3 are discussed and compared with those methods previously reported for the other type of DNA targeted agents in the literature. [source] Adsorptive Stripping Voltammetric Detection of Single-Stranded DNA at Electrochemically Modified Glassy Carbon ElectrodeELECTROANALYSIS, Issue 23 2002Huai-Sheng Wang Abstract Electrochemically modified glassy carbon electrode (GCE) was used to study the electrochemical oxidation and detection of denatured single-stranded (ss) DNA by means of adsorptive stripping voltammetry. The modification of GCE, by electrochemical oxidation at +1.75,V (vs.SCE) for 10,min and cyclic sweep between +0.3,V and ,1.3,V for 20,cycles in pH,5.0 phosphate buffer, results in 100-fold improvement in sensitivity for ssDNA detection. We speculated that the modified GCE has a high affinity to single-stranded DNA through hydrogen bond (specific static adsorption). Single-stranded DNA can accumulate at the GCE surface at open circuit and produce a well-defined oxidation peak corresponding to the guanine residues at about +0.80,V in pH,5.0 phosphate buffer, while the native DNA gives no signal under the same condition. The peak currents are proportional to the ssDNA concentration in the range of 0,18.0,,g,mL,1. The detection limit of denatured ssDNA is ca. 0.2,,g mL,1 when the accumulation time is 8,min at open circuit. The accumulation mechanism of ssDNA on the modified GCE was discussed. [source] Diagnostic assay of chromium (VI) in the ex vivo fluid of the urine of a smoker using a fluorine-doped handmade sensorJOURNAL OF CLINICAL LABORATORY ANALYSIS, Issue 2 2009Suw Young Ly Abstract A voltammetric diagnosis of a chromium (VI) ion was investigated using a fluorine-doped graphite pencil electrode. Square wave (SW) stripping working conditions were attained at a high range of 0.051,0.45,mg,L,1 and a microrange of 0.05,0.4,µg,L,1 in a 0.1,M NH4H2PO4 electrolyte solution, at a relative standard deviation of 1.68% (RSD, n=15), using 10.0,µg,L,1 Cr(VI). A fast experimental time was used only for the 120,sec SW accumulation time. An analytical detection-limit (DL) of 0.008,µg,L,1 was attained. DL appeared to be more sensitive than common voltammetric and spectrophotometric assays. The developed sensor was applied to tap water and the urine of a smoker. It was found that the methods can be applicable for in vivo fluid or medicinal diagnosis. J. Clin. Lab. Anal. 23:82,87, 2009. © 2009 Wiley-Liss, Inc. [source] Nano-level detection of naltrexone hydrochloride in its pharmaceutical preparation at Au microelectrode in flowing solutions by fast fourier transforms continuous cyclic voltammetry as a novel detectorJOURNAL OF PHARMACEUTICAL SCIENCES, Issue 8 2007P. Norouzi Abstract An easy and fast Fourier transform continuous cyclic voltammetric technique for monitoring of ultra trace amounts of naltrexone in a flow-injection system has been introduced in this work. The potential waveform, consisting of the potential steps for cleaning, stripping and potential ramp, was continuously applied on an Au disk microelectrode (with a 12.5 µm in radius). The proposed detection method has some of advantages, the greatest of which are as follows: first, it is no more necessary to remove oxygen from the analyte solution and second, this is a very fast and appropriate technique for determination of the drug compound in a wide variety of chromatographic analysis methods. The method was linear over the concentration range of 0.34,34000 pg/mL (r,=,0.9985) with a limit of detection 8.0,×,10,4 nM. The method has the requisite accuracy, sensitivity, precision, and selectivity to assay naltrexone in tablets. The influences of pH of eluent, accumulation potential, sweep rate, and accumulation time on the determination of the naltrexone were considered. © 2007 Wiley-Liss, Inc. and the American Pharmacists Association J Pharm Sci 96:2009,2017, 2007 [source] Fluorescence background suppression in Raman spectroscopy using combined Kerr gated and shifted excitation Raman difference techniquesJOURNAL OF RAMAN SPECTROSCOPY, Issue 4 2002P. Matousek An exceptionally high level of fluorescence rejection from resonance Raman spectra was achieved using a combination of two techniques, namely Kerr gated temporal rejection with shifted excitation Raman difference spectroscopy. The method was able to recover the resonance Raman spectrum from the intense fluorescence background with a signal-to-noise ratio at least 10 times higher than that achievable with either of the two approaches used individually. To demonstrate the effectiveness of the technique we obtained the resonance Raman spectrum of the laser dye rhodamine 6G (1 × 10,3 mol dm,3) in methanol by excitation at 532 nm and measuring under the maximum of fluorescence emission at 560,590 nm. The method reached the photon shot noise limit of the residual fluorescence providing a detection limit for Raman spectra 106 times lower than the original fluorescence intensity in an accumulation time of 800 s. A unique feature of the experiment was the way in which the optical parametric amplifier light source was configured to alternate automatically between the two excitation wavelengths using an optogalvanic mirror arrangement. The ultra-high sensitivity of the combined approach holds great promise for selective probing of complex biological systems using resonance Raman spectroscopy. Copyright © 2002 John Wiley & Sons, Ltd. [source] Monitoring of Anti Cancer Drug Letrozole by Fast Fourier Transform Continuous Cyclic Voltammetry at Gold MicroelectrodeCHINESE JOURNAL OF CHEMISTRY, Issue 7 2010Parviz Norouzi Abstract A continuous cyclic voltammetric study of letrozole at gold microelectrode was carried out. The drug in phosphate buffer (pH 2.0) is adsorbed at ,200 mV, giving rise to change in the current of well-defined oxidation peak of gold in the flow injection system. The proposed detection method has some of advantages, the greatest of which are as follows: first, it is no more necessary to remove oxygen from the analyte solution and second, this is a very fast and appropriate technique for determination of the drug compound in a wide variety of chromatographic analysis methods. Signal-to-noise ratio has significantly increased by application of discrete Fast Fourier Transform (FFT) method, background subtraction and two-dimensional integration of the electrode response over a selected potential range and time window. Also in this work some parameters such as sweep rate, eluent pH, and accumulation time and potential were optimized. The linear concentration range was of 1.0×10,7,1.0×10,10 mol/L (r=0.9975) with a limit of detection and quantitation 0.08 nmol/L and 0.15 nmol/L, respectively. The method has the requisite accuracy, sensitivity, precision and selectivity to assay letrozol in tablets. The influences of pH of eluent, accumulation potential, sweep rate, and accumulation time on the determination of the letrozol were considered. [source] Sediment compaction rates and subsidence in deltaic plains: numerical constraints and stratigraphic influencesBASIN RESEARCH, Issue 1 2007T. A. Meckel ABSTRACT Natural sediment compaction in deltaic plains influences subsidence rates and the evolution of deltaic morphology. Determining compaction rates requires detailed knowledge of subsurface geotechnical properties and depositional history, neither of which is often readily available. To overcome this lack of knowledge, we numerically forward model the incremental sedimentation and compaction of stochastically generated stratigraphies with geotechnical properties typical of modern depositional environments in the Mississippi River delta plain. Using a Monte Carlo approach, the range of probable compaction rates for stratigraphies with compacted thicknesses <150 m and accumulation times <20 kyr. varies, but maximum values rarely exceed a few mm yr,1. The fastest compacting stratigraphies are composed primarily of peat and bar sand, whereas the slowest compacting stratigraphies are composed of prodelta mud and natural levee deposits. These results suggest that compaction rates can significantly influence vertical and lateral stratigraphic trends during deltaic evolution. [source] | |||||||||||||