Anodic Stripping Voltammetry (anodic + stripping_voltammetry)

Distribution by Scientific Domains


Selected Abstracts


Simultaneous Quantitative Determination of Cadmium, Lead, and Copper on Carbon-Ink Screen-Printed Electrodes by Differential Pulse Anodic Stripping Voltammetry and Partial Least Squares Regression

ELECTROANALYSIS, Issue 23 2008
Michael Cauchi
Abstract Water is a vital commodity for every living entity on the planet. However, water resources are threatened by various sources of contamination from pesticides, hydrocarbons and heavy metals. This has resulted in the development of concepts and technologies to create a basis for provision of safe and high quality drinking water. This paper focuses on the simultaneous quantitative determination of three common contaminants, the heavy metals cadmium, lead and copper. Multivariate calibration was applied to voltammograms acquired on in-house printed carbon-ink screen-printed electrodes by the highly sensitive electrochemical method of differential pulse anodic stripping voltammetry (DPASV). The statistically inspired modification of partial least squares (SIMPLS) algorithm was employed to effect the multivariate calibration. The application of data pretreatment techniques involving range-scaling, mean-centering, weighting of variables and the effects of peak realignment are also investigated. It was found that peak realignment in conjunction with weighting and SIMPLS led to the better overall root mean square error of prediction (RMSEP) value. This work represents significant progress in the development of multivariate calibration tools in conjunction with analytical techniques for water quality determination. It is the first time that multivariate calibration has been performed on DPASV voltammograms acquired on carbon-ink screen-printed electrodes. [source]


Determination of Trace Amounts of Copper in Tap Water Samples with a Calix[4]arene Modified Carbon Paste Electrode by Differential Pulse Anodic Stripping Voltammetry

ELECTROANALYSIS, Issue 10 2007
Çelik Canpolat
Abstract A calix[4]arene modified carbon paste electrode was used for trace determination of copper. The study of the preconcentration of copper as well as the other heavy metal ions at the modified electrode, with subsequent measurement by differential pulse anodic stripping voltammetry (DPASV), indicates the efficient open-circuit accumulation of the analytes onto the electrode. Many parameters such as the composition of the paste, pH, preconcentration time and stirring rate influence the response of the measurement. The procedure was optimized for copper determination. For a 10-minute preconcentration time at pH,6.5,7.5, the detection limit (LOD) was 1.1,,g L,1. The optimized method was successfully applied to the determination of copper in tap water sample by means of standard addition procedure. The copper content of the sample was comparable with the result obtained with AAS method. [source]


Enhanced Resolution of Copper and Bismuth by Addition of Gallium in Anodic Stripping Voltammetry with the Bismuth Film Electrode

ELECTROANALYSIS, Issue 24 2006
Chad 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]


Determination of Lead and Cadmium at Silver Electrode by Subtractive Anodic Stripping Voltammetry in Plant Materials Containing Tl

ELECTROANALYSIS, Issue 9 2005
Beata Krasnod, bska-Ostr
Abstract Lead and cadmium have been determined by the subtractive anodic stripping voltammetry using the square-wave mode at a silver electrode without removal of oxygen. The samples containing large amount of thallium were collected from a highly contaminated region. The presence of thallium strongly affects the peak shape of Cd. The plant material digestion was performed with HNO3/HClO4 mixture using pressurised microwave decomposition. The proposed method used for the lead determination was validated by the inter-method comparison (ICP-MS). The cadmium determination was validated using certified reference material. The results obtained, supported by statistical tests, demonstrated the usefulness of the method for the lead determination in samples containing large amounts of Cd and Tl. It is important to note that Cd can only be quantified when the thallium concentration is much lower than that of cadmium. [source]


Fast Mapping of Gunshot Residues by Batch Injection Analysis with Anodic Stripping Voltammetry of Lead at the Hanging Mercury Drop Electrode

ELECTROANALYSIS, Issue 2 2005
Adriana De, Donato
Abstract The forensic analysis of lead in gunshot residues (GSR) sampled on the hands of potential shooters is rendered faster, simpler and less expensive by a new batch injection analysis (BIA) method, based on differential pulse anodic stripping voltammetry (DPASV). A simple "J" shaped adaptor was designed to direct the flux of the analyte injected with a micropipettor onto the hanging mercury drop electrode of any commercial electrode stand. Sampling methods for GSR were compared and lifting with adhesive tape was elected for field use. The tapes are glued on polyethylene screens and stored in capped vials. Sampling with multiple strips provides coarse mapping of the distribution of lead on the shooter's hands. After a dissolution/extraction step with chloroform/aqueous 0.10,mol,L,1 HCl, 100,,L of the aqueous phase are injected during 25,s for accumulation of lead on the HMDE at ,0.60,V (vs. Ag/AgCl). A detection limit of 20,ng/mL of Pb(II), outreaching for GSR analysis, is reached without oxygen removal, at a frequency of 20 injections per hour. Results for sequences of shootings with a revolver and a pistol are presented. [source]


A Study of the Determination of Cu(II) by Anodic Stripping Voltammetry on a Novel Nylon/Carbon Fiber Electrode

ELECTROANALYSIS, Issue 7 2004
A. Mylonakis
Abstract In this work we report a new electrode material formed by injection-moulding of a conducting polymer consisting of carbon fibers in a Nylon matrix. This material is highly conductive, inexpensive, easy to mould in different shapes and requires minimal pretreatment. The electrode was tested as a mercury-free sensor for the trace determination of Cu(II) by anodic stripping voltammetry (ASV). The deposition and stripping behavior of copper on the conducting material was initially studied by cyclic voltammetry and the chemical and instrumental parameters of the determination were investigated. The electrode has been shown to be suitable for the determination of Cu(II) in the range 8,,g L,1 to 30,mg,L,1 (with deposition times ranging from 30,s to 10,min) with a relative standard deviation of 2.2% (at the 0.5,mg,L,1 level) and a limit of detection of 8,,g L,1 Cu(II) for 10,min of accumulation (at a S/N ratio of 5). The electrode was, finally, applied to the determination of copper in tap-water, pharmaceutical tablets and bovine serum with recoveries of 97.4, 94.9 and 93.4%, respectively [source]


Characteristics of Subtractive Anodic Stripping Voltammetry of Lead, Cadmium and Thallium at Silver-Gold Alloy Electrodes

ELECTROANALYSIS, Issue 17 2003
Y. Bonfil
Abstract Silver-gold alloy electrodes have been studied for the purpose of the quantitative determination of heavy metals by subtractive anodic stripping voltammetry, (SASV). The results have been compared with those obtained with the silver and gold electrodes. The 50/50 a/o Ag/Au alloy electrode is the most suitable for quantifying thallium in the presence of lead and cadmium. The separation of its peak from those of lead and cadmium is 200,mV, which is about twice the separation obtained on the pure metal electrodes and is also better than on mercury. The silver electrode is suitable for the simultaneous determination of thallium, lead and cadmium. The peaks of lead and cadmium overlap on the 50/50 alloy. Pure silver or pure gold can be used for simultaneous quantification of these two metals. The use of gold for quantifying lead and cadmium is more limited because the peak potential of cadmium is shifted in the negative direction as its concentration increases and at [Cd2+]>200,nM, the two peaks merge. SASV enables correction for background currents and is of utmost importance for obtaining well-defined peaks. The peaks of lead, cadmium and thallium appear over a relatively narrow potential range (ca. 200,mV) on all the electrodes presented in this work. For this reason, the quantifying of a peak is based on the derivative at the inflection point of only one of its branches (ascending or descending). All SASV measurements were carried out without removal of oxygen. [source]


Stripping Voltammetry at Microdisk Electrode Arrays: Theory

ELECTROANALYSIS, Issue 24 2009

Abstract Anodic stripping voltammetry (ASV) is an extremely powerful tool for detection of metal ions in solution through a two step process of preconcentration of the metal at the electrode surface, followed by electrodissolution. The second phase produces an electroanalytical response proportional to the amount of material deposited in the first phase. This paper utilizes theory to explore the electrochemical signals produced when considering ASV at a microelectrode or ultramicroelectrode arrays. The theory outlined is applicable mostly to thin mercury film absorption and metal adsorption. [source]


Working Electrodes from Amalgam Paste for Electrochemical Measurements

ELECTROANALYSIS, Issue 4 2008
Bogdan Yosypchuk
Abstract Paste electrode with paste amalgam as an active electrode material is described here for the first time. Designed electrode from silver paste amalgam (AgA-PE) is solely metallic and does not contain any organic binder. Mechanical surface regeneration of AgA-PE is performed in the same way as for classical carbon paste electrodes and reproducibility of such regeneration is about 10%. Electrochemical surface regeneration appeared very efficient for most measurements. In dependence on paste metal content, the electrode surface can be liquid (resembling a film) or rather solid. The hydrogen overvoltage on AgA-PE is high, and the electrode allows measurements at highly negative potentials. AgA-PE is well suited for study of reduction or oxidation processes without an accumulation step. Anodic stripping voltammetry of some metals tested on the electrode is influenced by formation of intermetallic compounds. The measurement based on cathodic stripping voltammetry (adenine, cysteine) and on catalytic processes from adsorbed state (complex of osmium tetroxide with 2,2,-bipyridine) can be performed on AgA-PE practically under the same conditions as found earlier for HMDE and for silver solid amalgam electrode. The working electrode from paste amalgam combines the advantages of paste and metal electrodes. [source]


Simultaneous Determination of Cadmium, Lead, Copper and Mercury Ions Using Organofunctionalized SBA-15 Nanostructured Silica Modified Graphite,Polyurethane Composite Electrode

ELECTROANALYSIS, Issue 1 2010
Ivana Cesarino
Abstract A new sensor has been developed for the simultaneous detection of cadmium, lead, copper and mercury, using differential pulse and square wave anodic stripping voltammetry (DPASV and SWASV) at a graphite,polyurethane composite electrode with SBA-15 silica organofunctionalized with 2-benzothiazolethiol as bulk modifier. The heavy metal ions were preconcentrated on the surface of the modified electrode at ,1.1,V vs. SCE where they complex with 2-benzothiazolethiol and are reduced to the metals, and are then reoxidized. Optimum SWASV conditions lead to nanomolar detection limits and simultaneous determination of Cd2+, Pb2+, Cu2+ and Hg2+ in natural waters was achieved. [source]


Electroanalytical Determination of Cadmium(II) and Lead(II) Using an Antimony Nanoparticle Modified Boron-Doped Diamond Electrode

ELECTROANALYSIS, Issue 10 2009
Kathryn
Abstract We report the simultaneous electroanalytical determination of Pb2+ and Cd2+ by linear sweep anodic stripping voltammetry (LSASV) using an antimony nanoparticle modified boron doped diamond (Sb-BDD) electrode. Sb deposition was performed in situ with the analytes, from a solution of 1,mg L,1 SbCl3 in 0.1,M HCl (pH,1). Pb2+ inhibited the detection of Cd2+ during simultaneous additions at the bare BDD electrode, whereas in the presence of antimony, both peaks were readily discernable and quantifiable over the linear range 50,500,,g L,1. [source]


Quantitative Studies of Metal Ion Adsorption on a Chemically Modified Carbon Surface: Adsorption of Cd(II) and Hg(II) on Glutathione Modified Carbon

ELECTROANALYSIS, Issue 8 2009
Poobalasingam Abiman
Abstract The adsorption behavior of model toxic metal cations namely Cd(II) and Hg(II) on carbon surfaces chemically modified by glutathione was investigated as a function of the concentration of Cd2+ and Hg2+ ions, time and the amount of modified carbon used. Square wave and linear sweep anodic stripping voltammetry was used to monitor the uptake of Cd(II) and Hg(II) ions respectively. Kinetic and adsorption isotherm studies reveal that both Cd(II) and Hg(II) ions undergo similar large adsorption with the modified glutathione carbon material (Glu-carbon). [source]


Simultaneous Quantitative Determination of Cadmium, Lead, and Copper on Carbon-Ink Screen-Printed Electrodes by Differential Pulse Anodic Stripping Voltammetry and Partial Least Squares Regression

ELECTROANALYSIS, Issue 23 2008
Michael Cauchi
Abstract Water is a vital commodity for every living entity on the planet. However, water resources are threatened by various sources of contamination from pesticides, hydrocarbons and heavy metals. This has resulted in the development of concepts and technologies to create a basis for provision of safe and high quality drinking water. This paper focuses on the simultaneous quantitative determination of three common contaminants, the heavy metals cadmium, lead and copper. Multivariate calibration was applied to voltammograms acquired on in-house printed carbon-ink screen-printed electrodes by the highly sensitive electrochemical method of differential pulse anodic stripping voltammetry (DPASV). The statistically inspired modification of partial least squares (SIMPLS) algorithm was employed to effect the multivariate calibration. The application of data pretreatment techniques involving range-scaling, mean-centering, weighting of variables and the effects of peak realignment are also investigated. It was found that peak realignment in conjunction with weighting and SIMPLS led to the better overall root mean square error of prediction (RMSEP) value. This work represents significant progress in the development of multivariate calibration tools in conjunction with analytical techniques for water quality determination. It is the first time that multivariate calibration has been performed on DPASV voltammograms acquired on carbon-ink screen-printed electrodes. [source]


The Fabrication and Characterization of a Bismuth Nanoparticle Modified Boron Doped Diamond Electrode and Its Application to the Simultaneous Determination of Cadmium(II) And Lead(II)

ELECTROANALYSIS, Issue 16 2008
Kathryn
Abstract We report the simultaneous electroanalytical determination of Pb2+ and Cd2+ by square-wave anodic stripping voltammetry (SWASV) using a bismuth nanoparticle modified boron doped diamond (Bi-BDD) electrode. Bi deposition was performed in situ with the analytes, from a solution of 0.1,mM Bi(NO3)3 in 0.1,M HClO4 (pH,1.2), and gave detection limits of 1.9,,g L,1 and 2.3,,g L,1 for Pb(II) and Cd(II) respectively. Pb2+ and Cd2+ could not be detected simultaneously at a bare BDD electrode, whilst on a bulk Bi macro electrode (BiBE) the limits of detection for the simultaneous determination of Pb2+ and Cd2+ were ca. ten times higher. [source]


Stripping Voltammetry of Cerium(IIl) with a Chemically Modified Carbon Paste Electrode Containing Functionalized Nanoporous Silica Gel

ELECTROANALYSIS, Issue 2 2008
Mehran Javanbakht
Abstract This research introduces the design of an adsorptive stripping voltammetric method for the cerium(III) determination at a carbon paste electrode, chemically modified with dipyridyl-functionalized nanoporous silica gel (DPNSG-CPE). The electroanalytical procedure comprised two steps: the Ce(III) chemical accumulation at ,200,mV followed by the electrochemical detection of the Ce(III)/dipyridyl complex, using anodic stripping voltammetry. The factors, influencing the adsorptive stripping performance, were optimized including the modifier quantity in the paste, the electrolyte concentrations, the solution pH and the accumulation potential or time. The resulting electrode demonstrated a linear response over a wide range of Ce(III) concentration (1.0,28,ng mL,1). The precision for seven determinations of 4 and 10,ng mL,1 Ce(III) was 3.2% and 2.5% (relative standard deviation), respectively. The prepared electrode was used for the cerium determination in real samples and very good recovery results were obtained. [source]


Voltammetric Determination of Mercury(II) at Poly(3-hexylthiophene) Film Electrode.

ELECTROANALYSIS, Issue 24 2007
Effect 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]


Anodic Stripping Voltammetry Using a Vibrating Electrode

ELECTROANALYSIS, Issue 13 2007
Conrad
Abstract This work proposes a vibrating microwire electrode as working electrode in stripping voltammetry. The vibration was found to maintain a constant and thin (1,2,,m) diffusion layer during the deposition step. The electrode vibration eliminated the need for external stirring of the solution, thus facilitating in situ detection in the environment. The vibration was effected by fixing a low-voltage (3,V), asymmetric, electrical rotor to the working electrode (a gold microwire of either 5 or 25,,m). The sensitivity of the vibrated electrode was ca. 22×greater than stationary. Measurements of copper (4,nM) by anodic stripping voltammetry using the vibrating electrode had a low standard deviation (1% for n=6) indicating that the diffusion layer had only minor variability. The agitation mechanism was unaffected by water moving at >2,m s,1 and by water pressure equivalent to a depth of >40,m, indicating its suitability for in situ measurements. The vibrating probe was used for in situ detection of copper by anodic stripping voltammetry to a depth of 6,m. Using a 5,min deposition time, the limit of detection for labile copper was 38,pM. [source]


Voltammetry as an Alternative Tool for Trace Metal Detection in Peloid Marine Sediments

ELECTROANALYSIS, Issue 13 2007
Irena Ciglene
Abstract Here was demonstrated for the first time a possible application of abrasive stripping voltammetry in the direct measurement of trace metals in anoxic, sulfidic marine sediments (peloid mud) from a small and shallow (0.2,1,m) marine lagoon in Central Dalmatia, Croatia. Trace amounts of sample compounds are transferred to the graphite electrode surface and electrochemical reduction or oxidation processes are followed by the cyclic voltammetry in seawater or 0.55,M NaCl as electrolyte. After a preelectrolysis at potentials ranging from ,1.0 to ,1.5,V (vs. SCE) a well-defined anodic stripping peak corresponding to the oxidation of metal deposits generated at deposition potentials is obtained around ,0.74,V (vs. SCE). The same samples were studied by anodic stripping voltammetry at the Hg electrode and inductively coupled plasma-mass spectrometer (ICP-MS). ICP-MS showed higher concentrations of trace metals such as Al, Fe, Mo, Mn. A relatively high concentration of reduced sulfur species (RSS) (10,3 M) is determined electrochemically in porewater of the peloid mud, indicating that the magnitude of metal enrichment in the sediments is probably controlled by precipitation with sulfide. [source]


Determination of Trace Amounts of Copper in Tap Water Samples with a Calix[4]arene Modified Carbon Paste Electrode by Differential Pulse Anodic Stripping Voltammetry

ELECTROANALYSIS, Issue 10 2007
Çelik Canpolat
Abstract A calix[4]arene modified carbon paste electrode was used for trace determination of copper. The study of the preconcentration of copper as well as the other heavy metal ions at the modified electrode, with subsequent measurement by differential pulse anodic stripping voltammetry (DPASV), indicates the efficient open-circuit accumulation of the analytes onto the electrode. Many parameters such as the composition of the paste, pH, preconcentration time and stirring rate influence the response of the measurement. The procedure was optimized for copper determination. For a 10-minute preconcentration time at pH,6.5,7.5, the detection limit (LOD) was 1.1,,g L,1. The optimized method was successfully applied to the determination of copper in tap water sample by means of standard addition procedure. The copper content of the sample was comparable with the result obtained with AAS method. [source]


Construction and Evaluation of a Gold Tubular Electrode for Flow Analysis: Application to Speciation of Antimony in Water Samples

ELECTROANALYSIS, Issue 6 2007
Rodrigo Santos
Abstract A tubular gold electrode (TGE) is described for the first time by summarizing the important aspects of its construction and evaluation. Applicability of the TGE is evaluated in the speciation of Sb(III) and Sb(V) using anodic stripping voltammetry in a single flow manifold. Studies with surface active interferences and metallic cations were performed. The proposed conditions for antimony determination showed good tolerance towards cationic, anionic and nonionic surface active substances. A linear response for antimony was obtained for solutions containing significant amounts of several metallic cations. Linear calibration curves for Sb(III) were obtained in the range 1,10,ppb with a detection limit of 0.19,ppb (CV=2.91%, n=5, [Sb(III)]=5,ppb). For Sb(V), linear calibration curves were in the range 1,15,ppb with a detection limit of 0.32,ppb (CV=1.41%, n=5, [Sb(V)]=5,ppb). The figures of merit achieved sustain for the good applicability of the proposed method as it allows the determination of antimony at levels below maximum values permitted in consuming waters. Results of antimony concentration determined in water samples were validated against the ICP-MS reference procedure or compared with reference water samples. [source]


Enhanced Resolution of Copper and Bismuth by Addition of Gallium in Anodic Stripping Voltammetry with the Bismuth Film Electrode

ELECTROANALYSIS, Issue 24 2006
Chad 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]


Screen Printed Electrodes and Screen Printed Modified Electrodes Benefit from Insonation

ELECTROANALYSIS, Issue 9 2006
Biljana, ljuki
Abstract The synergy of power ultrasound with screen printed electrodes and screen printed modified electrodes is shown to be possible and beneficial. Proof-of-concept is shown for the anodic stripping voltammetry of lead at screen printed electrodes and screen printed calomel modified electrodes offering shorter deposition times and increased sensitivity. [source]


Simultaneous Determination of Copper and Bismuth by Anodic Stripping Voltammetry Using H-Point Standard Addition Method with Simultaneous Addition of Analytes

ELECTROANALYSIS, Issue 17 2005
Esmaeil 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]


Mercury Detection in Seawater Using a Mercaptoacetic Acid Modified Gold Microwire Electrode

ELECTROANALYSIS, Issue 10 2005
Antje Widmann
Abstract It is demonstrated here that it is possible to determine mercury in chloride containing media like seawater by anodic stripping voltammetry using a modified electrode. A gold microwire electrode is modified using mercaptoacetic acid (MAA) to eliminate the problem of calomel formation, allowing the mercury to become fully removed from the electrode surface after each scan. In a synthetic salt solution of KNO3 the sensitivity for mercury was found to be improved by the surface modification. In seawater the sensitivity was not significantly improved possibly because of complexation of the mercury by the abundant chloride; however, the MAA coating prevented the formation of calomel causing the background scan to be free of mercury. Measurements in seawater at various pH values demonstrated that mercury detection is possible at natural pH (around 8); however, best sensitivity was attained at pH,4.8 with a deposition time of 3,min. A peak for copper occurred at more negative potential but did not interfere at this pH. The calibration was linear between 0 and 37,nM mercury with a limit of detection of 1,nM mercury. [source]


Determination of Lead and Cadmium at Silver Electrode by Subtractive Anodic Stripping Voltammetry in Plant Materials Containing Tl

ELECTROANALYSIS, Issue 9 2005
Beata Krasnod, bska-Ostr
Abstract Lead and cadmium have been determined by the subtractive anodic stripping voltammetry using the square-wave mode at a silver electrode without removal of oxygen. The samples containing large amount of thallium were collected from a highly contaminated region. The presence of thallium strongly affects the peak shape of Cd. The plant material digestion was performed with HNO3/HClO4 mixture using pressurised microwave decomposition. The proposed method used for the lead determination was validated by the inter-method comparison (ICP-MS). The cadmium determination was validated using certified reference material. The results obtained, supported by statistical tests, demonstrated the usefulness of the method for the lead determination in samples containing large amounts of Cd and Tl. It is important to note that Cd can only be quantified when the thallium concentration is much lower than that of cadmium. [source]


Electrochemical Impedance Characterization of Nafion-Coated Carbon Film Resistor Electrodes for Electroanalysis

ELECTROANALYSIS, Issue 7 2005
Carla Gouveia-Caridade
Abstract Carbon film disk electrodes with Nafion coatings have been characterized by electrochemical impedance spectroscopy (EIS) with a view to a better understanding of their advantages and limitations in electroanalysis, particularly in anodic stripping voltammetry of metal ions. After initial examination by cyclic voltammetry, spectra were recorded over the full potential range in acetate buffer solution at the bare electrodes, electrodes electrochemically pretreated in acid solution, and Nafion-coated pretreated electrodes in the presence and absence of dissolved oxygen. EIS equivalent circuit analysis clearly demonstrated the changes between these electrode assemblies. In order to simulate anodic stripping voltammetry conditions, spectra were also obtained in the presence of cadmium and lead ions in solution at Nafion-coated electrodes, both after metal ion deposition and following re-oxidation. Permanent changes to the structure of the Nafion film occurred, which has implications for use of these electrode assemblies in anodic stripping voltammetry at relatively high trace metal ion concentrations. [source]


A Study of Heavy Metal Complexation in Grape Juice

ELECTROANALYSIS, Issue 5-6 2005
Íñigo Salinas
Abstract Differential pulse anodic stripping voltammetry, DPASV, has been used to monitor the initial stages of grape juice fermentation, focusing on Zn interactions with natural occurring ligands. Langmuir and Scatchard linearization methods have been employed. A 1,:,1 ratio has been found by either method; from Langmuir data analysis only one ligand population was found, while Scatchard approach gave rise to the detection of two ligand types. Both data analysis procedures led to the same total ligand concentration. When catechin was used as model ligand, a 1,:,1 ratio was found for Zn and also for Cu. [source]


Fast Mapping of Gunshot Residues by Batch Injection Analysis with Anodic Stripping Voltammetry of Lead at the Hanging Mercury Drop Electrode

ELECTROANALYSIS, Issue 2 2005
Adriana De, Donato
Abstract The forensic analysis of lead in gunshot residues (GSR) sampled on the hands of potential shooters is rendered faster, simpler and less expensive by a new batch injection analysis (BIA) method, based on differential pulse anodic stripping voltammetry (DPASV). A simple "J" shaped adaptor was designed to direct the flux of the analyte injected with a micropipettor onto the hanging mercury drop electrode of any commercial electrode stand. Sampling methods for GSR were compared and lifting with adhesive tape was elected for field use. The tapes are glued on polyethylene screens and stored in capped vials. Sampling with multiple strips provides coarse mapping of the distribution of lead on the shooter's hands. After a dissolution/extraction step with chloroform/aqueous 0.10,mol,L,1 HCl, 100,,L of the aqueous phase are injected during 25,s for accumulation of lead on the HMDE at ,0.60,V (vs. Ag/AgCl). A detection limit of 20,ng/mL of Pb(II), outreaching for GSR analysis, is reached without oxygen removal, at a frequency of 20 injections per hour. Results for sequences of shootings with a revolver and a pistol are presented. [source]


DNA Hybridization at Magnetic Nanoparticles with Electrochemical Stripping Detection

ELECTROANALYSIS, Issue 23 2004
Ningning Zhu
Abstract A simple and practical method for electrochemical DNA hybridization assay has been developed to take advantage of magnetic nanoparticles for ssDNA immobilization and zinc sulfide nanoparticle as oligonucleotide label. Magnetic nanoparticles were prepared by coprecipitation of Fe2+ and Fe3+ with NH4OH, and then amino silane was coated onto the surface of magnetite nanoparticles. The magnetic nanoparticles have the advantages of easy preparation, easy surface modification and low cost. The target ssDNA with the phosphate group at the 5, end was then covalently immobilized to the amino group of magnetite nanoparticles by forming a phosphoramidate bond in the presence of 1-ethyl-3-(3-dimeth-ylaminopropyl)carbodiimide (EDAC). The zinc sulfide (ZnS) nanoparticle-labeled oligonucleotides probe was used to identify the target ssDNA immobilized on the magnetic nanoparticles based on a specific hybridization reaction. The hybridization events were assessed by the dissolution of the zinc sulfide nanoparticles anchored on the hybrids and the indirect determination of the dissolved zinc ions by anodic stripping voltammetry (ASV) at a mercury film glassy carbon electrode (GCE). The proposed method couples the high sensitivity of anodic stripping analysis for zinc ions with effective magnetic separation for eliminating nonspecific adsorption effects and offers great promise for DNA hybridization analysis. [source]


Heavy Metals in Matrices of Food Interest: Sequential Voltammetric Determination at Trace and Ultratrace Level of Copper, Lead, Cadmium, Zinc, Arsenic, Selenium, Manganese and Iron in Meals

ELECTROANALYSIS, Issue 18 2004
Clinio Locatelli
Abstract The voltammetric methods are very suitable and versatile techniques for the simultaneous metal determination in complex matrices. The present work, regarding the sequential determination of Cu(II), Pb(II), Cd(II), Zn(II) by square-wave anodic stripping voltammetry (SWASV), As(III), Se(IV) by square-wave cathodic stripping voltammetry (SWCSV) and Mn(II), Fe(III) by square-wave voltammetry (SWV) in matrices involved in foods and food chain as wholemeal, wheat and maize meal, are an interesting example of the possibility to sequentially determine each single element in real samples. Besides the set up of the analytical method, particular attention is aimed either at the problem of possible signal interference or to show that, using the peak area Ap as instrumental datum, it is possible to achieve lower limits of detection. The analytical procedure was verified by the analysis of the standard reference materials: Wholemeal BCR-CRM 189, Wheat Flour NIST-SRM 1567a and Rice Flour NIST-SRM 1568a. Precision, as repeatability, and accuracy, expressed as relative standard deviation and relative error, respectively, were lower than 6% in all cases. In the presence of reciprocal interference, the standard addition method considerably improved the resolution of the voltammetric technique. Once set up on the standard reference materials, the analytical procedure was transferred and applied to commercial meals sampled on market for sale. A critical comparison with spectroscopic measurements is also discussed. [source]