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Sample records for pulse stripping voltammetry

  1. Differential Pulse Anodic Stripping Voltammetry for Mercury Determination

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    Vereștiuc Paul C.

    2015-07-01

    Full Text Available In the present work voltammetric investigations have been performed on HgCl2 aqueous solutions prepared from a Cz 9024 reagent. Carbon paste electrode (CPE, eriochrome black T modified carbon paste electrode (MCPE/EBT and KCl 1M as background electrolyte, were involved within the experimental procedures. Cyclic voltammetry (CV has been performed in order to compare the behaviour of the two electrodes in both K3[Fe(CN6] and mercury calibration aqueous solution. Differential pulse anodic stripping voltammetry (DPASV was used to determine the most suitable parameters for mercury determination. All experiments were performed at 25 ± 1 ℃, using an electrochemical cell with three-electrodes connected to an Autolab PG STAT 302N (Metrohm-Autolab potentiostat that is equipped with Nova 1.11 software. The measured potential values were generated by using the silver chloride electrode (AgClE as reference and a platinum wire electrode as auxiliary. A series of time depending equations for the pre-concentration and concentration steps were established, with the observation that a higher sensitivity can be obtained while increasing the pre-concentration time. DPASV were drawn using the CPE in 11.16 % coriander, as mercury complex, the voltamograms signals indicating mercury oxidation, with signal intensity increasing in time.

  2. Differential Pulse Anodic Stripping Voltammetry for Mercury Determination

    OpenAIRE

    2015-01-01

    In the present work voltammetric investigations have been performed on HgCl2 aqueous solutions prepared from a Cz 9024 reagent. Carbon paste electrode (CPE), eriochrome black T modified carbon paste electrode (MCPE/EBT) and KCl 1M as background electrolyte, were involved within the experimental procedures. Cyclic voltammetry (CV) has been performed in order to compare the behaviour of the two electrodes in both K3[Fe(CN)6] and mercury calibration aqueous solution. Differential pulse anodic st...

  3. Pulse Voltammetry.

    Science.gov (United States)

    Osteryoung, Janet

    1983-01-01

    Discusses the nature of pulse voltammetry, indicating that its widespread use arises from good sensitivity and detection limits and from ease of application and low cost. Provides analytical and mechanistic applications of the procedure. (JN)

  4. DIFFERENTIAL PULSE ANODIC STRIPPING VOLTAMMETRY FOR DETERMINATION OF SOME HEAVY METALS IN URANIUM

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    Saryati Saryati

    2010-06-01

    Full Text Available The direct determination of some metals impurity in uranium by using differential pulse anodic stripping voltammetry (DPASV method at a hanging mercury drop electrode and in a carbonate buffer media was developed. It was found that the carbonate buffer show the strongest affinity for uranium and gives the best separation between the DPASV peaks of heavy metals impurities. The carbonate concentration markedly affects the oxidation and reduction the major and the minor constituents of the uranium samples. In 0.1 M carbonate buffer solution pH 10, copper, bismuth, thalium, lead, cadmium, zinc, could be determined without the removal of the uranium matrix. Recovery and relative standard deviation (RSD of this method was in the range of 174% - 85.2% for recovery and 36.8% - 1.2% for RSD. The larger error of analytical result was obtained for Zn at low concentration. In general, the analytic results error and RSD decreased with increasing metals concentration.   Keywords: heavy metal determination, differential pulse anodic stripping voltammetry, uranium

  5. Determination of copper in whole blood by differential pulse adsorptive stripping voltammetry

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    Tarik Attar

    2014-02-01

    Full Text Available A selective and sensitive method for determination of copper in blood by adsorptive differential pulse cathodic stripping voltammetry is presented. The method is based on adsorptive accumulation of the complexes of Cu (II ions with benzenesulfonyl hydrazide onto hanging mercury drop electrode (HMDE, followed by the reduction of the adsorbed species by differential pulse cathodic stripping voltammetry. The effect of various parameters such as supporting electrolyte, concentration of benzenesulfonyl hydrazide, accumulation potential, accumulation time and stirring rate on the selectivity and sensitivity were studied. The optimum conditions for determination of copper include perchloric acid 0.03 M, concentration of benzenesulfonyl hydrazide 7.5×10-5 M, the accumulation potential of -350 mV (vs. Ag/AgCl, the accumulation time of 50 s, and the scan rate of 50 mV s-1. Under optimized conditions, linear calibration curves were established for the concentration of Cu (II in the range of 0.62-275 ng mL-1, with detection limit of 0.186 ng mL-1 for Cu (II. The procedure was successfully applied to the determination of copper ion in whole blood samples.

  6. Determination of trace amounts of morphine in human plasma by anodic adsorptive stripping differential pulse voltammetry

    Institute of Scientific and Technical Information of China (English)

    Ali Niazi; Ateesa Yazdanipour

    2008-01-01

    New adsorptive anodic differential pulse stripping voltammetry method for the direct determination of morphine at trace levels in human plasma of addicts is proposed.The procedure involves an adsorptive accumulation of morphine on a HMDE,followed by oxidation of adsorbed morphine by voltammetry scan using differential pulse modulation.The optimum conditions for the analysis of morphine are pH 10.5,Eacc of - 100 mV (vs.Ag/AgCl),and tacc of 120 s.The peak current is proportional to the concentration of morphine,and a linear calibration graph is obtained at 0.01-3.10 μg mL-1.A relative standard deviation of 1.06% (n=5) was obtained,and the limit of detection was 3 ng mL- 1.The capability of the method for the analysis of real samples was evaluated by the determination of morphine in spiked human plasma and addicts human plasma with satisfactory results.

  7. Estimation of Heavy Metals in Multivitamin Tablets by Differential Pulse Anodic Stripping Voltammetry

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    Kumar Rohit Raj

    2010-01-01

    Full Text Available Differential pulse anodic stripping voltammetry (DPASV was applied for the simultaneous determination of zinc and copper in multivitamin tablet (supradyn and centrum. Determination of the metals was made in ammonium acetate buffer (pH 4.5 with a scan rate of 0.01 V/s by Hanging Mercury Dropping Electrode (HMDE.The solution was stirred during electrolysis at -1.3 V for 300 s in the potential range of -1.3 to + 0.1 V. Concentrations of zinc and copper in supradyn drug sample were found to be 1.80 and 2.9 mg/tablet and for centrum drug sample were found to be 4.6 and 0.94 mg/tablet respectively.

  8. Determination of Selenium in infant formula by differential pulse cathodic stripping voltammetry

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    "Oveisi MR

    2002-07-01

    Full Text Available Selenium as a nonmetallic chemical element has received high attention of biologists because of its dual role as an essential trace nutrient and a toxic element. This interest has created a need for reliable analytical methods for determination of selenium. In this investigation determination of selenium by differential pulse cathodic stripping voltammetry and the influence of various parameters such as deposition potentials, deposition time. Cu concentration pH, etc. on selenium peak in voltammogram are described. Determination of selenium was accomplished in mixture of acetic acid, hydrochloric acid and sodium chloride buffer (pH=1 with a scan rate of 60 mv/s and a pulse height of 100 my by hanging mercury drop electrode (HMDE as working electrode. The solution was stirred during pre-electrolysis at - 350 mv (vs SCE for 30 s and the potential was scanned between - 350 mv and - 800 mv. The determination limit of the method was 0.005 mg/kg for the sample. The calibration curves were linear in the range of 0-30 μg/L (R2=0.996, p<0.001. Repeatability of the method at concentrations of 30 and 0.5 μg/L were 2.5 and 10.5% respectively.

  9. Determination of total gaseous selenium in atmosphere by honeycomb denuder/differential pulse cathodic stripping voltammetry.

    Science.gov (United States)

    Zhang, Bicheng; Xu, Hui; Yu, Jimmy C

    2002-05-16

    A new analytical method has been developed for the determination of total gaseous selenium in the atmosphere by honeycomb denuder collection followed by differential pulse cathodic stripping voltammetry (DPCSV) measurement. Gaseous selenium was collected in a denuder coating solution containing 2% HNO(3) and 2% glycerine. The soluble product, selenious acid, was then extracted by water for DPCSV analysis. The collection efficiency for gaseous selenium was 99.1% at a flow rate of 1 l min(-1) for 3 h. Excellent linearity in DPCSV was maintained up to Se concentration of 40 ng ml(-1). This was equivalent to a working concentration of 220 ng m(-3) of selenium in the atmosphere. A precision of 1.26% RSD (n=5) for 5 ng Se was obtained, and the detection limit (3sigma) and the quantitative determination limit were estimated to be 0.96 and 3.19 ng m(-3). The average recovery of selenium in three standard samples prepared by independent digestion of NIST SRM 1648 (Urban Particulate Matter) using our analytical system was 99.0%. The total content of gaseous selenium in the atmosphere of our laboratories was 3.2-4.4 ng m(-3).

  10. Quantification of sub-nanomolar levels of Penicillin G by differential pulse adsorptive stripping voltammetry.

    Science.gov (United States)

    Abbasi, S; Khodarahmian, K; Farmany, A

    2012-02-01

    A novel selective and sensitive method is developed for determination of Penicillin G by Differential Pulse Adsorptive Stripping Voltammetry (DPAdSV). Penicillin G gave well-resolved diffusion-controlled cathodic peaks at -0.42 and -0.584 V, respectively (vs Ag/AgCl) in pH 7.50 of borate buffer. Optimal conditions were obtained as pH 7.50, accumulation potential of -0.2 V (vs Ag/AgCl), accumulation time of 120 s, and scan rate of 100 mV/s. Under the optimized conditions, a linear calibration curve was established for the concentration of Penicillin G in the range of 0.007-2.13 µg/ml with a detection limit of 0.000717 µg/ml. The procedure was successfully applied to the determination of Penicillin G in various medicine and biological samples. The relative standard deviation of the method at 0.05 and 0.5 µg/ml Penicillin G, for 10 runs, was 2.55% and 2.06%, respectively. Copyright © 2011 John Wiley & Sons, Ltd.

  11. Differential pulse and square-wave cathodic stripping voltammetry of xanthine and xanthosine at a mercury electrode.

    Science.gov (United States)

    Temerk, Y M; Kamal, M M; Ahmed, G A W; Ibrahim, H S M

    2003-08-01

    The surface activity of xanthine (Xan) and xanthosine (Xano) at a hanging mercury drop electrode (HMDE) was studied using out-of-phase ac and cyclic dc voltammetry. The results show that Xan and Xano were strongly adsorbed and chemically interacted with the charged mercury surface, which is the prerequisite step for applying the cathodic adsorptive stripping voltammetric determination of such biologically important compounds. Differential pulse cathodic adsorptive stripping voltammetry (DPCASV) and square-wave cathodic adsorptive stripping voltammetry (SWCASV) were applied for the ultratrace determination of Xan and Xano compounds. Moreover, a rapid and sensitive controlled adsorptive accumulation of Cu(II) complexes of both compounds provided the basis of a direct stripping voltammetric determination of such compounds to submicromolar and nanomolar levels. Operational and solution conditions for the quantitative ultratrace determination of Xan and Xano were optimized in absence and presence of Cu(II). The calibration curve data were subjected to least-squares refinements. The effects of several types of inorganic and organic interfering species on the determination of Xan or Xano were considered.

  12. Cathodic adsorptive stripping voltammetry of drotaverine hydrochloride and its determination in tablets and human urine by differential pulse voltammetry.

    Science.gov (United States)

    Zayed, S I M; Issa, Y M

    2009-04-01

    The stripping voltammetric behaviour of drotaverine hydrochloride (DvCl) was studied using a hanging mercury drop electrode (HMDE). The adsorptive stripping response has been evaluated with respect to pH, accumulation time, accumulation potential, scan rate and other variables. Differential pulse DP mode; over the potential range -400 to -1200 mV, is used in the presence of 0.04 M Britton-Robinson buffer pH 2. Cyclic voltammetric study indicates that the reduction process is irreversible and controlled by adsorption. The response of DP technique is linear over the concentration range 21.70-257.34 ng/ml. Limit of detection and limit of quantification were 3.15 and 10.50 ng/ml, respectively. The proposed method was successfully applied for the determination of the drug in commercial tablets and spiked human urine samples.

  13. Aptasensors Based on Stripping Voltammetry

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    Wenjing Qi

    2016-07-01

    Full Text Available Aptasensors based on stripping voltammetry exhibit several advantages, such as high sensitivity and multi-target detection from stripping voltammetric technology, and high selectivity from the specific binding of apamers with targets. This review comprehensively discusses the recent accomplishments in signal amplification strategies based on nanomaterials, such as metal nanoparticles, semiconductor nanoparticles, and nanocomposite materials, which are detected by stripping voltammetry after suitable dissolution. Focus will be put in discussing multiple amplification strategies that are widely applied in aptasensors for small biomolecules, proteins, disease markers, and cancer cells.

  14. Determination of selenium in natural waters by adsorptive differential pulse cathodic stripping voltammetry.

    Science.gov (United States)

    Ashournia, Mehdi; Aliakbar, Alireza

    2009-08-30

    In this work bovine albumin was used innovatively as a medium for adsorptive accumulation of Se-I(2) on thin mercury film electrode. Se-I(2) was formed by reaction between Se(IV) and iodide in HCl media. The adsorbed Se-I(2) was stripped in 0.05 M HCl by differential pulse cathodic potential scan. The proposed method was successfully applied to analysis of Se(IV) and Se(VI) in natural waters sampled from some lagoons south of Caspian Sea. The optimum reaction conditions and other analytical parameters and influence of cations and anions were studied. The detection limit was 0.37 ng mL(-1). The obtained results were compared with the results of DPCSV after electrochemical preconcentration, HG-AAS and ICP-AES.

  15. Extending the dynamic range of copper determination in differential pulse adsorption cathodic stripping voltammetry using wavelet neural network.

    Science.gov (United States)

    Khayamian, T; Ensafi, Ali A; Benvidi, A

    2006-07-15

    A wavelet neural network (WNN) model is proposed for extending the dynamic range of Cu(II) determination by differential pulse adsorption cathodic stripping voltammetry (DP-AdSV) using xylenol orange (XO) as a suitable ligand. All of voltammograms data consisting of Cu(II) and Cu(II)-XO peak currents were used in WNN model. The WNN model consisted of three layers (2-8-1) with the Morlet mother wavelet transfer function in the hidden layer. The model was able to extend the dynamic range of Cu(II) from its narrow linear range (1-50 ng ml(-1)) to the higher dynamic range (1-1500 ng ml(-1)). The results of the WNN model was also compared with artificial neural network (ANN) model and it was demonstrated the superiority of the WNN model relative to ANN model.

  16. Evaluation of metal fractions in river sediments and waters: application of chelation chromatography-differential pulse anodic stripping voltammetry.

    Science.gov (United States)

    Sundd, S; Prasad, B B

    1995-10-01

    The ability of chelation chromatography in combination with differential pulse anodic stripping voltammetry (DPASV) to provide a simple, fast and reliable way of dealing with interionic interferences, competitive complexations, re-adsorption of released metal ions and sorption of spiking metal ions by organic/inorganic materials in the complex matrixes of real natural samples has been critically examined. The technique is based on the selective complexation of target metal fractions on some novel sorbents which are polymeric chelating resins doped on stationary supports (Whatman No. 1 paper and silica gel). The usual complications of leaching of the resin and/or the chelating ligand and colloid retention on the sorption bed at any stage of separation were largely obviated with these sorbents under the operational conditions of metal sorption. A detailed study on the application of such sorbents to the differentiation of ionic (free), labile (ionic plus weakly complexed) and bound (strongly complexed) metal fractions present in local river-sediment and water samples was carried out. Chelating resin-impregnated paper (CRIP) and chelating resin-immobilized silica gel column (CRISC) methods of chromatographic separation of analyte trace metals in combination with the follow-up 'standard addition' procedure of the DPASV technique were employed. A modest attempt has been made to formulate a speciation (fractionation) scheme for metal contents present in river-sediments and waters on the basis of selective retention of ionic and labile fractions on complexing resins.

  17. The Graphene/l-Cysteine/Gold-Modified Electrode for the Differential Pulse Stripping Voltammetry Detection of Trace Levels of Cadmium

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    Yu Song

    2016-06-01

    Full Text Available Cadmium(II is a common water pollutant with high toxicity. It is of significant importance for detecting aqueous contaminants accurately, as these contaminants are harmful to human health and environment. This paper describes the fabrication, characterization, and application of an environment-friendly graphene (Gr/l-cysteine/gold electrode to detect trace levels of cadmium (Cd by differential pulse stripping voltammetry (DPSV. The influence of hydrogen overflow was decreased and the current response was enhanced because the modified graphene extended the potential range of the electrode. The Gr/l-cysteine/gold electrode showed high electrochemical conductivity, producing a marked increase in anodic peak currents (vs. the glass carbon electrode (GCE and boron-doped diamond (BDD electrode. The calculated detection limits are 1.15, 0.30, and 1.42 µg/L, and the sensitivities go up to 0.18, 21.69, and 152.0 nA·mm−2·µg−1·L for, respectively, the BDD electrode, the GCE, and the Gr/l-cysteine/gold electrode. It was shown that the Gr/l-cysteine/gold-modified electrode is an effective means for obtaining highly selective and sensitive electrodes to detect trace levels of cadmium.

  18. Application of differential pulse stripping voltammetry and chemometrics for the determination of three antibiotic drugs in food samples

    Institute of Scientific and Technical Information of China (English)

    Yong Sheng Zhong; Yong Nian Ni; Serge Kokot

    2012-01-01

    A reliable method for simultaneous determination of three antibiotic drugs (levottoxacin,gatifloxacin and lomefloxacin) by differential pulse stripping voltammetry (DPSV) in Britton-Robinson buffer (pH 7.96) was presented.The method is based on adsorptive accumulation of the antibacterial drugs on a hanging mercury dropping electrode (HMDE),followed by the reduction of the adsorptive species by the technique of DPSV.Optimal conditions,the deposition time of 80 s,the deposition potential of - 1250 mV,and the scan rate of 25 mV/s,were obtained.The linear concentration ranges of 0.010-0.080 μg/mL were obtained for all these three antibiotic drugs,while the detection limits were 2.38,3.20 and 1.60 ng/mL for levofloxacin,gatifloxacin and lomefloxacin,respectively.In this work,chemometrics methods,such as classical least squares (CLS),partial least squares (PLS),principle component regression (PCR) and radial basis function-artificial neural networks (RBF-ANN),were used to quantitatively resolve the overlapping signals.It was found that PCR gave the best results with total relative prediction error (RPEr) of 7.71%.The proposed method was applied to determine these three drugs in several commercial food samples with spiked method and yielded satisfactory recoveries.

  19. SENSING OF PROSTATE SPESIFIC ANTIGEN BY DIFFERENTIAL PULSE ANODIC STRIPPING VOLTAMMETRY OF GOLD NANOPARTICLE - SILVER ENHANCED LABELS

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    Rika Endara Safitri

    2016-09-01

    Full Text Available A sensitive prostate specific antigen (PSA detection method based on peptide cleavage and silver enhancement of gold nanoparticle (AuNP has been developed. PSA is serine protease produced by both normal prostate glandular cells and prostate cancer cells. PSA widely used as a biomarker for prostate cancer (PCa. The activity of PSA was detected by following mechanism: first, some immobilized peptide on the bottom of wellplate was undergo cleaving process via biotin-avidin interaction, leaving short peptide (without thiol group that could not form a link with gold nanoparticle. Meanwhile, the remaining peptide which not undergo such process could self-assemble with AuNPs, followed by autocatalytic reduction with silver enhancement solutions to silver metal (Ag. The Ag content on AuNPs was determined by differential pulse anodic stripping voltammetry, after axidation of Ag metal to Ag+ ions, using screen printed carbon electrode. The measurement conditions and immunoassay components had been optimized in this study. The detection of PSA was successfully carried out by this method with limit detection value of 152.204 ng/mL, but further development is necessary to improve the limit detection value.

  20. Direct determination of praziquantel in pharmaceutical formulations and human plasma by cathodic adsorptive stripping differential-pulse voltammetry.

    Science.gov (United States)

    Ghoneim, M M; Mabrouk, M M; Tawfik, A

    2002-11-07

    The polarographic and cyclic voltammetric behaviour of praziquantel was studied in B.R. buffers of different pH values. Contradictory to that mentioned in a previously published work, praziquantel is an electro-active compound. Its polarogram exhibited a single 2-electron irreversible reduction wave in B.R. buffer of pH 5, the wave height decreased on the increase of pH till it disappeared in solution of pH >7. This wave was attributed to the reduction of the Cz.dbnd6;O double bond. The quantitative trace determination of bulk praziquantel was studied at a hanging mercury drop electrode by cathodic adsorptive stripping differential-pulse voltammetry. A fully validated sensitive procedure based on controlled adsorptive accumulation of the drug onto a HMDE was developed for its direct determination without derivatization. Accumulation of praziquantel was found to be optimized in 0.1 M Na(2)SO(4) solution as supporting electrolyte under the following conditions: accumulation potential, -1.2 V (vs. Ag/AgCl/KCl(s)); accumulation time, 30 s; scan rate, 10 mV/s and pulse height 100 mV. The proposed procedure was applied successfully for determination of praziquantel in its pharmaceutical formulations and human plasma. The mean recoveries of the drug were 98.85-99.42% and 99.12-100.47% with RSD of 0.49-0.95% and 0.45-0.52% in pharmaceutical formulations and human plasma, respectively. Limits of detection and quantitation of 1.14x10(-9) and 3.80x10(-9) M praziquantel, respectively, were achieved.

  1. Inorganic arsenic speciation by differential pulse anodic stripping voltammetry using thoria nanoparticles-carbon paste electrodes.

    Science.gov (United States)

    Pereira, F J; Vázquez, M D; Debán, L; Aller, A J

    2016-05-15

    Two novel thoria (ThO2) nanoparticles-carbon paste electrodes were used to evaluate an anodic stripping voltammetric method for the direct determination of arsenite and total inorganic arsenic (arsenite plus arsenate) in water samples. The effect of Ag((I)), Cu((II)), Hg((II)), Sb((III)) and Se((IV)) ions on the electrochemical response of arsenic was assayed. The developed electroanalytical method offers a rapid procedure with improved analytical characteristics including good repeatability (3.4%) at low As((III)) concentrations, high selectivity, lower detection limit (0.1 μg L(-1)) and high sensitivity (0.54 μA μg(-1) L). The analytical capability of the optimized method was demonstrated by the determination of arsenic in certified reference materials (trace elements in natural water, trace elements in water and coal fly ash).

  2. Determination of para-arsanilic acid with improved diazotization reaction using differential pulse cathodic stripping voltammetry in aqueous system.

    Science.gov (United States)

    Misni, Marpongahtun; Sathishkumar, Palanivel; Ahamad, Rahmalan; MohdYusoff, Abdull Rahim

    2015-01-01

    Para-arsanilic acid (p-ASA) has been widely used in the poultry industry to promote growth and prevent dysentery. It is excreted unchanged in the manure and released into non-target sites causing organoarsenic pollution risk to the environment and living system. Therefore, simple and effective analytical strategies are demanded for determining the samples that contain p-ASA. However, direct determination of both p-ASA and ortho-arsanilic acid (o-ASA) using differential pulse cathodic stripping voltammetry (DPCSV) gives the similar voltammograms that directly hamper the analysis used by the DPCSV technique. In this study, a method to determine and differentiate p-ASA from o-ASA via diazotization and coupling reaction of the amine groups followed by the direct DPCSV determination of diazo compounds is presented. The diazotization reaction carried out at pH 1.5 and 0 ± 1°C for 10 min showed two reduction peaks in DPCSV at-70 mV and -440 mV vs. Ag/AgCl (KCl 3 M). However, when the diazotization reaction was performed at pH 12.5 and 0 ± 1°C for 40 min, a coloured azo compound was produced and the DPCSV showed only one reduction peak that appeared at -600 mV vs. Ag/AgCl (3 M of KCl). The results of this study show that only p-ASA compound gave a reduction peak, whereas o-ASA compound did not give any peak. The detection limit of p-ASA was found to be 4 × 10(-8 )M. As a result, the proposed electro-analytical technique might be a good candidate to determine and differentiate the p-ASA present in the poultry and environmental samples.

  3. Strategy for copper speciation in white wine by differential pulse anodic stripping voltammetry, potentiometry with an ion-selective electrode and kinetic photometric determination

    Energy Technology Data Exchange (ETDEWEB)

    Wiese, C. [Inst. fuer Anorganische und Analytische Chemie, Technische Univ. Clausthal, Clausthal-Zellerfeld (Germany); Schwedt, G. [Inst. fuer Anorganische und Analytische Chemie, Technische Univ. Clausthal, Clausthal-Zellerfeld (Germany)

    1997-07-01

    Differential pulse anodic stripping voltammetry (DPASV), potentiometry with a copper ion-selective electrode and a kinetic photometric method were used to determine copper species in white wines. The kinetic method is based on the catalytic effect of labile copper(II) species on the oxidation of 3-hydroxybenzaldehyde azine by potassium peroxidisulfate in an ammonical medium at room temperature. The total copper concentrations were determined by flame atomic absorption spectrometry. Free copper(II) ions, labile and tightly bound copper species could be quantified in 16 non pre-treated wine samples. (orig.). With 3 figs., 5 tabs.

  4. Determination of Cr (in small quantities) by adsorptive stripping voltammetry: a comparative study of square wave versus differential pulse

    Energy Technology Data Exchange (ETDEWEB)

    Misiego, A.Sanchez; Carra, R.M.Garcia-Monco; Carracedo, P.Ambel; Torre, M.E.Majado [Departamento de Quimica Analitica y Electroquimica, Universidad de Extremadura, 06071, Badajoz (Spain)

    2003-08-01

    The usefulness of an analytical method must be measured according to its practical application possibilities. A comparative study has been carried out here between the SW (working in an open atmosphere) and DP (working with de-aerated solutions) variants of catalytic-stripping adsorptive voltammetry applied to the determination of chromium traces in triethylenetetraminehexaacetic acid (TTHA) medium. In order to optimise the analytical signal, accumulation potential, nitrate ion concentration, pH, and TTHA concentration parameters were evaluated. Four linearity ranges were established within the interval 0.5-2000 nmol L{sup -1} chromium concentration in the cell, each with the recommended accumulation time. Quality parameters such as repeatability, linear regression, validity limits, precision, and sensitivity were evaluated. The SW variant is significantly advantageous when the chromium concentration in cell is less than 10 nmol L{sup -1} and even more if analysis time, cost, and being able to work in an open atmosphere are considered. The results are comparable to those obtained using GTAAS. Employing a CRM (tomato leaves), the accuracy is 1-4%. The proposed procedure, using tree leaves as samples, has been successfully tested for the possible monitoring of chromium contamination of the atmosphere. (orig.)

  5. Anodic Stripping Voltammetry: An Instrumental Analysis Experiment.

    Science.gov (United States)

    Wang, Joseph

    1983-01-01

    Describes an experiment designed to acquaint students with the theory and applications of anodic stripping voltammetry (ASV) as well as such ASV problems as contamination associated with trace analysis. The experimental procedure, instrumentation, and materials discussed are designed to minimize cost and keep procedures as simple as possible. (JM)

  6. Copper determination in ethanol fuel by differential pulse anodic stripping voltammetry at a solid paraffin-based carbon paste electrode modified with 2-aminothiazole organofunctionalized silica.

    Science.gov (United States)

    Takeuchi, Regina M; Santos, André L; Padilha, Pedro M; Stradiotto, Nelson R

    2007-02-15

    Solid paraffin-based carbon paste electrodes modified with 2-aminothiazole organofunctionalized silica have been applied to the anodic stripping determination of copper ions in ethanol fuel samples without any sample treatment. The proposed method comprised four steps: (1) copper ions preconcentration at open circuit potential directly in the ethanol fuel sample; (2) exchange of the solution and immediate cathodic reduction of the absorbate at controlled potential; (3) differential pulse anodic stripping voltammetry; (4) electrochemical surface regeneration by applying a positive potential in acid media. Factors affecting the preconcentration, reduction and stripping steps were investigated and the optimum conditions were employed to develop the analytical procedure. Using a preconcentration time of 20min and reduction time of 120s at -0.3V versus Ag/AgCl(sat) a linear range from 7.5x10(-8) to 2.5x10(-6)mol L(-1) with detection limit of 3.1x10(-8)mol L(-1) was obtained. Interference studies have shown a decrease in the interference effect according to the sequence: Ni>Zn>Cd>Pb>Fe. However, the interference effects of these ions have not forbidden the application of the proposed method. Recovery values between 98.8 and 102.3% were obtained for synthetic samples spiked with known amounts of Cu(2+) and interfering metallic ions. The developed electrode was successfully applied to the determination of Cu(2+) in commercial ethanol fuel samples. The results were compared to those obtained by flame atomic absorption spectroscopy by using the F-test and t-test. Neither F-value nor t-value have exceeded the critical values at 95% confidence level, confirming that there are no significant differences between the results obtained by both methods.

  7. Anodic stripping voltammetry enhancement by redox magnetohydrodynamics.

    Science.gov (United States)

    Clark, Emily A; Fritsch, Ingrid

    2004-04-15

    The effect of an external magnetic field on linear scan anodic stripping voltammetry (ASV) in solutions of 10(-6)-10(-7) M concentrations of lead, cadmium, and copper at mercury films on glassy carbon electrodes has been investigated. A high concentration of Hg(2+) was added to the analyte solution to induce a large cathodic current during the deposition step. Therefore, a large Lorentz force from the net flux of charge through the magnetic field resulted in convection due to magnetohydrodynamics. The faster delivery of analytes to the mercury film electrode during deposition caused an increase in the anodic stripping peaks. The effect of varying Hg(2+) concentrations (0-60 mM) and magnetic field strengths (0-1.77 T) on the enhancement of the stripping peaks was investigated. Enhancements as large as 129% for peak currents and 167% for peak areas were observed. An enhancement of approximately 100% was observed when 60 mM Fe(3+) replaced high concentrations of Hg(2+). This method of convection exhibits promise for small-volume ASV analysis with possible improved limits of detection and decreased preconcentration times.

  8. Determination of chitosan by cathodic stripping voltammetry.

    Science.gov (United States)

    Lu, Guanghan; Wang, Lirong; Wang, Ruixia; Zeng, Yan; Huang, Xi

    2006-04-01

    A sensitive method for the determination of chitosan (CTS) by cathodic stripping voltammetry is presented. The method exploits a pair of oxidation-reduction peaks of CTS at -0.62 V (vs. SCE) and -0.54 V (vs. SCE), and an enhancement of the peak current of CTS observed in a 0.05 mol l(-1) potassium hydrogenphthalate buffer solution (pH 2.5). The peak current is linear with the concentration of CTS from 5.0 x 10(-7) to 1.5 x 10(-5) g ml(-1), and the detection limit is 1.0 x 10(-7) g ml(-1). We studied the characteristics and the mechanism of the electrode reaction, which proved that this process was diffusion controlled. This method was applied to determine the content of CTS in real samples with satisfactory results.

  9. Differential pulse anodic stripping voltammetry for detection of As (III) by Chitosan-Fe(OH)3 modified glassy carbon electrode: A new approach towards speciation of arsenic.

    Science.gov (United States)

    Saha, Suparna; Sarkar, Priyabrata

    2016-09-01

    An efficient electrochemical sensor for As(III) was developed based on adsorption of arsenic on a specially modified electrodes at some applied potential and subsequent i) stripping at a fixed potential by anodic stripping voltammetry ii) analysis by generating surface plasmon resonance (SPR). The working glassy carbon electrode was modified by Chitosan-Fe(OH)3 composite and a reducing agent L-cysteine. The composite enhanced adsorption of As(III) and subsequent reduction to As(O) moieties and measurement by anodic stripping. The surface property of modified electrode was characterized by SEM, AFM, FTIR, XPS and electrochemistry was analyzed by impedance spectroscopy (EIS). Surface Plasmon resonance (SPR) was also employed to investigate the As(III) binding capability of polymer matrix. Several optimum voltammetric parameters e.g supporting electrolyte; 0.1M acetate buffer (pH 5.2) deposition potential, -0.9V; deposition time, 100s were established for anodic stripping voltammetry (ASV). A linear correlation was obtained in the range of 2-100ppb for ASV (R(2) 0.974) with limit of detection 0.072ppb. A variety of common coexistent ions such as Mn, Zn, Pb, Cu, Cd in water samples showed no interferences on the As (III) determination. The method was applied successfully to real samples collected from arsenic affected areas of West Bengal, India.

  10. Determination of ultra-trace amounts of silver in water by differential pulse anodic stripping voltammetry using a new modified carbon paste electrode.

    Science.gov (United States)

    El-Mai, Hafida; Espada-Bellido, Estrella; Stitou, Mostafa; García-Vargas, Manuel; Galindo-Riaño, Maria Dolores

    2016-05-01

    A highly sensitive and selective new procedure for the determination of silver in aqueous media was developed using a modified carbon paste electrode (MCPE) by differential pulse anodic stripping voltammetry (DPASV). The modified electrode was based on the incorporation of 2-hydroxybenzaldehyde benzoylhydrazone (2-HBBH) in the carbon paste electrode. Silver ions were preconcentrated on the modified electrode at open-circuit by complexation with the ligand and reduced to zero valent at a potential of 0V, and followed by the reoxidation of adsorbed ions onto the electrode by scanning the potential in a positive direction. The oxidation peak of Ag(I) was observed at 0.2V (versus Ag/AgCl). The analysis of Ag(I) was carried out in a cell containing the sample solution (20mL) buffered by 0.1molL(-1) K2HPO4/NaOH at pH 5.5 in aqueous solution and nitric acid (pH 1) in real water samples. The optimum conditions for the analysis of silver include a reduction potential of 0V and a pulse amplitude of 100mV, among others. The optimum carbon paste composition was found to be 14.1% (w/w) 2-HBBH, 56.2% (w/w) graphite powder and 29.7% (w/w) paraffin oil. Differential pulse anodic stripping voltammetric response was used as the analytical signal. Under the selected conditions, the voltammetric signal was proportional to the Ag(I) concentration in the range of 0.001-100μgL(-1) with favorable limits of detection and quantification of 1.1ngL(-1) and 3.7ngL(-1) after 3min of accumulation time, respectively. By increasing the accumulation time to 10min, detection and quantification limits can be further improved up to 0.1ngL(-1) and 0.34ngL(-1), respectively. In addition, the results showed a highly reproducible procedure showing a relative standard deviation of 1.5% for 12 replicate measurements. Many coexisting metal ions were investigated and very few interferences were found on the determination of Ag(I). The proposed method was validated using certified reference estuarine waters

  11. Cathodic adsorptive stripping square-wave voltammetry of the anti-inflammatory drug meloxicam.

    Science.gov (United States)

    Radi, A E; Ghoneim, M; Beltagi, A

    2001-10-01

    The adsorptive behavior of the anti-inflammatory drug meloxicam was studied by cyclic, differentia-pulse and square-wave voltammetry on a hanging mercury drop electrode (HMDE). The drug was accumulated at HMDE and a well-defined stripping peak current was obtained at -1.42 V vs. Ag/AgCl (saturated KCl) electrode in acetate buffer solution (pH 5.0). A voltammetric procedure was developed for the determination of meloxicam using square-wave cathodic adsorptive stripping voltammetry (SW-CASV). The optimum working conditions for the determination of the drug were established. The analysis of meloxicam in human plasma was carried out satisfactorily.

  12. Self-doped anthranilic acid-pyrrole copolymer/gold electrodes for selective preconcentration and determination of Cu(I) by differential pulse anodic stripping voltammetry.

    Science.gov (United States)

    Nateghi, M R; Fallahian, M H

    2007-05-01

    Electropolymerization of anthranilic acid/pyrrole (AA/PY) at solid substrate electrodes (platinum, gold, and glassy carbon) gave stable and water-insoluble films under a wide range of pH. Combining high conductivity of the polypyrrole (PPY) and pH independence of the electrochemical activity of the self-doped carboxylic acid-substituted polyaniline allows us to prepare an improved functionalized PPY-modified electrode to collect and measure Cu(I) species. The differential pulse stripping analysis of the copper ions using a polyanthranilic acid-co-polypyrrole (PAA/PPY)-modified electrode consisted of three steps: accumulation, electrochemical reduction to the elemental copper and stripping step. Factors affecting these steps, including electropolymerization conditions, accumulation and stripping medium, reduction potential, reduction time and accumulation time, were systematically investigated. A detection limit of 5.3 x 10(-9) M Cu(I) was achieved for a 7.0 min accumulation. For 12 determinations of Cu(I) at concentrations of 1.0 x 10(-8) M, an RSD of 3.5% was obtained. The log I(p) was found to vary linearly with log[Cu(I)] in the concentration range from 7.0 x 10(-9) to 1.0 x 10(-5) M.

  13. Analytical possibilities of microelectrode use for stripping voltammetry

    Energy Technology Data Exchange (ETDEWEB)

    Matysik, F.M. (Leipzig Univ. (Germany). Dept. of Chemistry); Glaeser, P. (Leipzig Univ. (Germany). Dept. of Chemistry); Werner, G. (Leipzig Univ. (Germany). Dept. of Chemistry)

    1994-07-01

    The analytical utility of microelectrodes for stripping voltammetry is discussed from several points of view. The application of microelectrodes for microanalysis is demonstrated using a novel capillary flow injection system. Heavy metals at [mu]g l[sup -1] concentrations have been determined in [mu]l-samples. The influence of electrode size and convection during the deposition period of anodic stripping voltammetry on the reproducibility of trace metal determination was studied for various types of electrodes. In the case of mercury film microelectrodes, the precision can be improved if the accumulation of the analyte is performed under quiescent conditions. Practical examples of stripping voltammetry with microelectrodes such as copper determination in whisky and trace metal measurements in drinking water are given. (orig.)

  14. Manganese detection in marine sediments: anodic vs. cathodic stripping voltammetry.

    Science.gov (United States)

    Banks, Craig E; Kruusma, Jaanus; Moore, Ryan R; Tomcík, Peter; Peters, Judith; Davis, James; Komorsky-Lovrić, Sebojka; Compton, Richard G

    2005-01-30

    Three different electroanalytical techniques for the detection of manganese in marine sediments are evaluated. The anodic stripping voltammetry of manganese at an in situ bismuth-film-modified boron-doped diamond electrode and cathodic stripping voltammetry at a carbon paste electrode are shown to lack the required sensitivity and reproducibility whereas cathodic stripping voltammetry at a bare boron-doped diamond electrode is shown to be reliable and selective with a limit of detection, from applying a 60s accumulation period of 7.4 x 10(-7)M and a sensitivity of 0.24AM(-1). The method was used to evaluate the manganese content of marine sediments taken from Sibenik, Croatia.

  15. Trace analysis of Ponceau 4R in soft drinks using differential pulse stripping voltammetry at SWCNTs composite electrodes based on PEDOT:PSS derivatives.

    Science.gov (United States)

    Wang, Zifei; Zhang, Hui; Wang, Zhipeng; Zhang, Jie; Duan, Xuemin; Xu, Jingkun; Wen, Yangping

    2015-08-01

    Ponceau 4R, an edible synthetic colorant used in drinks, syrups, and sweets, has been successfully detected using differential pulse voltammetry at a single-walled carbon nanotubes-modified composite electrode based on poly(3,4-ethylenedioxythiophene):poly(styrene sulfonate) and two derivatives thereof. The electrochemical parameters of three Ponceau 4R sensors, such as pH value, pre-concentration time, and scan rate, have been optimized, and their electrochemical performances have been compared. A poly(acrylate-modified 3,4-ethylenedioxythiophene-co-3,4-ethylenedioxythiophene):poly(styrene sulfonate)-single-walled carbon nanotubes-poly(vinyl alcohol)-modified electrode showed the best electrocatalytic activity, with the highest response current, lowest detection limit (1.8 nm), widest linear range (0.0055-110.6 μm), and best sensing stability. Additionally, the modified electrode has also been successfully employed for real sample analysis with soft drinks. Satisfactory results were obtained, demonstrating this to be an easy and effective approach for trace analysis of Ponceau 4R in food samples.

  16. Simultaneous determination of trace Cd(II), Pb(II) and Cu(II) by differential pulse anodic stripping voltammetry using a reduced graphene oxide-chitosan/poly-l-lysine nanocomposite modified glassy carbon electrode.

    Science.gov (United States)

    Guo, Zhuo; Li, Dong-di; Luo, Xian-Ke; Li, Ya-Hui; Zhao, Qi-Nai; Li, Meng-Meng; Zhao, Yang-Ting; Sun, Tian-Shuai; Ma, Chi

    2017-03-15

    The reduced graphene oxide (RGO) and Chitosan (CS) hybrid matrix RGO-CS were coated onto the glassy carbon electrode (GCE) surface, then, poly-l-lysine films (PLL) were prepared by electropolymerization with cyclic voltammetry (CV) method to prepare RGO-CS/PLL modified glassy carbon electrode (RGO-CS/PLL/GCE) for the simultaneous electrochemical determination of heavy metal ions Cd(II), Pb(II) and Cu(II). Combining the advantageous features of RGO and CS, RGO and CS are used together because the positively charged CS can interact with the negatively changed RGO to prevent their aggregation. Furthermore, CS has many amino groups along its macromolecular chains and possessed strongly reactive with metal ions. Moreover, PLL modified electrodes have good stability, excellent permselectivity, more active sites and strong adherence to electrode surface, which enhanced electrocatalytic activity. The RGO-CS/PLL/GCE was characterized voltammetrically using redox couples (Fe(CN)6(3-/4-)), complemented with electrochemical impedance spectroscopy (EIS). Differential pulse anodic stripping voltammetry (DPASV) has been used for the detection of Cd(II), Pb(II) and Cu(II). The detection limit of RGO-CS/PLL/GCE toward Cd(II), Pb(II) and Cu(II) is 0.01μgL(-1), 0.02μgL(-1) and 0.02μgL(-1), respectively. The electrochemical parameters that exert influence on deposition and stripping of metal ions, such as supporting electrolytes, pH value, deposition potential, and deposition time, were carefully studied.

  17. Differential pulse voltammetry and additive differential pulse voltammetry with solvent polymeric membrane ion sensors.

    Science.gov (United States)

    Ortuño, J A; Serna, C; Molina, A; Gil, A

    2006-12-01

    The ion transfer across the water-solvent polymeric membrane interface is investigated by using a new device based on a modification of a commercial ion-selective electrode body that permits the accommodation of a platinum counter electrode inside the inner filling solution compartment and, therefore, use of a four-electrode potentiostat with ohmic drop compensation. This device is used here to apply two different double potential pulse techniques--differential pulse voltammetry and additive differential pulse voltammetry--which are more advantageous than other voltammetric techniques, such as normal pulse voltammetry or cyclic voltammetry, for the determination of the characteristic electrochemical parameters of the system. This is due to the concurrence of two factors in these double potential pulse techniques, the peak-shaped response together with a considerable reduction of undesirable current contributions.

  18. Anodic stripping voltammetry of silver nanoparticles: aggregation leads to incomplete stripping.

    Science.gov (United States)

    Cloake, Samantha J; Toh, Her Shuang; Lee, Patricia T; Salter, Chris; Johnston, Colin; Compton, Richard G

    2015-02-01

    The influence of nanoparticle aggregation on anodic stripping voltammetry is reported. Dopamine-capped silver nanoparticles were chosen as a model system, and melamine was used to induce aggregation in the nanoparticles. Through the anodic stripping of the silver nanoparticles that were aggregated to different extents, it was found that the peak area of the oxidative signal corresponding to the stripping of silver to silver(I) ions decreases with increasing aggregation. Aggregation causes incomplete stripping of the silver nanoparticles. Two possible mechanisms of 'partial oxidation' and 'inactivation' of the nanoparticles are proposed to account for this finding. Aggregation effects must be considered when anodic stripping voltammetry is used for nanoparticle detection and quantification. Hence, drop casting, which is known to lead to aggregation, is not encouraged for preparing electrodes for analytical purposes.

  19. Hyphenation of ionic liquid albumin glassy carbon biosensor or protein label-free sensor with differential pulse stripping voltammetry for interaction studies of human serum albumin with fenoprofen enantiomers.

    Science.gov (United States)

    Abd El-Hady, Deia; Youssef, Ahmed K

    2013-04-15

    A new biosensor or protein label-free sensor composed of 1-butyl-3-methylimidazolium hexafluorophosphates (BMIMPF6)-human serum albumin (HSA) film on glassy carbon electrode (GCE) was produced. Unfortunately, the native proteins themselves are often unstable in physiological conditions. Here, we introduced conjugation with ionic liquid (IL) such as BMIMPF6 which improved the stability and binding affinity of protein onto GCE. A rapid, simple and reliable method for the chiral discrimination and real time protein binding studies of fenoprofen enantiomers with HSA was developed by hyphenating ionic liquid albumin glassy carbon (ILAGC) biosensor with differential pulse cathodic stripping voltammetry under physiological conditions. The electrochemical behavior of chiral fenoprofen was monitored by cyclic voltammetry, from which large response was obtained from l-fenoprofen. The surface coverage of fenoprofen enantiomers was calculated by double potential-step chronocoulometry. The binding constants of chiral fenoprofen with HSA were estimated to be 3.2×10(5)±0.3 L mol(-1) and 0.8×10(4)±0.4 L mol(-1) for L- and D-fenoprofen, respectively giving acceptable precision (SD ≤ 0.4) and good agreement with the literature values. The competitive interactions of ibuprofen with fenoprofen enantiomers-HSA were studied giving a significant decreasing in the binding degrees of analytes to HSA. The reciprocal competitive experiments indicated that L-fenoprofen replaced D-fenoprofen from HSA. The proposed electrochemical biosensor holds great potential for chiral discrimination and real time binding studies of drugs with protein. Copyright © 2013 Elsevier B.V. All rights reserved.

  20. Adsorptive stripping voltammetry of antibiotics rifamycin SV and rifampicin at renewable pencil electrodes.

    Science.gov (United States)

    Kawde, Abdel-Nasser; Temerk, Yassein; Farhan, Nasser

    2014-01-01

    Adsorptive stripping voltammetry of antibiotics of rifamycin SV (RSV) and rifampicin (RIF) was investigated by cyclic voltammetry and differential pulse voltammetry using a renewable pencil graphite electrode (PGE). The nature of the oxidation process of RSV and RIF taking place at the PGE was characterized. The results show that the determination of highly sensitive oxidation peak current is the basis of a simple, accurate and rapid method for quantification of RSV and RIF in bulk forms, pharmaceutical formulations and biological fluids by differential pulse adsorptive stripping voltammetry (DPASV). Factors influencing the trace measurement of RSV and RIF at PGE are assessed. The limits of detection for the determination of RSV and RIF in bulk forms are 6.0 × 10(-8) mol/L and 1.3 × 10(-8) mol/L, respectively. Moreover, the proposed procedure was successfully applied to assay both RSV and RIF in pharmaceutical formulations and in biological fluids. The capability of the proposed procedure for simultaneous assay of antibiotics RSV-isoniazid and RIF-isoniazid was achieved. The statistical analysis and calibration curve data for trace determination of RSV and RIF are reported.

  1. Determination of mobile form contents of Zn, Cd, Pb and Cu in soil extracts by combined stripping voltammetry

    Energy Technology Data Exchange (ETDEWEB)

    Nedeltcheva, T. [Department of Analytical Chemistry, University of Chemical Technology and Metallurgy, 8 Kl. Ohridsi Blvd., 1756 Sofia (Bulgaria)]. E-mail: nedel@uctm.edu; Atanassova, M. [Department of Analytical Chemistry, University of Chemical Technology and Metallurgy, 8 Kl. Ohridsi Blvd., 1756 Sofia (Bulgaria); Dimitrov, J. [N. Pushkarov Institute of Soil Science and Agroecology, 7 Shosse Bankya St., 1080 Sofia (Bulgaria); Stanislavova, L. [N. Pushkarov Institute of Soil Science and Agroecology, 7 Shosse Bankya St., 1080 Sofia (Bulgaria)

    2005-01-10

    The amount of mobile forms of Zn, Pb, Cd and Cu in extracts obtained by treating soil samples with ammonium nitrate were determined by an appropriate combination of anodic and cathodic stripping voltammetry with hanging mercury drop electrode. Every analysis required three mercury drops: on the first one, zinc was determined; on the second, cadmium and lead; on the third, copper was determined. Zinc, lead and cadmium were determined by conventional differential-pulse anodic stripping voltammetry. For copper determination, adsorptive differential-pulse cathodic stripping voltammetry with amalgamation using chloride ions as a complexing agent was applied. The standard deviation of the results was from 1 to 10% depending on the metal content in the sample. Voltammetric results were in good agreement with the AAS analysis. No microwave digestion of soil extracts was necessary.

  2. Simultaneous determination of textile dyes by Adsorptive Cathodic Stripping Voltammetry - doi: 10.4025/actascitechnol.v35i2.16595

    National Research Council Canada - National Science Library

    Lidia Brizola Santos; Fernando Santos Domingues; Fernando Rosseto; Vitor de Cinque Almeida; Juliana Carla Garcia; Nilson Evelázio de Souza

    2013-01-01

    The Adsorptive Cathodic Stripping Voltammetry (ACSV - differential pulse) proved to be an efficient method in the separation and quantification of two reactive textile dyes, Procion Yellow (PY) and Procion Red (PR...

  3. Determination of Platinum Metals in Carbonaceous Mineral Raw Materials by Stripping Voltammetry

    OpenAIRE

    Kolpakova, Nina Alexandrovna; Oskina, Yuliya Aleksandrovna; Dyachenko, Elena Nikolaevna; Pshenichkin, Anatoliy Yakovlevich

    2015-01-01

    The paper considers the possibility of determining platinum metals in mineral raw materials by stripping voltammetry on a graphite electrode modified by metals. Stripping voltammetry method is characterized by low determination limit, wide intervals of determined content and high sensitivity. As a result of the research the conditions for the determination of gold, platinum and palladium by stripping voltammetry have been selected. The comparison of the results of gold, palladium and platinum...

  4. Arsenic speciation in natural waters by cathodic stripping voltammetry.

    Science.gov (United States)

    Gibbon-Walsh, Kristoff; Salaün, Pascal; van den Berg, Constant M G

    2010-03-03

    Contamination of groundwater with arsenic (As) is a major health risk through contamination of drinking and irrigation water supplies. In geochemically reducing conditions As is mostly present as As(III), its most toxic species. Various methods exist to determine As in water but these are not suitable for monitoring arsenic speciation at its original pH and without preparation. We present a method that uses cathodic stripping voltammetry (CSV) to determine reactive As(III) at a vibrating, gold, microwire electrode. The As(III) is detected after adsorptive deposition of As(OH)(3)(0), followed by a potential scan to measure the reduction current from As(III) to As(0). The method is suitable for waters of pH 7-12, has an analytical range of 1 nM to 100 microM As (0.07-7500 ppb) and a limit of detection of 0.5 nM with a 60 s deposition time. The As speciation protocol involves measuring reactive As(III) by CSV at the original pH and acidification to pH 1 to determine inorganic As(III)+As(V) by anodic stripping voltammetry (ASV) using the same electrode. Total dissolved As is determined by ASV after UV-digestion at pH 1. The method was successfully tested on various raw groundwater samples from boreholes in the UK and West Bengal. Copyright 2010 Elsevier B.V. All rights reserved.

  5. Underpotential deposition and anodic stripping voltammetry at mesoporous microelectrodes.

    Science.gov (United States)

    Sanchez, Pablo Lozano; Elliott, Joanne M

    2005-05-01

    Using the technique of liquid crystal templating a series of high surface area mesoporous platinum microelectrodes was fabricated. The underpotential deposition of metal ions at such electrodes was found to be similar to that at conventional platinum electrodes. The phenomena of underpotential deposition, in combination with the intrinsic properties of mesoporous microelectrodes (i.e. a high surface area and efficient mass transport) was exploited for the purpose of anodic stripping voltammetry. In particular the underpotential deposition of Ag(+), Pb(2+) and Cu(2+) ions was investigated and it was found that mesoporous microelectrodes were able to quantify the concentration of ions in solution down to the ppb range. The overall behaviour of the mesoporous electrodes was found to be superior to that of conventional microelectrodes and the effects of interference by surfactants were minimal.

  6. Determination of Pesticide Ethion by Linear Sweep Stripping Voltammetry

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

    The presence of the pesticide ethion was determined using an electroanalytical method, i. e. , linear sweep stripping voltammetry at a hanging mercury drop electrode in the Britton-Robbinson buffer with pH = 8. 36, based on its reduction peak observed at - 690 mV following its alkaline hydrolysis. The experimental parameters, namely, the preconcentration potential, the preconcentration time, and the scan rate were investigated and -300 mV (vs. Ag/AgCl), 270 s, and 100 mV/s were selected as the optimal values, respectively. The linear relationship between the peak current and the concentration was found to be in the range of 0. 02-0. 16 mg/L, with a detection limit of 0.0087 mg/L. The proposed method was applied to the determination of ethion in spiked vegetable and fruit samples via a preextraction with anhydrous ethanol.

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

    Science.gov (United States)

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

    2015-06-16

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

  8. Square-wave adsorptive cathodic stripping voltammetry of pantoprazole.

    Science.gov (United States)

    Radi, A

    2003-11-24

    Adsorption and reduction of pantoprazole were investigated by cyclic and square-wave voltammetry on a hanging mercury drop electrode in Britton-Robinson buffers at pH 2.0-11.0. The reduction process gave rise to a single peak within the entire pH range. Study of the variation of the reduction signal with solution variables such as pH and concentration of pantoprazole and instrumental variables such as accumulation time and potential, frequency, pulse height and pulse amplitude, has resulted in optimization of the reduction signal for analytical purposes. The voltammetric procedure was applied successfully to give a rapid and precise assay of pantoprazole in a tablet dosage form.

  9. STUDY ON DETERMINATION FOLIC ACID IN FOODSTUFF BY DIFFERENT PULSE STRIPPING VOLTAMMETRY%差示脉冲溶出伏安法测定粮食中叶酸的研究

    Institute of Scientific and Technical Information of China (English)

    张娟; 靳保辉; 刘灵芳; 冶保献

    2001-01-01

    利用差示脉冲溶出伏安技术和叶酸在电极表面的吸附特性,建立了测定痕量叶酸的电化学分析方法.方法具有快速、简便、灵敏度高、干扰少的优点.在不富集的实验条件下,差示峰电流与叶酸浓度在3.39×10-8~3.73×10-7mol/L范围内呈良好线性关系;而在-0.25V电位吸附富集70s条件下,其线性范围为6.78×-10~2.27×10-8mol/L,检测限达1.0×10-11mol/L。将该方法应用于小米和玉米中微量和痕量叶酸的测定,结果满意,回收率在94%~102%之间.%Electrochemical analysis is used to determine trace folic acid by Different Pulse Stripping Voltammetry and to absorb properties of folic acid in electrode face.This method has the characteristics of being fast,used easily,high-sensitivity and little interference.The peak currents have linear relation with folic acid concentration in the range 3.39×10-8~3.73×10-7mol/L without preconcentration,and 6.78×10-10~2.72×10-8mol/L with preconcentration for 70S under-0.25V.The detect limit is 1.0×10-11mol/L.This method has satisfactory result in determining trace folic acid in millet and maize.Its recovery rate is between 94% and 102%.

  10. Manganese Detection with a Metal Catalyst Free Carbon Nanotube Electrode: Anodic versus Cathodic Stripping Voltammetry

    Science.gov (United States)

    Yue, Wei; Bange, Adam; Riehl, Bill L.; Riehl, Bonnie D.; Johnson, Jay M.; Papautsky, Ian; Heineman, William R.

    2013-01-01

    Anodic stripping voltammetry (ASV) and cathodic stripping voltammetry (CSV) were used to determine Mn concentration using metal catalyst free carbon nanotube (MCFCNT) electrodes and square wave stripping voltammetry (SWSV). The MCFCNTs are synthesized using a Carbo Thermal Carbide Conversion method which results in a material that does not contain residual transition metals. Detection limits of 120 nM and 93 nM were achieved for ASV and CSV, respectively, with a deposition time of 60 s. CSV was found to be better than ASV in Mn detection in many aspects, such as limit of detection and sensitivity. The CSV method was used in pond water matrix addition measurements. PMID:24235806

  11. Manganese Detection with a Metal Catalyst Free Carbon Nanotube Electrode: Anodic versus Cathodic Stripping Voltammetry.

    Science.gov (United States)

    Yue, Wei; Bange, Adam; Riehl, Bill L; Riehl, Bonnie D; Johnson, Jay M; Papautsky, Ian; Heineman, William R

    2012-10-01

    Anodic stripping voltammetry (ASV) and cathodic stripping voltammetry (CSV) were used to determine Mn concentration using metal catalyst free carbon nanotube (MCFCNT) electrodes and square wave stripping voltammetry (SWSV). The MCFCNTs are synthesized using a Carbo Thermal Carbide Conversion method which results in a material that does not contain residual transition metals. Detection limits of 120 nM and 93 nM were achieved for ASV and CSV, respectively, with a deposition time of 60 s. CSV was found to be better than ASV in Mn detection in many aspects, such as limit of detection and sensitivity. The CSV method was used in pond water matrix addition measurements.

  12. Differential linear scan voltammetry: analytical performance in comparison with pulsed voltammetry techniques.

    Science.gov (United States)

    Sheth, Disha B; Gratzl, Miklós

    2013-06-01

    We report here on differential linear scan voltammetry, DLSV, that combines the working principles of linear scan voltammetry, LSV, and the numerous existing pulsed voltammetry techniques. DLSV preserves the information from continuous interrogation in voltage and high accuracy that LSV provides about electrochemical processes, and the much better sensitivity of differential pulsed techniques. DLSV also minimizes the background current compared to both LSV and pulsed voltammetry. An early version of DLSV, derivative stationary electrode polarography, DSEP, had been proposed in the 1960s but soon abandoned in favor of the emerging differential pulsed techniques. Relative to DSEP, DLSV takes advantage of the flexibility of discrete smoothing differentiation that was not available to early investigators. Also, DSEP had been explored in pure solutions and with reversible electrochemical reactions. DLSV is tested in this work in more challenging experimental contexts: the measurement of oxygen with a carbon fiber microelectrode in buffer, and with a gold microdisc electrode exposed to a live biological preparation. This work compares the analytical performance of DLSV and square wave voltammetry, the most popular pulsed voltammetry technique.

  13. Determination of Antimony (III) in Real Samples by Anodic Stripping Voltammetry Using a Mercury Film Screen-Printed Electrode

    OpenAIRE

    Olga Domínguez-Renedo; M. Julia Arcos-Martínez; M. Jesús Gómez González

    2009-01-01

    This paper describes a procedure for the determination of antimony (III) by differential pulse anodic stripping voltammetry using a mercury film screen-printed electrode as the working electrode. The procedure has been optimized using experimental design methodology. Under these conditions, in terms of Residual Standard Deviation (RSD), the repeatability (3.81 %) and the reproducibility (5.07 %) of the constructed electrodes were both analyzed. The detection limit for Sb (III) was calculated ...

  14. Pulse Voltammetry in Single Cells Using Platinum Microelectrodes

    Science.gov (United States)

    1991-11-22

    ring electrodes [18) in a solution of 1.OxlO’ M H2PtCl6 and 0.5 M H2SO4 and reducing platinum at 0.0 V vs SSCE for a desired deposition time. Cyclic ...E. and the range for Ed in multiple pulse voltammetry can be chosen from examination of voltammograms obtained by cyclic voltammetry or lin-ir sweep... voltametry [3,13]. As pointed out by Sinru et al. [14) the potential and time of each pulse has a direct effect on the nature of the voltammetry

  15. Topics in Chemical Instrumentation: CII. Automated Anodic Stripping Voltammetry.

    Science.gov (United States)

    Stock, John T.; Ewing, Galen W., Ed.

    1980-01-01

    Presents details of anodic stripping analysis (ASV) in college chemistry laboratory experiments. Provides block diagrams of the analyzer system, circuitry and power supplies of the automated stripping analyzer, and instructions for implementing microcomputer control of the ASV. (CS)

  16. Determination of Lamotrigine in Pharmaceutical Preparations by Adsorptive Stripping Voltammetry Using Screen Printed Electrodes

    Science.gov (United States)

    Domínguez-Renedo, Olga; Calvo, M. Encarnación Burgoa; Arcos-Martínez, M. Julia

    2008-01-01

    This paper describes a procedure that has been optimized for the determination of lamotrigine by Differential Pulse Adsorptive Stripping Voltammetry (DPAdSV) using carbon screen-printed electrodes (CSPE) and mercury coated carbon screen-printed electrodes. Selection of the experimental parameters was made using experimental design methodology. The detection limit found was 5.0 × 10-6 M and 2.0 × 10-6 M for the non modified and Hg modified CSPE, respectively. In terms of reproducibility, the precision of the above mentioned methods was calculated in %RSD values at 9.83% for CSPE and 2.73% for Hg-CSPE. The Hg-coated CSPEs developed in this work were successfully applied in the determination of lamotrigine in pharmaceutical preparations. PMID:27879931

  17. Determination of Lamotrigine in Pharmaceutical Preparations by Adsorptive Stripping Voltammetry Using Screen Printed Electrodes

    Directory of Open Access Journals (Sweden)

    M. Julia Arcos-Martínez

    2008-07-01

    Full Text Available This paper describes a procedure that has been optimized for the determination of lamotrigine by Differential Pulse Adsorptive Stripping Voltammetry (DPAdSV using carbon screen-printed electrodes (CSPE and mercury coated carbon screen-printed electrodes. Selection of the experimental parameters was made using experimental design methodology. The detection limit found was 5.0 x 10-6 M and 2.0 x 10-6 M for the non modified and Hg modified CSPE, respectively. In terms of reproducibility, the precision of the above mentioned methods was calculated in %RSD values at 9.83% for CSPE and 2.73% for Hg-CSPE. The Hg-coated CSPEs developed in this work were successfully applied in the determination of lamotrigine in pharmaceutical preparations.

  18. Iron organic speciation determination in rainwater using cathodic stripping voltammetry.

    Science.gov (United States)

    Cheize, Marie; Sarthou, Géraldine; Croot, Peter L; Bucciarelli, Eva; Baudoux, Anne-Claire; Baker, Alex R

    2012-07-29

    A sensitive method using Competitive Ligand Exchange-Adsorptive Cathodic Stripping Voltammetry (CLE-ACSV) has been developed to determine for the first time iron (Fe) organic speciation in rainwater over the typical natural range of pH. We have adapted techniques previously developed in other natural waters to rainwater samples, using the competing ligand 1-nitroso-2-naphthol (NN). The blank was equal to 0.17±0.05 nM (n=14) and the detection limit (DL) for labile Fe was 0.15 nM which is 10-70 times lower than that of previously published methods. The conditional stability constant for NN under rainwater conditions was calibrated over the pH range 5.52-6.20 through competition with ethylenediaminetetraacetic acid (EDTA). The calculated value of the logarithm of β'(Fe(3+)(NN)(3)) increased linearly with increasing pH according to log β'(Fe(3+)(NN)(3)) (salinity=2.9, T=20 °C). The validation of the method was carried out using desferrioxamine mesylate B (DFOB) as a natural model ligand for Fe. Adequate detection windows were defined to detect this class of ligands in rainwater with 40 μM of NN from pH 5.52 to 6.20. The concentration of Fe-complexing natural ligands was determined for the first time in three unfiltered and one filtered rainwater samples. Organic Fe-complexing ligand concentrations varied from 104.2±4.1 nM equivalent of Fe(III) to 336.2±19.0 nM equivalent of Fe(III) and the logarithm of the conditional stability constants, with respect to Fe(3+), varied from 21.1±0.2 to 22.8±0.3. This method will provide important data for improving our understanding of the role of wet deposition in the biogeochemical cycling of iron. Copyright © 2012 Elsevier B.V. All rights reserved.

  19. Direct determination of molybdenum in seawater by adsorption cathodic stripping square-wave voltammetry.

    Science.gov (United States)

    Sun, Y C; Mierzwa, J; Lan, C R

    2000-06-30

    A reliable and very sensitive procedure for the determination of trace levels of molybdenum in seawater is proposed. The complex of molybdenum with 8-hydroxyquinoline (Oxine) is analyzed by cathodic stripping square-wave voltammetry based on the adsorption collection onto a hanging mercury drop electrode (HMDE). This procedure of molybdenum determination was found to be more favorable than differential pulse cathodic stripping voltammetry because of inherently faster scan rate and much better linearity obtained through the one-peak (instead of one-of-two peaks) calibration. The variation of polarographic peak and peak current with a pH, adsorption time, adsorption potential, and some instrumental parameters such as scan rate and pulse height were optimized. The alteration of polarographic wave and its likely mechanism are also discussed. The relationship between peak current and molybdenum concentration is linear up to 150 mug l(-1). Under the optimal analytical conditions, the determination limit of 0.5 mug l(-1) Mo was reached after 60 s of the stirred collection. The estimated detection limit is better than 0.1 mug l(-1) of Mo. The applicability of this method to analysis of seawater was assessed by the determination of molybdenum in two certified reference seawater samples (CASS-2 and NASS-2) and the comparison of the analytical results for real seawater samples (study on a vertical distribution of Mo in the seawater column) with the results obtained by Zeeman-corrected electrothermal atomization atomic absorption spectrometry (Zeeman ETAAS). A good agreement between two used methods of molybdenum determination was obtained.

  20. Square-Wave Voltammetry of Cathodic Stripping Reactions. Diagnostic Criteria, Redox Kinetic Measurements, and Analytical Applications

    OpenAIRE

    Gulaboski, Rubin; Mirceski, Valentin; Komorsky-Lovrić, Šebojka; Lovrić, Milivoj

    2004-01-01

    A comparative study of different types of cathodic stripping reactions under conditions of square-wave voltammetry is presented. Cathodic stripping processes involving reactions of second order as well as reactions coupled by adsorption of the reacting ligand are analyzed The inherent parameters, controlling the overall voltammetric behavior of each cathodic stripping electrode reaction are derived. The criteria for qualitative distinguishing of each mechanism are established as w...

  1. Sono-cathodic stripping voltammetry of manganese at a polished boron-doped diamond electrode: application to the determination of manganese in instant tea.

    Science.gov (United States)

    Saterlay, A J; Foord, J S; Compton, R G

    1999-12-01

    Ultrasonically assisted cathodic stripping voltammetry at a boron-doped diamond electrode was developed for the detection of manganese. Differential-pulse voltammetry was used to give the analytical signal from a cathodic strip of electrodeposited MnO2; linearity was observed from 10(-11) M to at least 3 x 10(-7) M, with 10(-11) M being the detection limit for a 2 min deposition. The procedure involves both ultrasonic-anodic deposition of MnO2 and ultrasonic-cathodic stripping. This novel analytical tool is robust, reproducible, mercury free, oxygen insensitive and highly specific towards manganese. The differential-pulse sono-cathodic stripping voltammetric technique was used to determine successfully the manganese content of two instant tea samples, giving excellent agreement with independent AAS analyses.

  2. International comparison of Cd content in a quality control material of Navajuelas (Tagelus dombeii) determined by anodic stripping voltammetry, atomic absorption spectrometry and neutron activation analysis

    Energy Technology Data Exchange (ETDEWEB)

    Queirolo, F. (Universidad Catolica del Norte, Antofagasta (Chile). Dept. of Chemistry Forschungszentrum Juelich GmbH (Germany, F.R.). Inst. fuer Angewandte Physikalische Chemie Universidad de Extremadura, Badajoz (Spain). Dept. of Analytical Chemistry and Electrochemistry); Ostapczuk, P. (Forschungszentrum Juelich GmbH (Germany, F.R.). Inst. fuer Angewandte Physikalische Chemie); Valenta, P.; Stegen, S. (Forschungszentrum Juelich GmbH (Germany, F.R.). Inst. fuer Angewandte Physikalische Chemie Universidad de Extremadura, Badajoz (Spain). Dept. of Analytical Chemistry and Electrochemistry); Marin, C.; Vinagre, F.; Sanchez, A. (Universidad de Extremadura, Badajoz (Spain). Dept. of Analytical Chemistry and Electrochemistry)

    1991-05-01

    The determination of Cd was performed by neutron activation analysis (NAA), atomic absorption spectrometry (AAS) with flame or in the electrothermal mode and anodic stripping voltammetry in the differential pulse mode (DPASV) and the square wave mode (SWASV). (orig./EF).

  3. Quantification of the Vasoactive Agent Buflomedil HCl in Pharmaceutical Formulation and Human Serum by Stripping Voltammetry and Liquid Chromatography.

    Science.gov (United States)

    El-Desoky, Hanaa S; Ghoneim, Mohamed M; Abdel-Galeil, Mohamed M

    2010-06-01

    Buflomedil HCl, was reduced at the mercury electrode in buffered solutions of various pH values (2-11) via a single 2-electron irreversible step corresponding to reduction of its C=O double bond. Buflomedil HCl has interfacial adsorptive behavior onto the mercury electrode surface and a monolayer surface coverage of 2.37 × 10-10 mol cm-2 was estimated. Each adsorbed buflomedil HCl molecule was found to occupy an area of 0.69 nm2 onto the HMDE surface. Differential-pulse (DP), liner-sweep (LS) and square-wave (SW) adsorptive cathodic stripping voltammetry (AdCSV) methods were described for its determination in the bulk form. The sensitivity of the described electro-analytical methods increases in the direction: DP-AdCSV voltammetry method is much more sensitive than the described chromatographic one. However the described chromatographic method is substantially simpler, faster and more sensitive than the previously reported HPLC methods.

  4. Lead-Testing Service to Elementary and Secondary Schools Using Anodic Stripping Voltammetry

    Science.gov (United States)

    Goebel, Amanda; Vos, Tracy; Louwagie, Anne; Lundbohm, Laura; Brown, Jay H.

    2004-01-01

    The undergraduate chemistry club of the Southwest Minnesota State University offers assistance in lead-testing through the anodic stripping voltammetry (ASV) technique to elementary and secondary schools. Emphasis is given to this community service activity, which has increased club membership, and promoted discussion of water quality problems in…

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

    Science.gov (United States)

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

    2005-01-01

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

  6. Adsorptive stripping voltammetry of trimethoprim: mechanistic studies and application to the fast determination in pharmaceutical suspensions.

    Science.gov (United States)

    Carapuça, Helena M; Cabral, David J; Rocha, Luciana S

    2005-06-15

    The adsorptive stripping voltammetric behaviour of trimethoprim (TMP) was studied at pH 3.8 and 7.0 by linear-sweep (LS) and cyclic voltammetry at the hanging mercury drop electrode. The charges and surface concentrations of the protonated TMP species were determined at both pH values. Taking advantage of the adsorption features of TMP fast voltammetric techniques (LS and square-wave (SW) voltammetry) were applied to the determination of TMP at the 10(-7)mol dm(-3) concentration level (pH 3.8). For these concentrations the relative standard deviations were cathodic stripping voltammetry originated a very fast and sensitive method for the direct analysis of TMP in pharmaceutical suspensions without any matrix effects or interference from sulfamethoxazole. No sample pre-treatments or solvent extraction procedures were needed. The quantitative results were in agreement with the data supplied by the manufacturer.

  7. General theory of cathodic and anodic stripping voltammetry at solid electrodes: mathematical modeling and numerical simulations.

    Science.gov (United States)

    Ward Jones, Sarah E; Chevallier, François G; Paddon, Christopher A; Compton, Richard G

    2007-06-01

    Theory is presented to describe the voltammetric signals associated with the stripping phase of stripping voltammetry at solid electrodes. Three mathematical models are considered, and the importance of the hemispherical diffusion associated with electrochemical dissolution of particles in the micrometer range is investigated. Model A considers a "monolayer" system where the coverage at a specific point cannot exceed a maximum value. Model B considers a thin layer of metal or metal oxide, but in contrast to model A, the maximum surface coverage is not restricted. Model C represents the stripping of a "thick layer" where the deposition is also unrestricted.

  8. Application of different methodologies in the preparation of organic matrices for determination of trace elements by differential pulse anodic stripping voltammetry; Aplicacao de diferentes metodologias na preparacao de matrizes organicas para a determinacao voltametrica de elementos traco

    Energy Technology Data Exchange (ETDEWEB)

    Sisti, Cristina

    2001-07-01

    The determination of trace elements in food samples is of great importance for the human health, considering the factors of essentiality and toxicity. On the other hand, the chemical analysis is largely affected for the steps of sample preparation; laboratory contamination of the sample and the reagents or still volatilization and losses of the elements. If these parameters are not controlled the achieved precision and accuracy could be low. In this work, the content of zinc, cadmium, lead and copper was determined in adults diet samples collected by duplicate portion technique and bovine liver, applying the differential pulse anodic stripping voltametry - (DP-ASV) technique. In the digestion of the matrices in acid medium, conventional methodologies were used, conductive heating in open recipients and equipment with microwaves source in open and closed vessels. The best procedure was the sample digestion by microwaves, in closed vessels and the other treatments made in controlled atmosphere with hood laminar-airflow class 100. The established methodology was validated with the use of a certified sample as reference (NIST - bovine liver 1577b). (author)

  9. Determination of the leaching of polymeric ion-selective membrane components by stripping voltammetry.

    Science.gov (United States)

    Paczosa-Bator, Beata; Piech, Robert; Lewenstam, Andrzej

    2010-05-15

    This paper focuses on the quantitative determination of the loss of the components from plastic membranes of ion-selective electrodes (ISEs) during contact with aqueous bathing solutions. The leaching processes, which affect the ISE responses, are rarely characterized by independent methods. For this purpose, differential pulse cathodic stripping voltammetry (DP CSV) is used. This method, owing to its high sensitivity, acceptable recovery and accuracy, is a good tool to characterize the kinetics of leakage of the lipophilic salts. Sodium tetraphenylborate (NaTPB) leakage from the PVC-based sodium-selective membrane containing two different plasticizers, o-nitrophenyl octyl ether (o-NPOE) or di(2-ethylhexyl) sebacate (DOS) is presented. Correlation between the rate of leaching of the lipophilic salt and dielectric constants of the plasticizers is observed. The data obtained by DP CSV correlate well with potentiometric and electrochemical impedance responses. The observed outflow of TPB(-) is associated with decreasing potentiometric sensitivity to sodium and increasing bulk membrane resistance.

  10. Simultaneous determination of ultra trace amounts of lead and cadmium in food samples by adsorptive stripping voltammetry.

    Science.gov (United States)

    Abbasi, Shahryar; Khodarahmiyan, Kobra; Abbasi, Freshteh

    2011-09-01

    A selective and sensitive method for simultaneous determination of lead and cadmium by adsorptive differential pulse cathodic stripping voltammetry is presented. The method is based on adsorptive accumulation of the complexes of Pb (II) and Cd (II) ions with 2-mercaptobenzothiazole onto hanging mercury drop electrode (HMDE), followed by the reduction of the adsorbed species by differential pulse cathodic stripping voltammetry. Optimal conditions were obtained at pH 8.0, 2-mercaptobenzothiazole concentration of 1.0×10(-4)M, the accumulation potential of -0.4V (vs. Ag/AgCl), the accumulation time of 160s, and the scan rate of 100mV/s. Under optimised conditions, linear calibration curves were established for the concentration of Pb (II) and Cd (II) in the range of 0.5-70 and 0.2-30ng/ml, respectively, with detection limit of 0.017ng/ml for Pb (II) and 0.01ng/ml for Cd (II). The procedure was successfully applied to the simultaneous determination of both ions in food samples (rice, soya and sugar). Published by Elsevier Ltd.

  11. Use of a modified, high-sensitivity, anodic stripping voltammetry method for determination of zinc speciation in the North Atlantic Ocean

    Energy Technology Data Exchange (ETDEWEB)

    Jakuba, Rachel Wisniewski [Massachusetts Institute of Technology, Woods Hole Oceanographic Institution Joint Program in Chemical Oceanography, 266 Woods Hole Road, Woods Hole, MA 02543 (United States)], E-mail: jakuba.rachel@epa.gov; Moffett, James W. [Department of Marine Chemistry and Geochemistry, Woods Hole Oceanographic Institution, 266 Woods Hole Road, Woods Hole, MA 02543 (United States)], E-mail: jmoffett@usc.edu; Saito, Mak A. [Department of Marine Chemistry and Geochemistry, Woods Hole Oceanographic Institution, 266 Woods Hole Road, Woods Hole, MA 02543 (United States)

    2008-05-05

    Zinc speciation is considered to be an important determinant of the biological availability of zinc. Yet in oceanic surface waters, characterization of zinc speciation is difficult due to the low concentrations of this essential micronutrient. In this study, an anodic stripping voltammetry method previously developed for the total determination of cadmium and lead was successfully adapted to the measurement of zinc speciation. The method differs from previous zinc speciation anodic stripping voltammetry methods in that a fresh mercury film is plated with each sample aliquot. The fresh film anodic stripping voltammetry method was compared to competitive ligand exchange cathodic stripping voltammetry in a profile from the North Atlantic Ocean. Results using the fresh film anodic stripping voltammetry method were similar to those determined using the cathodic stripping voltammetry method, though ligand concentrations determined by fresh film anodic stripping voltammetry were generally slightly higher than those determined by cathodic stripping voltammetry. There did not seem to be a systematic difference between methods for the estimates of conditional stability constants. The ligand concentration in the North Atlantic profile ranged from 0.9 to 1.5 nmol L{sup -1} as determined by fresh film anodic stripping voltammetry and 0.6 to 1.3 nmol L{sup -1} as determined by cathodic stripping voltammetry. The conditional stability constants determined by fresh film anodic stripping voltammetry were 10{sup 9.8}-10{sup 10.5} and by cathodic stripping voltammetry were 10{sup 9.8}-10{sup 11.3}.

  12. Use of a modified, high-sensitivity, anodic stripping voltammetry method for determination of zinc speciation in the North Atlantic Ocean.

    Science.gov (United States)

    Jakuba, Rachel Wisniewski; Moffett, James W; Saito, Mak A

    2008-05-05

    Zinc speciation is considered to be an important determinant of the biological availability of zinc. Yet in oceanic surface waters, characterization of zinc speciation is difficult due to the low concentrations of this essential micronutrient. In this study, an anodic stripping voltammetry method previously developed for the total determination of cadmium and lead was successfully adapted to the measurement of zinc speciation. The method differs from previous zinc speciation anodic stripping voltammetry methods in that a fresh mercury film is plated with each sample aliquot. The fresh film anodic stripping voltammetry method was compared to competitive ligand exchange cathodic stripping voltammetry in a profile from the North Atlantic Ocean. Results using the fresh film anodic stripping voltammetry method were similar to those determined using the cathodic stripping voltammetry method, though ligand concentrations determined by fresh film anodic stripping voltammetry were generally slightly higher than those determined by cathodic stripping voltammetry. There did not seem to be a systematic difference between methods for the estimates of conditional stability constants. The ligand concentration in the North Atlantic profile ranged from 0.9 to 1.5 nmol L(-1) as determined by fresh film anodic stripping voltammetry and 0.6 to 1.3 nmol L(-1) as determined by cathodic stripping voltammetry. The conditional stability constants determined by fresh film anodic stripping voltammetry were 10(9.8)-10(10.5) and by cathodic stripping voltammetry were 10(9.8)-10(11.3).

  13. Detection of heavy metals in biological samples through anodic stripping voltammetry

    OpenAIRE

    Buzea, Vlad; Florescu, Monica; Badea, Mihaela

    2012-01-01

    The toxicological aspects due to the presence of heavy metals in biological samples impose to have accurate and rapid methods for their detection. This paper is aimed to review approaches to anodic stripping voltammetry (ASV) determination of several heavy metals (lead, cadmium, copper, mercury, zinc) in biological matrices (blood, urine, saliva, tissue sample). Analytical performances (LOD, data linearity range, sensitivity) of the reviewed methods were presented for several electrochemical ...

  14. Cathodic stripping voltammetry of trace Mn(II) at carbon film electrodes

    OpenAIRE

    Filipe, Olga M. S.; Brett,Christopher M.A.

    2003-01-01

    A sensitive voltammetric method is presented for the determination of tract levels of Mn (II) using carbon film electrodes fabricated from carbon resistors of 2 [Omega]. Determination of manganese was made by square wave cathodic stripping voltammetry (CSV), with deposition of manganese as manganese dioxide. Chronoamperometric experiments were made to study MnO2 nucleation and growth. As a result, it was found to be necessary to perform electrode conditioning at a more positive potential to i...

  15. Cathodic stripping voltammetry of cysteine using silver and copper solid amalgam electrodes.

    Science.gov (United States)

    Yosypchuk, B; Novotný, L

    2002-04-01

    Silver and copper solid amalgam electrodes (modified with mercury meniscus and based on amalgamation of fine metallic powder) have been successfully tested for cathodic stripping voltammetry of cysteine. In the case of the silver solid amalgam electrode AgSAE the relative standard deviation (RSD) and the detection limit (3 SD) reached +/-2.3% and 3x10(-9) mol l(-1) cysteine, respectively.

  16. Graphene electroanalysis: inhibitory effects in the stripping voltammetry of cadmium with surfactant free graphene.

    Science.gov (United States)

    Brownson, Dale A C; Lacombe, Alexandre C; Kampouris, Dimitrios K; Banks, Craig E

    2012-01-21

    We explore the use of surfactant free graphene towards the electroanalytical sensing of cadmium(II) ions via anodic stripping voltammetry. In line with literature methodologies, we modify an electrode substrate which exhibits relatively fast electron transfer with commercially available graphene which is free from surfactants. Surprisingly, we find that graphene reduces the analytical performance and hence inhibits the electrochemical detection of cadmium(II) ions, with calibration plots in model aqueous solutions revealing no advantages of employing graphene in this analytical context.

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

    Science.gov (United States)

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

    2016-01-15

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

  18. Accurate analytical expressions for stripping voltammetry in the Henry adsorption limit.

    Science.gov (United States)

    Calvente, Juan José; Andreu, Rafael

    2011-08-15

    A strategy is developed to derive accurate analytical expressions for low-coverage cathodic stripping voltammetry. The procedure relies on the observation that diffusion affects the location of simulated voltammetric waves but not their shape, provided that physisorption of the analyte is negligible. As a proof of the generality of the proposed approach and having in mind the stripping of thiols, analytical solutions are derived for the cathodic stripping of monomers, dimers, and a mixture of monomers and dimers, whose reliability is proved by their comparison with numerically simulated voltammograms. Application to the deposition and reductive desorption of mercaptoacetic acid at a mercury electrode demonstrates that these approximate solutions can be used to get insights into the interfacial organization of incipient films. For this particular system, a transition from monomeric to dimeric behavior is identified upon increasing the thiol surface concentration. Further generalization of the proposed methodology is achieved by deriving an approximate analytical solution for thin-layer anodic stripping voltammetry, which is satisfactorily compared to the existing summation series solution.

  19. Electrochemical behavior of folic acid at calixarene based chemically modified electrodes and its determination by adsorptive stripping voltammetry

    Energy Technology Data Exchange (ETDEWEB)

    Vaze, Vishwanath D. [Department of Chemistry, University of Mumbai, Vidyanagari, Santacruz (East), Mumbai 400098 (India); Srivastava, Ashwini K. [Department of Chemistry, University of Mumbai, Vidyanagari, Santacruz (East), Mumbai 400098 (India)], E-mail: aksrivastava@chem.mu.ac.in

    2007-12-31

    Voltammetric behavior of folic acid at plain carbon paste electrode and electrode modified with calixarenes has been studied. Two peaks for irreversible oxidation were observed. Out of the three calixarenes chosen for modification of the electrodes, p-tert-butyl-calix[6]arene modified electrode (CME-6) was found to have better sensitivity for folic acid. Chronocoulometric and differential pulse voltammetric studies reveal that folic acid can assemble at CME-6 to form a monolayer whose electron transfer rate is 0.00273 s{sup -1} with 2-electron/2-proton transfer for the peak at +0.71 V against SCE. An adsorption equilibrium constant of 5 x 10{sup 3} l/mol for maximum surface coverage of 2.89 x 10{sup -10} mol/cm{sup 2} was obtained. The current is found to be rectilinear with concentration by differential pulse voltammetry. However, linearity in the lower range of concentration 8.79 x 10{sup -12} M to 1.93 x 10{sup -9} M with correlation coefficient of 0.9920 was achieved by adsorptive stripping voltammetry. The limit of detection obtained was found to be 1.24 x 10{sup -12} M. This method was used for the determination of folic acid in a variety of samples, viz. serum, asparagus, spinach, oranges and multivitamin preparations.

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

    Science.gov (United States)

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

    2014-12-16

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

  1. Determination of Antimony (III) in Real Samples by Anodic Stripping Voltammetry Using a Mercury Film Screen-Printed Electrode.

    Science.gov (United States)

    Domínguez-Renedo, Olga; Gómez González, M Jesús; Arcos-Martínez, M Julia

    2009-01-01

    This paper describes a procedure for the determination of antimony (III) by differential pulse anodic stripping voltammetry using a mercury film screen-printed electrode as the working electrode. The procedure has been optimized using experimental design methodology. Under these conditions, in terms of Residual Standard Deviation (RSD), the repeatability (3.81 %) and the reproducibility (5.07 %) of the constructed electrodes were both analyzed. The detection limit for Sb (III) was calculated at a value of 1.27×10(-8) M. The linear range obtained was between 0.99 × 10(-8) - 8.26 × 10(-8) M. An analysis of possible effects due to the presence of foreign ions in the solution was performed and the procedure was successfully applied to the determination of antimony levels in pharmaceutical preparations and sea water samples.

  2. Detection of iron(III)-binding ligands originating from marine phytoplankton using cathodic stripping voltammetry.

    Science.gov (United States)

    Hasegawa, Hiroshi; Maki, Teruya; Asano, Kohnosuke; Ueda, Kentaro; Ueda, Kazumasa

    2004-01-01

    The sample preparation and analytical methodology are described for detecting biologically produced iron(III)-binding ligands in laboratory cultures of coastal marine phytoplankton. The iron(III)-binding ligands from the culture media were purified by passage through a column packing with a hydrophobic absorbent. The concentrations and stability constants of the ligands were determined by adsorptive cathodic stripping voltammetry with competitive ligand equilibration. The analytical results of the cultivated cultures suggest that eukaryotic phytoplankton would produce iron(III)-binding ligands in analogy with other microorganisms.

  3. Anodic stripping voltammetry of nickel ions and nickel hydroxide nanoparticles at boron-doped diamond electrodes

    Science.gov (United States)

    Musyarofah, N. R. R.; Gunlazuardi, J.; Einaga, Y.; Ivandini, T. A.

    2017-04-01

    Anodic stripping voltammetry (ASV) of nickel ions in phosphate buffer solution (PBS) have been investigated at boron-doped diamond (BDD) electrodes. The deposition potential at 0.1 V (vs. Ag/AgCl) for 300 s in 0.1 M PBS pH 3 was found as the optimum condition. The condition was applied for the determination of nickel contained in nickel hydroxide nanoparticles. A linear calibration curve can be achieved of Ni(OH)2-NPs in the concentration range of x to x mM with an estimated limit of detection (LOD) of 5.73 × 10-6 mol/L.

  4. Selective method for the determination of gold by anodic stripping voltammetry.

    Science.gov (United States)

    Korolczuk, M

    1996-12-01

    A highly selective method for the deter- mination of gold by anodic stripping voltammetry is described. For preconcentration a glassy carbon electrode, activated by deposition of small amounts of gold before the measurement, is proposed. The Au(3+) reduction process at such an electrode is effective starting with the potential +0.4 V vs. Ag/AgCl electrode. A linear dependence of the current of the gold stripping peak on the gold concentration was obtained in the range from 5x10(-8) to 1x10(-6) mol/l. The relative standard deviation for 2x10(-7) mol/l HAuCl(4) was 4.2% (n=5). The detection limit was 4x10(-9) mol/l. The accuracy of the method was verified by the determination of gold in reference materials.

  5. The versatility of salicylaldehyde thiosemicarbazone in the determination of copper in blood using adsorptive stripping voltammetry.

    Science.gov (United States)

    Mahajan, Rakesh Kumar; Walia, T P S; Sumanjit; Lobana, T S

    2005-10-15

    The adsorptive cathodic stripping voltammetry technique (AdCSV) is used to determine copper(II) using salicylaldehyde thiosemicarbazone (N, S- donor) as a complexing agent on hanging mercury drop electrode at pH 9.3. Variable factors affecting the response, i.e. the concentration of ligand, pH, adsorption potential and adsorption time are assessed and optimized. The adsorbed complex of copper(II) and salicylaldehyde thiosemicarbazone gives a well defined cathodic stripping peak current at -0.35 V, which has been used for the determination of copper in the concentration range of 7.85 x 10(-9) to 8.00 x 10(-6)M with accumulation time of 360 s at -0.1 V versus Ag/AgCl. This technique has been applied for the determination of copper in various digested samples of whole blood at trace levels.

  6. Detection of aniline at boron-doped diamond electrodes with cathodic stripping voltammetry.

    Science.gov (United States)

    Spătaru, Tanţa; Spătaru, Nicolae; Fujishima, Akira

    2007-09-15

    Boron-doped diamond (BDD) electrodes were used to investigate the possibility of detecting aniline by linear-sweep cathodic stripping voltammetry. It was found that the dimeric species (p-aminodiphenylamine and benzidine) formed by anodic oxidation of aniline during the accumulation period are involved in electrochemically reversible redox processes and, in acidic media, the shape of the stripping voltammetric response is suitable for aniline detection in the micromolar concentration range. The low background current of conductive diamond is an advantage compared to other electrode materials and allows a detection limit of 1muM. Weak adsorption properties and the extreme electrochemical stability are additional advantages of BDD and it was found that, even after long-time measurements, the electrode surface can regain its initial activity by an anodic polarization in the potential region of water decomposition.

  7. Catalytic Adsorptive Stripping Voltammetry at a Carbon Paste Electrode for the Determination of Amiodarone

    Institute of Scientific and Technical Information of China (English)

    LIU Ning; GAO Wei; SONG Jun-Feng

    2006-01-01

    Voltammetry using solid electrodes usually suffers from the contamination due to the deposition of the redox products of analytes on the electrode surface. The contamination has resulted in poor reproducibility and overelaborate operation procedures. The use of the chemical catalysis of oxidant on the reduction product of analyte not only can eliminate the contamination of analyte to solid electrodes but also can improve the faradaic response of analyte. This work introduced both the catalysis of oxidant K2S2O8 and the enhancement of surfactant Triton X-100 on the faraday response of amiodarone into an adsorptive stripping voltammetry at a carbon paste electrode for the determination of amiodarone. The method exhibits high sensitivity, good reproducibility and simple operation procedure. In 0.2 mol·L-1 HOAc-NaOAc buffer (pH=5.3) containing 2.2 × 10-2 mol·L-1 K2S2O8 and 0.002% Triton X-100, the 2.5th-order derivative stripping peak current of the catalytic wave at 0.3 V (vs. Ag/AgCl) is rectilinear to amiodarone concentration in the range of 2.0× 10-10-2.3× 10-8 mol·L-1 with a detection limit of 1.5× l0-10 mol·L-1 after accumulation at 0 V for 30 s.

  8. Determination of trace amounts of thallium by adsorptive cathodic stripping voltammetry with xylenol orange.

    Science.gov (United States)

    Shams, Esmaeil; Yekehtaz, Mehdi

    2002-09-01

    Trace amounts of thallium(I) can be determined using adsorptive cathodic stripping voltammetry in the presence of Xylenol Orange (XO). The reduction current of the thallium(I)-XO complex ion was measured by square-wave cathodic stripping voltammetry. The peak potential was at -0.44 V vs. Ag/AgCl. The effect of various parameters (pH, ligand concentration, accumulation potential and collection time) on the response are discussed. The response was linearly related to the thallium concentration in the range 0.5-110 ng ml(-1) and 110-2000 ng ml(-1). The limit of detection was 0.2 ng ml(-1). The relative standard deviation for the determination of 80 ng ml(-1) thallium was 2.8%. Many common anions and cations did not interfere with the determination of thallium. The interference of lead was reduced by the addition of 0.003 M sodium carbonate. The voltammetric procedure was then successfully applied to the determination of thallium in various complex samples.

  9. Electrochemical characterisation and anodic stripping voltammetry at mesoporous platinum rotating disc electrodes.

    Science.gov (United States)

    Lozano-Sanchez, Pablo; Elliott, Joanne M

    2008-02-01

    Using the technique of liquid crystal templating a rotating disc electrode (RDE) was modified with a high surface area mesoporous platinum film. The surface area of the electrode was characterised by acid voltammetry, and found to be very high (ca. 86 cm(2)). Acid characterisation of the electrode produced distorted voltammograms was interpreted as being due to the extremely large surface area which produced a combination of effects such as localised pH change within the pore environment and also ohmic drop effects. Acid voltammetry in the presence of two different types of surfactant, namely Tween 20 and Triton X-100, suggested antifouling properties associated with the mesoporous deposit. Further analysis of the modified electrode using a redox couple in solution showed typical RDE behaviour although extra capacitive currents were observed due to the large surface area of the electrode. The phenomenon of underpotential deposition was exploited for the purpose of anodic stripping voltammetry and results were compared with data collected for microelectrodes. Underpotential deposition of metal ions at the mesoporous RDE was found to be similar to that at conventional platinum electrodes and mesoporous microelectrodes although the rate of surface coverage was found to be slower at a mesoporous RDE. It was found that a mesoporous RDE forms a suitable system for quantification of silver ions in solution.

  10. The influence of the capping agent on the oxidation of silver nanoparticles: nano-impacts versus stripping voltammetry.

    Science.gov (United States)

    Toh, Her Shuang; Jurkschat, Kerstin; Compton, Richard G

    2015-02-09

    The influence of capping agents on the oxidation of silver nanoparticles was studied by using the electrochemical techniques of anodic stripping voltammetry and anodic particle coulometry ("nano-impacts"). Five spherical silver nanoparticles each with a different capping agent (branched polyethylenimine (BPEI), citrate, lipoic acid, polyethylene glycol (PEG) and polyvinylpyrrolidone (PVP)) were used to perform comparative experiments. In all cases, regardless of the capping agent, complete oxidation of the single nanoparticles was seen in anodic particle coulometry. The successful quantitative detection of the silver nanoparticle size displays the potential application of anodic particle coulometry for nanoparticle characterisation. In contrast, for anodic stripping voltammetry using nanoparticles drop casting, it was observed that the capping agent has a very significant effect on the extent of silver oxidation. All five samples gave a low oxidative charge corresponding to partial oxidation. It is concluded that the use of anodic stripping voltammetry to quantify nanoparticles is unreliable, and this is attributed to nanoparticle aggregation.

  11. Anodic stripping voltammetry of gold nanoparticles at boron-doped diamond electrodes and its application in immunochromatographic strip tests.

    Science.gov (United States)

    Ivandini, Tribidasari A; Wicaksono, Wiyogo P; Saepudin, Endang; Rismetov, Bakhadir; Einaga, Yasuaki

    2015-03-01

    Anodic stripping voltammetry (ASV) of colloidal gold-nanoparticles (AuNPs) was investigated at boron-doped diamond (BDD) electrodes in 50 mM HClO4. A deposition time of 300 s at-0.2 V (vs. Ag/AgCl) was fixed as the condition for the ASV. The voltammograms showed oxidation peaks that could be attributed to the oxidation of gold. These oxidation peaks were then investigated for potential application in immunochromatographic strip tests for the selective and quantitative detection of melamine, in which AuNPs were used as the label for the antibody of melamine. Linear regression of the oxidation peak currents appeared in the concentration range from 0.05-0.6 μg/mL melamine standard, with an estimated LOD of 0.069 μg/mL and an average relative standard deviation of 8.0%. This indicated that the method could be considered as an alternative method for selective and quantitative immunochromatographic applications. The validity was examined by the measurements of melamine injected into milk samples, which showed good recovery percentages during the measurements.

  12. Determination of Lead in Vegetables by Differential Pulse Stripping Voltammetry on Nafion Modified Mercury Film Electrode%Nafion修饰汞膜电极微分脉冲阳极溶出伏安法测定蔬菜中的铅

    Institute of Scientific and Technical Information of China (English)

    王志登; 孙汝东

    2013-01-01

    采用Nafion修饰汞膜电极微分脉冲阳极溶出伏安法测定蔬菜中的铅,选择0.1 mol/L NH4NO3作为支持电解质,富集时间420 s,搅拌速度300 r/min,Nafion修饰体积10 μL,考察了共存离子的干扰.方法在0.01 μg/L~ 14.0 μg/L范围内线性良好,检出限为0.2 μg/L,铅酸电池厂附近蔬菜样品的测定结果与石墨炉原子吸收光谱法相吻合,加标回收率为89.5%~106%.%A new method based on Nafion modified mercury film electrode has been established for detection of Pb2 + in vegetables from the vicinity of lead-acid battery factory by differential pulse stripping voltammetry. The parameters of this method is 0. 1 mol/L NH4NO3 as supporting electrolyte, accumulation time of 420 s, stirring rate of 300 r/min, the Nafion modified volume of 10μL and interfering ions were investigated. It showed good linear relationship between peak current and Pb2+ in the range of 0.01μg/L to 14.0μg/L. The detection limit was 0.2 μg/L. The vegetable sample measurement results using this method have good consistency with GFAAS, and the spiked recoveries ranged from 89.5% to 106%.

  13. Determination of water in room temperature ionic liquids by cathodic stripping voltammetry at a gold electrode.

    Science.gov (United States)

    Zhao, Chuan; Bond, Alan M; Lu, Xunyu

    2012-03-20

    An electrochemical method based on cathodic stripping voltammetry at a gold electrode has been developed for the determination of water in ionic liquids. The technique has been applied to two aprotic ionic liquids, (1-butyl-3-ethylimidazolium tetrafluoroborate and 1-butyl-3-methylimidazolium hexafluorophosphate), and two protic ionic liquids, (bis(2-hydroxyethyl)ammonium acetate and triethylammonium acetate). When water is present in an ionic liquid, electrooxidation of a gold electrode forms gold oxides. Thus, application of an anodic potential scan or holding the potential of the electrode at a very positive value leads to accumulation of an oxide film. On applying a cathodic potential scan, a sensitive stripping peak is produced as a result of the reduction of gold oxide back to gold. The magnitude of the peak current generated from the stripping process is a function of the water concentration in an ionic liquid. The method requires no addition of reagents and can be used for the sensitive and in situ determination of water present in small volumes of ionic liquids. Importantly, the method allows the determination of water in the carboxylic acid-based ionic liquids, such as acetate-based protic ionic liquids, where the widely used Karl Fischer titration method suffering from an esterification side reaction which generates water as a side product.

  14. SQUARE WAVE CATHODIC STRIPPING VOLTAMMETRY ADSORPTIVE FOR NICKEL AND COBALT ANALYSIS

    Directory of Open Access Journals (Sweden)

    Saryati Saryati

    2010-06-01

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

  15. The cyclic renewable mercury film silver based electrode for determination of molybdenum(VI) traces using adsorptive stripping voltammetry.

    Science.gov (United States)

    Piech, Robert; Baś, Bogusław; Kubiak, Władysław W

    2008-07-15

    The new cyclic renewable mercury film silver based electrode (Hg(Ag)FE), applied for the determination of molybdenum(VI) traces using differential pulse adsorptive cathodic stripping voltammetry (DP AdSV) is presented. The Hg(Ag)FE electrode is characterized by very good surface reproducibility (pulse height, step potential and supporting electrolyte composition are optimized. The calibration graph is linear from 2 nM (192 ng L(-1)) to 200 nM (19 microg L(-1)) for an accumulation time of 15s, with correlation coefficient of 0.9995. For a Hg(Ag)FE with a surface area of 3.5mm(2) the detection limit for an accumulation time of 60s is as low as 8 ng L(-1). The repeatability of the method at a concentration level of the analyte as low as 2.4 microg L(-1), expressed as R.S.D. is 1.3% (n=7). The proposed method was successfully applied and validated by studying the certified reference material TMRAIN-95 and simultaneous recovering of Mo(VI) from spiked water and sediment samples.

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

    Science.gov (United States)

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

    2014-12-01

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

  17. Cathodic stripping voltammetry of trace Mn(II) at carbon film electrodes.

    Science.gov (United States)

    Filipe, Olga M S; Brett, Christopher M A

    2003-12-04

    A sensitive voltammetric method is presented for the determination of tract levels of Mn (II) using carbon film electrodes fabricated from carbon resistors of 2 Omega. Determination of manganese was made by square wave cathodic stripping voltammetry (CSV), with deposition of manganese as manganese dioxide. Chronoamperometric experiments were made to study MnO(2) nucleation and growth. As a result, it was found to be necessary to perform electrode conditioning at a more positive potential to initiate MnO(2) nucleation. Under optimised conditions the detection limit obtained was 4 nM and the relative standard deviation for eight measurements of 0.22 nM was 5.3%. Interferences from various metal ions on the response CSV of Mn(II) were investigated, namely Cd(II), Ni(II), Cu(II), Cr(VI), Pb(II), Zn(II) and Fe(II). Application to environmental samples was demonstrated.

  18. Determination of picomolar levels of iron in seawater using catalytic cathodic stripping voltammetry.

    Science.gov (United States)

    Obata, H; van den Berg, C M

    2001-06-01

    A new procedure for the direct determination of picomolar levels of iron in seawater is presented. Cathodic stripping voltammetry (CSV) is preceded by adsorptive accumulation of the iron(III)-2,3-dihydroxynaphthalene (DHN) complex from seawater, containing 20 microM DHN at pH 8.0, onto a static mercury drop electrode, followed by reduction of the adsorbed species. The reduction current is catalytically enhanced by the presence of 20 mM bromate. Optimized conditions include a 60-s adsorption period at -0.1 V and a voltammetric scan using sampled dc modulation at 10 Hz. In these conditions, a detection limit of 13 pM iron in seawater was achieved which can be lowered further by extending the adsorption time to 300 s. The new catalytic CSV method is approximately 5 times more sensitive than existing CSV methods and was tested on samples from the Atlantic Ocean.

  19. Lead migration from toys by anodic stripping voltammetry using a bismuth film electrode.

    Science.gov (United States)

    Leal, M Fernanda C; Catarino, Rita I L; Pimenta, Adriana M; Souto, M Renata S; Afonso, Christelle S; Fernandes, Ana F Q

    2016-09-02

    Metals may be released from toys via saliva during mouthing, via sweat during dermal contact, or via gastric and intestinal fluids after partial or whole ingestion. In this study, we determined the lead migration from toys bought on the Portuguese market for children below 3 years of age. The lead migration was performed according to the European Committee for Standardization EN 71-3, which proposes a 2-hour migration test that simulates human gastric conditions. The voltammetric determination of migrated lead was performed by anodic stripping voltammetry (ASV) at a bismuth film electrode (BiFE). For all the analyzed toys, the values of migrated lead did not exceed the limits imposed by the European Committee for Standardization EN 71-3 (90 mg kg(-1)) and by the EU Directive 2009/48/EC (13.5 mg kg(-1)) on the safety of toys.

  20. Bare and Polymer-Coated Indium Tin Oxide as Working Electrodes for Manganese Cathodic Stripping Voltammetry.

    Science.gov (United States)

    Rusinek, Cory A; Bange, Adam; Warren, Mercedes; Kang, Wenjing; Nahan, Keaton; Papautsky, Ian; Heineman, William R

    2016-04-19

    Though an essential metal in the body, manganese (Mn) has a number of health implications when found in excess that are magnified by chronic exposure. These health complications include neurotoxicity, memory loss, infertility in males, and development of a neurologic psychiatric disorder, manganism. Thus, trace detection in environmental samples is increasingly important. Few electrode materials are able to reach the negative reductive potential of Mn required for anodic stripping voltammetry (ASV), so cathodic stripping voltammetry (CSV) has been shown to be a viable alternative. We demonstrate Mn CSV using an indium tin oxide (ITO) working electrode both bare and coated with a sulfonated charge selective polymer film, polystyrene-block-poly(ethylene-ran-butylene)-block-polystyrene-sulfonate (SSEBS). ITO itself proved to be an excellent electrode material for Mn CSV, achieving a calculated detection limit of 5 nM (0.3 ppb) with a deposition time of 3 min. Coating the ITO with the SSEBS polymer was found to increase the sensitivity and lower the detection limit to 1 nM (0.06 ppb). This polymer modified electrode offers excellent selectivity for Mn as no interferences were observed from other metal ions tested (Zn(2+), Cd(2+), Pb(2+), In(3+), Sb(3+), Al(3+), Ba(2+), Co(2+), Cu(2+), Ni(3+), Bi(3+), and Sn(2+)) except Fe(2+), which was found to interfere with the analytical signal for Mn(2+) at a ratio 20:1 (Fe(2+)/Mn(2+)). The applicability of this procedure to the analysis of tap, river, and pond water samples was demonstrated. This simple, sensitive analytical method using ITO and SSEBS-ITO could be applied to a number of electroactive transition metals detectable by CSV.

  1. Application of thin-shielded mercury microelectrodes in anodic stripping voltammetry.

    Science.gov (United States)

    Daniele, Salvatore; Bragato, Carlo; Baldo, M Antonietta; Ciani, Ilenia

    2008-10-19

    The performance in anodic stripping voltammetry (ASV) of hemispherical mercury microelectrodes, fabricated by electrodeposition of liquid mercury on the surface of Pt microdisks which were surrounded by a rather thick or thin insulating shield, was compared. The Pt microdisks were produced by sealing a wire of 25 microm diameter into a glass capillary, and by coating the cylindrical length of the Pt wire with a cathodic electrophoretic paint. The ratio of the overall tip radius b, to the basal radius of the electrode a, so-called RG=b/a, was equal to 110+/-10 and 1.52+/-0.01 for the thick- and thin-shielded microdisk, respectively. The mercury microelectrodes were characterized by cyclic voltammetry at 1 mVs(-1), in 1mM Ru(NH(3))(6)(3+) aqueous solution. The steady-state voltammogram recorded with the thin-shielded mercury microelectrode displayed less hysteresis, while the steady-state current was about 30% higher than that of the thicker one. This was a consequence of the additional flux due to diffusion from behind the plane of the electrode. The flux enhancement, which was operative at the thin-shielded mercury microelectrode during the deposition step in the ASV experiments, allowed recording stripping peaks for Cd and Pb, which resulted about 32% larger than those recorded at the thicker shielded mercury microelectrode, under same experimental conditions. The usefulness of the thin-shielded mercury microelectrode for ASV measurements in real samples was verified by determining the content of heavy metal ions released in the pore water (pH 4.5) of a soil slurry.

  2. Zinc Detection in Serum by Anodic Stripping Voltammetry on Microfabricated Bismuth Electrodes.

    Science.gov (United States)

    Jothimuthu, Preetha; Wilson, Robert A; Herren, Josi; Pei, Xing; Kang, Wenjing; Daniels, Rodney; Wong, Hector; Beyette, Fred; Heineman, William R; Papautsky, Ian

    2013-02-01

    Zinc (Zn) homeostasis is required for a functional immune system. Critically ill patients often exhibit decreased Zn serum concentrations and could potentially benefit from Zn supplementation as a therapeutic strategy. However, the conventional approaches to monitoring Zn are time consuming and costly. This work reports on detection of Zn by anodic stripping voltammetry (ASV) on bismuth electrodes in a microfabricated electrochemical cell. The working potential window of the electrodeposited bismuth film electrode was investigated by cyclic voltammetry, while square wave ASV was used for measuring Zn in acetate buffer and blood serum. Conditions critical to sensing, such as preconcentration potential, preconcentration time, and buffer pH, were optimized for Zn detection. The sensor was successfully calibrated with pH 6 acetate buffer in the physiologically-relevant range of 5 μM to 50μM Zn and exhibited well-defined and highly repeatable peaks. The sensor was used to demonstrate measurement of Zn in blood serum digested in HCl. The results of this work show that Zn detection in serum is possible with smaller sample volumes (μL vs. μL) and faster turnaround time (hours vs. days) as compared with the conventional spectroscopic methods.

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

    Science.gov (United States)

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

    2017-02-01

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

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

    Science.gov (United States)

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

    2002-07-19

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

  5. An optimization procedure for determination of metallothionein by square wave cathodic stripping voltammetry: application to marine worms.

    Science.gov (United States)

    El Hourch, Mohamed; Dudoit, Arnaud; Amiard, Jean-Claude

    2004-02-01

    Electrochemical determination of metallothionein (MT) is widely used for environmental studies. This article describes the development and optimization of the procedure for the quantification of metallothionein by square wave cathodic stripping voltammetry. The determination is based on the complexation of cisplatin and MT and the subsequent reduction of the complexes at the electrode. In order to achieve the highest possible sensitivity and resolution of the peak, an optimization of the experimental parameters has been carried out using experimental design methodology (response surface). Seven chemical and physical parameters, namely, pH, cisplatin concentration, buffer concentration, deposition potential, square wave frequency, amplitude of pulse, and step potential, have been optimized to give 9.0, 5.9 microM, 0.65 M, -0.2 mV, 229 Hz, 46 mV, and 2 mV, respectively. Method characterization has been performed, leading to a detection limit of 0.1 microg L(-1). Quantification of MT in polychaetes and comparison with the modified Brdicka procedure were also carried out.

  6. Application of bismuth bulk annular band electrode for determination of ultratrace concentrations of thallium(I) using stripping voltammetry.

    Science.gov (United States)

    Węgiel, Krystian; Jedlińska, Katarzyna; Baś, Bogusław

    2016-06-05

    A study of a new type of mercury-free working electrode - the bismuth bulk annular band working electrode (BiABE) - applied for thallium(I) detection via differential pulse anodic stripping voltammetry (DP ASV), preceded by the complexation of interfering ions (Cd(2+), Pb(2+)) with EDTA in an acetate buffer (pH 4.5), is reported. The optimisation of experimental conditions included selection of the appropriate supporting electrolyte solution, potential and time of preconcentration, and DP mode parameters. The peak current was proportional to the concentration of Tl(I) in the range from 0.5 to 49nmolL(-1) (R=0.9992) and from 0.05 to 1.4nmolL(-1) (R=0.9987) for accumulation times of 60s and 300s, respectively. For 60s of accumulation time, the LOD was 0.005nmolL(-1) (1ngL(-1)) (at S/N=3), and the sensitivity of 18.5nA/nM was achieved. The relative standard deviation for 4.9nmolL(-1) of Tl(I) was 4.3% (n=5). Finally, the proposed method was successfully applied to determine Tl(I) in the certified reference materials-waters (SPS-SW1 and SPS-SW2) as well as the spiked tap and river water samples.

  7. Determination of Antimony (III in Real Samples by Anodic Stripping Voltammetry Using a Mercury Film Screen-Printed Electrode

    Directory of Open Access Journals (Sweden)

    Olga Domínguez-Renedo

    2009-01-01

    Full Text Available This paper describes a procedure for the determination of antimony (III by differential pulse anodic stripping voltammetry using a mercury film screen-printed electrode as the working electrode. The procedure has been optimized using experimental design methodology. Under these conditions, in terms of Residual Standard Deviation (RSD, the repeatability (3.81 % and the reproducibility (5.07 % of the constructed electrodes were both analyzed. The detection limit for Sb (III was calculated at a value of 1.27×10–8 M. The linear range obtained was between 0.99 × 10–8 – 8.26 × 10–8 M. An analysis of possible effects due to the presence of foreign ions in the solution was performed and the procedure was successfully applied to the determination of antimony levels in pharmaceutical preparations and sea water samples.

  8. Pseudo-stir bar hollow fiber solid/liquid phase microextraction combined with anodic stripping voltammetry for determination of lead and cadmium in water samples.

    Science.gov (United States)

    Es'haghi, Zarrin; Hoseini, Hasan Ali; Mohammadi-Nokhandani, Saeed; Ebrahimi, Javad

    2014-11-01

    A new procedure is presented for the determination of low concentrations of lead and cadmium in water samples. Ligand assisted pseudo-stir bar hollow fiber solid/liquid phase microextraction using sol-gel sorbent reinforced with carbon nanotubes was combined with differential pulse anodic stripping voltammetry for simultaneous determination of cadmium and lead in tap water, and Darongar river water samples. In the present work, differential pulse anodic stripping voltammetry (DPASV) using a hanging mercury drop electrode (HMDE) was used in order to determine the ultra trace level of lead and cadmium ions in real samples. This method is based on accumulation of lead and cadmium ions on the electrode using different ligands; Quinolin-8-ol, 5,7-diiodo quinoline-8-ol, 4,5-diphenyl-1H-imidazole-2(3H)-one and 2-{[2-(2-Hydroxy-ethylamino)-ethylamino]-methyl}-phenol as the complexing agent. The optimized conditions were obtained. The relationship between the peak current versus concentration was linear over the range of 0.05-500 ng mL(-1) for Cd (II) and Pb (II). The limits of detection for lead and cadmium were 0.015 ng mL(-1) and 0.012 ng mL(-1), respectively. Under the optimized conditions, the pre-concentration factors are 2440 and 3710 for Cd (II) and Pb (II) in 5 mL of water sample, respectively.

  9. Detecting Naturally-Produced Sulfide Nanoparticles by Adsorptive, Cathodic Stripping Voltammetry.

    Science.gov (United States)

    Helz, G. R.; Krznaric, D.; Bura-Nakic, E.; Ciglenecki, I.

    2007-12-01

    Growing evidence implies that metal sulfide nanoparticles of natural origin exist in some aquatic environments. These nanoparticles could play important roles as mediators of trace metal nutrition and toxicity. Thermodynamics suggests that in sulfidic environments (total transition metaltotal sulfide) the most insoluble metal sulfide (usually Hg or Cu) will form the predominant sulfide nanoparticle. New experimental methods for detecting and distinguishing between such nanoparticles are needed. We report that mercury electrodes effectively preconcentrate a number of different metal sulfide nanoparticles, enabling their detection by adsorptive cathodic stripping voltammetry. Voltammetrically, nanoparticulate analytes differ fundamentally from dissolved analytes; e.g. analyte accumulation is very sensitive to electrolyte composition and concentration in accord with the Schulze-Hardy Rule. EDTA or acid treatment of samples is useful for distinguishing highly insoluble nanoparticles (HgS, CuS) from FeS. Nanoparticulate sulfur potentially interferes. Supersaturated solutions can generate artifactual analyte on Hg electrode surfaces. Despite such potential pitfalls, progress is encouraging. Preliminary, qualitative results from natural waters will be reported.

  10. Determination of diclofenac using electromembrane extraction coupled with stripping FFT continuous cyclic voltammetry.

    Science.gov (United States)

    Mofidi, Zahra; Norouzi, Parviz; Seidi, Shahram; Ganjali, Mohammad Reza

    2017-06-15

    For the first time, on-line and ultra-sensitive determination of trace amount of diclofenac in whole blood sample was performed by coupling of electromembrane extraction (EME) and stripping fast Fourier transform continuous cyclic voltammetry (SFFTCCV). In SFFTCCV, the potential waveform was continuously applied on a carbon paste electrode and the electrode response was obtained by subtracting the background current and integrating the current in potential range of the analyte oxidation. A central composite design was used for the optimization of the parameters influencing the extraction efficiency. By applying a DC potential of 20 V during 28 min of extraction, diclofenac was migrated from the sample solution (pH 5), into a thin layer of 1-octanol immobilized in the pores of a porous flat sheet membrane and then into the acceptor solution (pH 7). The method presented a good linearity within the range of 5-1000 ng mL(-1) with a determination coefficient of 0.993 in whole blood samples. Limits of detection (LOD) and quantification (LOQ) were found to be 1.0 ng mL(-1) and 5.0 ng mL(-1) respectively. Copyright © 2017 Elsevier B.V. All rights reserved.

  11. Determination of Sulpiride by Linear Sweep Stripping Voltammetry at a Mercury Electrode

    Institute of Scientific and Technical Information of China (English)

    2003-01-01

    This paper reports the electrochemical properties of sulpiride at a mercury electrode, especially its adsorptive characteristic. Sulpiride dissolved in a supporting electrolyte of a McIlvaine buffer at pH 6.8 represents a sensitive and well defined reduction wave by linear sweep stripping voltammetry. This method is based on the pre-concentration and the reduction of sulpiride at a hung mercury drop electrode. The reduction peak potential is -1.72 V(vs. Ag-AgCl) and the peak current is proportional to the concentration of sulpiride in the range of 0.1-0.6 μg/mL. The detection limit is 0.025 μg/mL obtained under the experimental conditions selected in this work. The electrochemical properties of this system were investigated, and the proposed method was applied to the determination of sulpiride in pharmaceutical tablets with satisfactory results. It was compared well with the UV spectrophotometric method, showing a superior sensitivity.

  12. Determination of humic substances in natural waters by cathodic stripping voltammetry of their complexes with iron.

    Science.gov (United States)

    Laglera, Luis M; Battaglia, Gianluca; van den Berg, Constant M G

    2007-09-05

    A new voltammetric method is presented for the measurement of humic substances (HS) in natural waters. The method is based on catalytic cathodic stripping voltammetry (CSV) and makes use of adsorptive properties of iron-HS complexes on the mercury drop electrode at natural pH. A fulvic acid standard (IHSS) was used to confirm the voltammetric response (peak potential and sensitivity) for the HS for natural water samples. Optimized conditions included the linear-sweep mode, deposition at -0.1 V, pH buffered at 8 and a scan rate of 50 mV s(-1). At a deposition time of 240 s in the presence of 10 nM iron and 30 mM bromate, the detection limit was 5 microg L(-1) HS in seawater, which could be lowered further by an increase in the bromate concentration, or in the adsorption time. The method was used to determine HS in the Irish Sea which were found to occur at levels between 60 and 600 microg L(-1). The new method is sufficiently sensitive to detect the low HS content in oceanic samples and has implications to the study of iron speciation.

  13. Determination of copper speciation in highway stormwater runoff using competitive ligand exchange - Adsorptive cathodic stripping voltammetry.

    Science.gov (United States)

    Nason, Jeffrey A; Sprick, Matthew S; Bloomquist, Don J

    2012-11-01

    Low concentrations of dissolved copper have been shown to adversely affect the olfactory system of salmonid species, impairing their ability to avoid predators and likely increasing mortality. These studies have resulted in increased regulatory scrutiny of stormwater discharges to surface waters inhabited by threatened and endangered salmonid species. Because it is primarily the free ionic (Cu(2+)) and weakly complexed forms of copper that are bioavailable, it is critical to understand the speciation of copper in stormwater. This paper reports on the characterization of copper binding ligands and copper speciation in composite samples of highway stormwater runoff collected at four sites in Oregon, USA using competitive ligand exchange - adsorptive cathodic stripping voltammetry (CLE-ACSV). Although the concentration and strength of copper binding ligands in stormwater varied considerable between sites and storms, the vast majority (>99.9%) of the total dissolved copper in composite samples was complexed by organic ligands in stormwater. Although total dissolved copper concentrations range from 2 to 20 μg/L, the analytically determined free ionic copper concentrations did not exceed 10(-10) M (6.3 ng/L) in any of the fully characterized samples, suggesting that much of the copper in highway stormwater is not bioavailable. Analytically determined free ionic copper concentrations were compared with those predicted by a readily available chemical equilibrium models and found to be in reasonable agreement. Copyright © 2012 Elsevier Ltd. All rights reserved.

  14. Advantages of using a mercury coated, micro-wire, electrode in adsorptive cathodic stripping voltammetry.

    Science.gov (United States)

    Gun, Jenny; Salaün, Pascal; van den Berg, Constant M G

    2006-06-30

    A mercury coated, gold, micro-wire electrode is used here for the determination of iron in seawater by catalytic cathodic stripping voltammetry (CSV) with a limit of detection of 0.1 nM Fe at a 60s adsorption time. It was found that the electrode surface is stable for extended periods of analyses (at least five days) and that it is reactivated by briefly (2s) applying a negative potential prior to each scan. Advantages of this electrode over mercury drop electrodes are that metallic mercury use is eliminated and that it can be readily used for flow analysis. This is demonstrated here by the determination of iron in seawater by continuous flow analysis. It is likely that this method can be extended to other elements. Experiments using bismuth coated, carbon fibre, electrodes showed that the bismuth catalyses the oxidation of the important oxidants bromate and hydrogen peroxide, which makes it impossible to use bismuth based electrodes for catalytic CSV involving these oxidants. For this reason mercury coated electrodes retain a major advantage for catalytic voltammetric analyses.

  15. Chemical speciation of iron in seawater by cathodic stripping voltammetry with dihydroxynaphthalene.

    Science.gov (United States)

    van den Berg, Constant M G

    2006-01-01

    The chemical speciation of iron in seawater is determined by cathodic stripping voltammetry using 2,3-dihydroxynaphthalene (DHN) as adsorptive and competing ligand. The optimized conditions include a DHN concentration of 0.5-1 microM, seawater at its original pH of 8, and equilibration overnight. The alpha-coefficient for DHN (=[FeDHN]/[Fe']) was calibrated against EDTA giving values of 166 for 0.5 microM DHN and 366 at 1 microM DHN and a value of 8.51 +/- 0.07 for log K'(Fe'DHN). The dissociation of the natural iron species FeL was found to have a characteristic reaction time of 50 min, indicating that titrations should be equilibrated overnight rather than the shorter periods sometimes used onboard ship. The method was applied to samples from the Pacific giving ligand concentrations of 1.1 and 1.6 nM for deep and surface waters, respectively, with an average value for log K'(FeL) of 11.9 +/- 0.3 compared to a value of 11.5 for the siderophore deferoxamine. The results are similar to those obtained previously for similar samples, but the new method has much greater sensitivity for iron than previous methods, leading to lower limits of detection and shorter analysis time.

  16. Electrochemical analysis of the alanine phenylthiohydantoin derivative by cathodic stripping voltammetry.

    Science.gov (United States)

    Vilaseca, C; Quintana, M C; Vicente, J; Hernández, P; Hernández, L

    2008-08-01

    A square-wave cathodic stripping voltammetry method for alanine determination as its phenylthiohydantoin (PTH-alanine) derivative is developed. To this end, all the chemical and instrumental variables affecting the determination of PTH-alanine are optimized. From studies of the mechanisms governing the electrochemical response of PTH-alanine, it was concluded that it is an electrochemically irreversible system with a diffusive-adsorptive reduction phenomenon. Under optimal conditions, the variation of analytical signal (I(p)) with PTH-alanine concentration is linear in the 2.4x10(-8)-4.8x10(-7) M range, with a LOD of 1.2x10(-8) M and a LOQ of 4.2x10(-8) M, a RSD (%) less than 11%, and a E(r) (%) less than 10%. The optimized method was applied to the determination of PTH-alanine obtained from a synthetic protein after Edman reaction and the results were corroborated by high-performance liquid chromatography with UV detection.

  17. Rapid determination of picomolar titanium in seawater with catalytic cathodic stripping voltammetry.

    Science.gov (United States)

    Croot, Peter L

    2011-08-15

    Titanium (Ti) is present as a trace element in seawater at extremely low concentrations (5-350 pM, where 1 pM = 10(-12) mol L(-1)) throughout the water column. Presently, little is known about the marine biogeochemistry of Ti and there is a distinct lack of oceanic measurements of Ti , because of the combined difficulties of trace-metal clean sampling for an element at such low levels and the lack of a suitable shipboard method of analysis. Here, a new cathodic stripping voltammetry procedure is presented for the rapid determination of Ti at pM concentrations in seawater that is capable of being used directly at sea. This method utilizes the catalytic enhancement of the reduction of the complex formed between Cupferron (N-nitrosophenylhydroxylamine) and Ti(IV). While Cupferron itself acts as both a complexing agent and an oxidizing agent, it was found that the optimal sensitivity was with bromate as an auxiliary oxidant. An advantage of this method is that it is useable over the pH range of 5.5-8. Under the conditions employed in this work, detection limits ranged from 5 pM to 12 pM. This new catalytic method is significantly more sensitive than existing methods and has been extensively tested at sea in the Atlantic and Southern Oceans.

  18. Direct analysis of palladium in active pharmaceutical ingredients by anodic stripping voltammetry.

    Science.gov (United States)

    Rosolina, Samuel M; Chambers, James Q; Xue, Zi-Ling

    2016-03-31

    Anodic stripping voltammetry, a classical electroanalytical method has been optimized to analyze trace Pd(II) in active pharmaceutical ingredient matrices. The electroanalytical approach with an unmodified glassy carbon electrode was performed in both aqueous and 95% DMSO/5% water (95/5 DMSO/H2O) solutions, without pretreatment such as acid digestion or dry ashing to remove the organics. Limits of detection (LODs) in the presence of caffeine and ketoprofen were determined to be 11 and 9.6 μg g(-1), with a relative standard deviation (RSD) of 5.7% and 2.3%, respectively. This method is simple, highly reproducible, sensitive, and robust. The instrumentation has the potential to be portable and the obviation of sample pretreatment makes it an ideal approach for determining lost catalytic metals in pharmaceutical-related industries. Furthermore, the simultaneous detection of Pd(II) with Cd(II) and Pb(II) in the low μg L(-1) range indicates that this system is capable of simultaneous multi-analyte analysis in a variety of matrices.

  19. Determination of Anionic Surfactants Using Atomic Absorption Spectrometry and Anodic Stripping Voltammetry

    Science.gov (United States)

    John, Richard; Lord, Daniel

    1999-09-01

    An experiment has been developed for our undergraduate analytical chemistry course that demonstrates the indirect analysis of anionic surfactants by techniques normally associated with metal ion determination; that is, atomic absorption spectroscopy (AAS) and anodic stripping voltammetry (ASV). The method involves the formation of an extractable complex between the synthetic surfactant anion and the bis(ethylenediamine)diaqua copper(II) cation. This complex is extracted into chloroform and then back-extracted into dilute acid. The resulting Cu(II) ions are determined by AAS and ASV. Students are required to determine the concentration of a pre-prepared "unknown" anionic surfactant solution and to collect and analyze a real sample of their choice. After the two extraction processes, students typically obtain close to 100% analytical recovery. Correlation between student AAS and ASV results is very good, indicating that any errors that occur probably result from their technique (dilutions, extractions, preparation of standards, etc.) rather than from the end analyses. The experiment is a valuable demonstration of the following analytical principles: indirect analysis; compleximetric analysis; liquid-liquid (solvent) extraction; back-extraction (into dilute acid); analytical recovery; and metal ion analysis using flame-AAS and ASV.

  20. Anodic stripping voltammetry at in situ bismuth-plated carbon and gold microdisc electrodes in variable electrolyte content unstirred solutions.

    Science.gov (United States)

    Baldrianova, L; Svancara, I; Economou, A; Sotiropoulos, S

    2006-10-27

    Carbon and gold microdisc electrodes (30 and 10 microm, respectively) have been tested as substrates for in situ bismuth film plating from unstirred solutions of variable acetate buffer content and were subsequently used in the anodic stripping voltammetry determination of Pb(II) and Cd(II) ions. The effects of Bi(III) concentration, analyte accumulation time, stirring as well as supporting electrolyte content have been studied. Under optimal conditions good voltammetric responses were obtained by means of square wave anodic stripping voltammetry in unstirred analyte solutions of 5 x 10(-8) to 10(-6)M, even in the absence of added buffer. In an indicative application, Pb(II) ion levels were determined in tap water using bismuth-plated carbon microdisc electrodes.

  1. Redox magnetohydrodynamics enhancement of stripping voltammetry of lead(II), cadmium(II) and zinc(II) ions using 1,4-benzoquinone as an alternative pumping species.

    Science.gov (United States)

    Ensafi, Ali A; Nazari, Z; Fritsch, I

    2012-01-21

    Differential pulse anodic stripping voltammetry (DPASV) coupled with redox-magnetohydrodynamics (MHD) is used to enhance the anodic stripping voltammetry (ASV) response using a mercury thin film-glassy carbon electrode. The sensitivity increased to at least a factor of two (at 1.2 T) and is facilitated by using 20.0 mmol L(-1) 1,4-benzoquinone as an alternative pumping species to enhance ASV by redox-MHD. The MHD force formed by the cross-product of ion flux with magnetic field induces solution convection during the deposition step, enhancing mass transport of the analytes to the electrode surface and increasing their preconcentrated quantity in the mercury thin film. Therefore, larger ASV peaks and improved sensitivities are obtained, compared with analyses performed without a magnet. The influence of pH, 1,4-benzoquinone concentration, accumulation potential, and time are also investigated. Detection limits of 0.05, 0.09 and 2.2 ng mL(-1) Cd(II), Pb(II) and Zn(II) were established with an accumulation time of 65 s. The method is used for the analysis of Cd(II), Pb(II) and Zn(II) in different water samples, certified reference materials, and saliva samples with satisfactory results.

  2. Determination of Total Iodine Concentration in Aquatic Environments Using Cathodic Stripping Voltammetry Combined with Sodium Hypochlorite (NaClO) Oxidation

    National Research Council Canada - National Science Library

    SATOH, Yuhi; OTOSAKA, Shigeyoshi; SUZUKI, Takashi

    2014-01-01

    An easy and fast method for the determination of total iodine in environmental samples by cathodic stripping voltammetry combined with sodium-hydrochlorous-induced oxidation (NaClO oxidation) has been developed...

  3. Laser pulse modulation instabilities in partially stripped plasma

    Institute of Scientific and Technical Information of China (English)

    Hu Qiang-Lin; Liu Shi-Bing; Jiang Yi-Jian

    2005-01-01

    The laser pulse modulation instabilities in partially stripped plasma were discussed based on the phase and group velocities of the laser pulse and the two processes that modulation instabilities excited. The excitation condition and growth rate of the modulation instability were obtained. It was found that the positive chirp and competition between normal and abnormal dispersions play important roles in the modulation instability. In the partially stripped plasma,the increased positive chirp enhances the modulation instability, and the dispersion competition reduces it.

  4. Speciation study of aluminium in beverages by Competitive Ligand Exchange-Adsorptive Stripping Voltammetry.

    Science.gov (United States)

    Magnier, A; Fekete, V; Van Loco, J; Bolle, F; Elskens, M

    2014-05-01

    Competitive Ligand Exchange-Adsorptive Stripping Voltammetry (CLE-AdSV) was used for determining the speciation of aluminium in commonly consumed beverages (water, tea, infusion, coffee, orange juice, tomato juice, beer and red wine). Aluminium determination involves the adsorption of Al-complexes with the ligand cupferron onto a hanging mercury drop electrode. All samples were studied at pH 6.5 with an accumulation step at -0.60 V (all potential values in the paper are given versus the Ag/AgCl, [KCl]=3 M reference electrode) during 60 s, and a final cupferron concentration of 4 × 10(-4)M. These conditions were used to establish (i) the concentration of electro-labile aluminium, (ii) the range of ligand concentrations and (iii) the conditional stability constants of beverage samples using titration procedures. The results based on Ruzic plots were compared to computer simulation with Visual MINTEQ. This comparison suggests that labile monomeric Al-forms and soluble organic complexes of low molecular weight can be quantified by the CLE-AdSV procedure. Overall the relative uncertainties on the determination of the electro-active Al fraction and the complexing parameters, i.e., concentration and conditional stability constant of natural ligands in the samples, are less than 15%. Thanks to these results, information on Al bioavailability in beverages was collected and discussed. This study also illustrates the value of computer simulations when complex, time-consuming voltammetric techniques are applied. Copyright © 2014 Elsevier B.V. All rights reserved.

  5. Determination of trace cobalt concentrations in human serum by adsorptive stripping voltammetry.

    Science.gov (United States)

    Kajic, Petra; Milosev, Ingrid; Pihlar, Boris; Pisot, Venceslav

    2003-01-01

    The goal of our study was to develop an accurate and reliable method for determining trace cobalt concentrations in human serum. The method was used to determine cobalt in the sera of healthy persons and patients with orthopaedic implants containing cobalt - a possible source of systemic release of cobalt into the human body. This goal is of vital interest since cobalt and its compounds are classified by IARC as potentially carcinogenic to humans. We used an electrochemical method, adsorptive stripping voltammetry (AdSV), which made possible the low detection limit and high sensitivity needed for measurements in human serum. The serum was acid digested by a combination of H2SO4, HNO3 and H2O2 in a 10 mL Kjeldhal flask. The digested sample was then dissolved in 0.1 mol/L ammonia buffer, pH 9.0 +/- 0.2. The determination is based on the adsorptive collection of the complex of cobalt (II) with dimethylglyoxime on a hanging mercury drop electrode (HMDE). The optimum values of adsorption potential and time were determined to be -0.8 V and 60 s. The optimisation of the sample digestion protocol and measurement procedures ensured the reliable assessment of low cobalt concentrations, down to 0.03 microg/L. The mean concentration of serum cobalt in four healthy persons was 0.11 +/- 0.06 microg/L, and in four patients with total hip replacements 0.34 +/- 0.07 microg/L. This method will be used routinely for measuring serum cobalt levels in patients with total hip replacements.

  6. Anodic stripping voltammetry of synthesized CdS nanoparticles at boron-doped diamond electrodes

    Energy Technology Data Exchange (ETDEWEB)

    Hayat, Mohammad; Ivandini, Tribidasari A., E-mail: ivandini.tri@sci.ui.ac.id; Saepudin, Endang [Department of Chemistry, FMIPA, Universitas Indonesia, Kampus UI Depok (Indonesia); Einaga, Yasuaki [Department of Chemistry, Keio University (Japan)

    2016-04-19

    Cadmium sulphide (CdS) nanoparticles were chemically synthesized using reverse micelles microreactor methods. By using different washing treatments, UV-Vis spectroscopy showed that the absorption peaks appeared at 465 nm, 462 nm, 460 nm, and 459 nm respectively for CdS nanoparticles without and with 1, 2, and 3 times washing treatments using pure water. In comparison with the absorbance peak of bulk CdS at 512 nm, the shifted absorption peaks, indicates that the different sizes of CdS can be prepared. Anodic stripping voltammetry of the CdS nanoparticles was then studied at a boron-doped diamond electrode using 0.1 M KClO{sub 4} and 0.1 M HClO{sub 4} as the electrolytes. A scan rate of 100 mV/s with a deposition potential of -1000 mV (vs. Ag/AgCl) for 60 s at a potential scan from -1600 mV to +800 mV (vs. Ag/AgCl) was applied as the optimum condition of the measurements. Highly-accurate linear calibration curves (R{sup 2} = 0.99) in 0.1 M HClO{sub 4} with the sensitivity of 0.075 mA/mM and the limit of detection of 81 µM in 0.1 M HClO{sub 4} can be achieved, which is promising for an application of CdS nanoparticles as a label for biosensors.

  7. Electrochemical determination of closantel in the commercial formulation by square-wave adsorptive stripping voltammetry.

    Science.gov (United States)

    Brycht, Mariola; Nosal-Wiercińska, Agnieszka; Sipa, Karolina; Rudnicki, Konrad; Skrzypek, Sławomira

    2017-01-01

    In this paper, the square-wave adsorptive stripping voltammetric (SWAdSV) determination of the veterinary drug closantel using a renewable silver amalgam film electrode (Hg(Ag)FE) is presented. As observed in SWAdSV, closantel provided one well-shaped reduction peak suitable for analytical purposes at potential ca. -1.4 V in the Britton-Robinson (B-R) buffer at pH 7.0. At optimal conditions, the SWAdSV response of Hg(Ag)FE for determining closantel was linear over two concentration ranges of 5.0 × 10(-8) to 2.0 × 10(-7) mol dm(-3) and 2.0 × 10(-7) to 1.2 × 10(-6) mol dm(-3) with a detection limit of 1.1 × 10(-8) mol dm(-3). In addition, a relevance of the developed SWAdSV method was successfully verified by the quantitative analysis of closantel in the commercial formulation Closamectin Pour-On with satisfactory results (RSD = 5.8%, recovery = 101.8%). The results showed that the developed procedure can be adequate for screening purposes. Also, the electrochemical behavior of closantel was characterized by cyclic voltammetry, and it was found that closantel exhibited a quasi-reversible behavior with cathodic peak on the forward scan at ca. -1.4 V and anodic peak on the reverse scan at ca. -1.35 V vs. Ag/AgCl in B-R buffer, pH 7.0. As the obtained results showed that the electrode mechanism of closantel is controlled by the adsorption, the effect of adsorption was studied using the electrochemical impedance spectroscopy technique.

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

    Science.gov (United States)

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

    2016-07-01

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

  9. Determination of nitrofurantoin drug in pharmaceutical formulation and biological fluids by square-wave cathodic adsorptive stripping voltammetry.

    Science.gov (United States)

    Hammam, Essam

    2002-10-15

    Nitrofurnation is an antibacterial drug. It is used in the treatment of initial or recurrent urinary tract infections caused by susceptible organisms. The cyclic voltammogram of the drug in Britton-Robinson buffers (pH 2-11) exhibited a single well-defined cathodic peak at the hanging mercury drop electrode, that due to the reduction of its nitro group to the amine stage. A fully validated, sensitive, and reproducible developed procedure was described for determination of the drug in bulk form, pharmaceutical formulation, human serum and human urine using, square-wave cathodic adsorptive stripping voltammetry. The optimal experimental parameters for the drug assay were: accumulation potential = -0.4 V (vs. Ag/AgCl/ KCl(s)), accumulation time = 40 s, frequency = 120 Hz, pulse amplitude = 50 mV and scan increment = 10 mV in Britton-Robinson buffer (pH 10). A mean percentage recovery of 100.68 +/- 0.17 (n = 5) and a detection limit of 1.32 x 10(-10) M of bulk drug were achieved. Applicability to assay of the drug in pharmaceutical formulation, human serum and human urine was studied and illustrated. The mean percentage recoveries were found as: 101.49 +/- 0.65, 103.94 +/- 0.73 and 101.98 +/- 0.52 (n = 5) in pharmaceutical formulation, human serum and human urine, respectively. Detection limits of 2.86 x 10(-10) M and 5.77 x 10(-10) M nitrofurantoin were achieved in human serum and urine, respectively. Copyright 2002 Elsevier Science B.V.

  10. Simultaneous determination of textile dyes by Adsorptive Cathodic Stripping Voltammetry - doi: 10.4025/actascitechnol.v35i2.16595

    Directory of Open Access Journals (Sweden)

    Lidia Brizola Santos

    2013-04-01

    Full Text Available The Adsorptive Cathodic Stripping Voltammetry (ACSV - differential pulse proved to be an efficient method in the separation and quantification of two reactive textile dyes, Procion Yellow (PY and Procion Red (PR, each containing two azo groups as chromophores and two monochlorotriazine reactive groups, at nanomolar level. The linearity of the method obtained for each reactive dye was 30.15 – 633.15 nmol L-1 for PY in B-R buffer pH 8.0, and 62.56 – 982.291 nmol L-1 for PR in B-R buffer pH 8.0, using preconcentration at -0.1 V during 60 s.   

  11. Investigations on the use of anodic stripping voltammetry for the analyses of lead in saline environments

    Energy Technology Data Exchange (ETDEWEB)

    Case, C.W.

    1978-08-01

    Research is reported directed to modification of the anodic stripping voltammetry (ASV) analytic method in order to acquire data for lead from ambient sea water conditions, and development of a chemical model which uses these data to identify inorganic lead species for saline environments. Laboratory and field samples were analyzed for lead partitioning in: (a) KCl electrolyte solutions; (b) I.A.P.S.O. Standard Sea Water; (c) seawater samples from Quatsino Sound, British Columbia; (d) a series of seawater samples from San Francisco Bay; and (e) seawater samples from the Gulf of Mexico. The electrochemical traits of the lead species and the ASV oxidation potential expression are the fundamental constituents of the chemical model. The model uses the data from the analyses to provide the mass balance relationships for lead partitioned among the major anions in seawater. The laboratory analyses of KCl electrolyte and Standard Seawater give the following results. The modified ASV method and chemical model provide information on ambient labile and non-labile inorganic lead complexes in these saline solutions down to the parts-per-billion level. No purge and the simple electrodes cause some erratic behavior and spurious potentials, but the data are reproducible. In addition to Pb/sup 2 +/, the most dominant measured lead species in order include PbCO/sub 3//sup 0/, PbSO/sub 4//sup 0/, PbCl/sup +/, and Pb(NO/sub 3/)/sub 2//sup 0/ from the lead additions solution. The analyses of the field samples give the following results. Samples were taken from the partially anoxic basin in Quatsino Sound, British Columbia with one successful analysis which is for somewhat normal dissolved oxygen conditions. Data show that lead is partitioned among Pb/sup 2 +/, Pb(OH)/sub 2//sup 0/, PbCO/sub 3//sup 0/, and PbSO/sub 4//sup 0/. The analyses with purge for the San Francisco Bay water partitions lead among Pb/sup 2 +/, PbCO/sub 3//sup 0/, PbSO/sub 4//sup 0/, PbCl/sup +/, and Pb

  12. Cathodic adsorptive stripping voltammetry of an anti-emetic agent Granisetron in pharmaceutical formulation and biological matrix

    Institute of Scientific and Technical Information of China (English)

    Rajeev Jain; Ramkishor Sharma

    2012-01-01

    Granisetron showed one well-defined reduction peak at Hanging Mercury Drop Electrode (HMDE) in the potential range from -1.3 to -1.5 V due to reduction of C=N bond. Solid-phase extraction technique was employed for extraction of Granisetron from spiked human plasma. Granisetron showed peak current enhancement of 4.45% at square-wave voltammetry and 5.33% at cyclic voltammetry as compared with the non stripping techniques. The proposed voltammetric method allowed quantification of Granisetron in pharmaceutical formulation over the target concentration range of 5-200 ng/mL with detection limit 13.63 ng/mL, whereas in human plasma 50-225 ng/mL with detection limit 11.75 ng/mL.

  13. Recent Advances in Voltammetry

    Science.gov (United States)

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

    2015-01-01

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

  14. Recent Advances in Voltammetry.

    Science.gov (United States)

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

    2015-06-01

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

  15. Determination of Soil Base—Soluble Se by Anodic Stripping Voltammetry with Aurum Thin—Film Electrode

    Institute of Scientific and Technical Information of China (English)

    YANGZENG; HEYING; 等

    1994-01-01

    Determination of soil Se by anodic stripping voltammetry(ASV) with aurum thin-film electrode(ATFE)overcomes the interference of gold peak with selenium peak,and thus has a higher sensitivity with the miniumum detectable concentration being 0.017μg/mL,the standard deviation of the measured results leww than 0.012μg/g,the coefficient of variation lwoer than 10% ,and the recovery rate between 86% to 103%.Besides the measurement conditions,the digestion of soil sample was also studied in detail.

  16. Determination of trace amounts of Ga(III) by adsorptive stripping voltammetry with in situ plated bismuth film electrode.

    Science.gov (United States)

    Grabarczyk, Malgorzata; Wasąg, Joanna

    2015-11-01

    The determination of trace gallium using adsorptive stripping voltammetry at an in situ plated bismuth film electrode was described. The method was based on simultaneous film formation and the Ga(III)-cupferron complex preconcentration at -0.65 V and its cathodic stripping during the potential scan. The effect of Bi(III) and cupferron concentration, the influence of deposition potential and time, and the scan rate on the determination of Ga(III) were studied. A linear response in the concentration range of 3×10(-10) to 3×10(-7) mol L(-1) (r=0.998) was obtained with detection limit of 1.05×10(-10) mol L(-1) using accumulation time of 180 s. Finally, the bismuth film electrode was successfully applied for the determination of Ga(III) in certified reference material seawater NASS-5 with satisfactory results.

  17. Fabrication and Demonstration of Mercury Disc-Well Probes for Stripping-Based Cyclic Voltammetry Scanning Electrochemical Microscopy.

    Science.gov (United States)

    Barton, Zachary J; Rodríguez-López, Joaquín

    2017-03-07

    Scanning electrochemical microscopy (SECM) is a rising technique for the study of energy storage materials. Hg-based probes allow the extension of SECM investigations to ionic processes, but the risk of irreversible Hg amalgam saturation limits their operation to rapid timescales and dilute analyte solutions. Here, we report a novel fabrication protocol for Hg disc-well ultramicroelectrodes (UMEs), which retain access to stripping information but are less susceptible to amalgam saturation than traditional Hg sphere-caps or thin-films. The amalgamation and stripping behaviors of Hg disc-well UMEs are compared to those of traditional Hg sphere-cap UMEs and corroborated with data from finite element simulations. The improved protection against amalgam saturation allows Hg disc-wells to operate safely in highly concentrated environments at long timescales. The utility of the probes for bulk measurements extends also to SECM studies, where the disc geometry facilitates small tip-substrate gaps and improves both spatial and temporal resolution. Because they can carry out slow, high-resolution anodic stripping voltammetry approaches and imaging in concentrated solutions, Hg disc-well electrodes fill a new analytical niche for studies of ionic reactivity and are a valuable addition to the electrochemical toolbox.

  18. Glyphosate detection with ammonium nitrate and humic acids as potential interfering substances by pulsed voltammetry technique

    OpenAIRE

    MARTÍNEZ GIL, PABLO; Laguarda Miró, Nicolás; Soto Camino, Juan; Masot Peris, Rafael

    2013-01-01

    Pulsed voltammetry has been used to detect and quantify glyphosate on buffered water in presence of ammonium nitrate and humic substances. Glyphosate is the most widely used herbicide active ingredient in the world. It is a non-selective broad spectrum herbicide but some of its health and environmental effects are still being discussed. Nowadays, glyphosate pollution in water is being monitored but quantification techniques are slow and expensive. Glyphosate wastes are often detected in count...

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

    Science.gov (United States)

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

    2014-01-31

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

  20. Lab-on-a-Chip Sensor with Evaporated Bismuth Film Electrode for Anodic Stripping Voltammetry of Zinc

    Science.gov (United States)

    Kang, Wenjing; Pei, Xing; Yue, Wei; Bange, Adam; Heineman, William R.; Papautsky, Ian

    2013-01-01

    In this work, we report on the development of a lab-on-a-chip electrochemical sensor that uses an evaporated bismuth electrode to detect zinc using square wave anodic stripping voltammetry. The microscale electrochemical cell consists of a bismuth working electrode, an integrated silver/silver chloride reference electrode, and a gold auxiliary electrode. The sensor demonstrated linear response in 0.1 M acetate buffer at pH 6 with zinc concentrations ranging from 1 μM to 30 μM and a calculated detection limit of 60 nM. The sensor was also able to successfully detect zinc in a bovine serum extract and the results were verified with independent AAS measurements. These results demonstrate the advantageous qualities of this lab-on-a-chip electrochemical sensor for clinical applications, which include a small sample volume (μL scale), reduced cost, short response time and high accuracy at low concentrations of analyte. PMID:24436575

  1. Square-wave stripping voltammetry for direct determination of eight heavy metals in soil and indoor-airborne particulate matter.

    Science.gov (United States)

    Farghaly, Othman A; Ghandour, M A

    2005-03-01

    The application of square-wave voltammetry (SWV) for the determination of eight elements viz. Cd(II), Pb(II), Cu(II), Zn(II), Co(II), Ni(II), Cr(VI), and Mo(VI) in soil and indoor-airborne particulate matter has been examined and optimized. The cathodic and anodic types of the SWV technique were examined for the detection of these metal ions. It was found that the square-wave anodic stripping voltammetry is the conventional technique for the determination of Zn(II), Cd(II), Pb(II), and Cu(II), but square-wave adsorptive cathodic stripping voltammetric method is used for the determination of Co(II), Ni(II), Mo(VI) and Cr(VI). Various experimental parameters, which influenced the response of the mercury film electrode to these metal ions, were optimized. The detection limits of these metal ions were 0.03, 0.4, 0.04, 0.1, 0.15, 0.05, 0.2, and 3.2 microg/kg for Cd(II), Pb(II), Cu(II), Zn(II), Co(II), Ni(II), Cr(VI), and Mo(VI), respectively, with very good accuracy (standard deviation is below 2%). Interference from coexisting ions was successfully investigated. A comparison of analytical data for analyzing real samples was carried out between the SWV method and the graphite furnace atomic absorption spectrophotometric (GFAAS) method. By the standard addition method, the recoveries were 96.6-104% with SD of 0.75-2.5%. The great advantage of SWV is the simplicity, selectivity, sensitivity, and shortening analysis time over the GFAAS method.

  2. Linear sweep anodic stripping voltammetry: Determination of Chromium (VI) using synthesized gold nanoparticles modified screen-printed electrode

    Indian Academy of Sciences (India)

    Salamatu Aliyu Tukur; Nor Azah Yusof; Reza Hajian

    2015-06-01

    A highly sensitive electrochemical sensor has been constructed for determination of Cr(VI) with the lowest limit of detection (LOD) reported to date using gold nanoparticles (AuNPs) modified screen-printed electrode (SPE). The modification of SPE by casting pure AuNPs increases the sensitivity for detection of Cr(VI) ion using anodic stripping voltammetry. Cr(VI) ions are reduced to chromium metal on SPE-AuNPs by applying deposition potential of –1.1 V for 180 s. Afterwards, the oxidation peak current of chromium is obtained by linear sweep voltammetry in the range of −1.0 V to 0.2 V. Under the optimized conditions (HClO4, 0.06 mol L−1; deposition potential, –1.1 V; deposition time, 180s; scan rate, 0.1 V s−1), the limit of detection (LOD) was 1.6 pg mL−1. The fabricated electrode was successfully used for detection of Cr(VI) in tap and seawater.

  3. Determination of ultra trace amount of enrofloxacin by adsorptive cathodic stripping voltammetry using copper(II) as an intermediate.

    Science.gov (United States)

    Ensaifi, Ali A; Khayamian, T; Taei, M

    2009-05-15

    In this work, a simple and sensitive electroanalytical method was developed for the determination of enrofloxacin (ENRO) by adsorptive cathodic stripping voltammetry (ADSV) using Cu(II) as a suitable probe. The complex of copper(II) with ENRO was accumulated at the surface of a hanging mercury drop electrode at -0.10 V for 40 s. Then, the preconcentrated complex was reduced and the peak current was measured using square wave voltammetry (SWV). The optimization of experimental variables was conducted by experimental design and support vector machine (SVM) modeling. The model was used to find optimized values for the factors such as pH, Cu(II) concentration and accumulation potential. Under the optimized conditions, the peak current at -0.30 V is proportional to the concentration of ENRO over the range of 10.0-80.0 nmol L(-1) with a detection limit of 0.33 nmol L(-1). The influence of potential interfering substances on the determination of ENRO was examined. The method was successfully applied to determination of ENRO in plasma and pharmaceutical samples.

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

    Science.gov (United States)

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

    2014-10-01

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

  5. Determination of bosentan in pharmaceutical preparations by linear sweep, square wave and differential pulse voltammetry methods.

    Science.gov (United States)

    Atila, Alptug; Yilmaz, Bilal

    2015-01-01

    In this study, simple, fast and reliable cyclic voltammetry (CV), linear sweep voltammetry (LSV), square wave voltammetry (SWV) and differential pulse voltammetry (DPV) methods were developed and validated for determination of bosentan in pharmaceutical preparations. The proposed methods were based on electrochemical oxidation of bosentan at platinum electrode in acetonitrile solution containing 0.1 M TBACIO4. The well-defined oxidation peak was observed at 1.21 V. The calibration curves were linear for bosentan at the concentration range of 5-40 µg/mL for LSV and 5-35 µg/mL for SWV and DPV methods, respectively. Intra- and inter-day precision values for bosentan were less than 4.92, and accuracy (relative error) was better than 6.29%. The mean recovery of bosentan was 100.7% for pharmaceutical preparations. No interference was found from two tablet excipients at the selected assay conditions. Developed methods in this study are accurate, precise and can be easily applied to Tracleer and Diamond tablets as pharmaceutical preparation.

  6. Adsorption of pyrantel pamoate on mercury from aqueous solutions: studies by stripping voltammetry.

    Science.gov (United States)

    Gupta, Vinod K; Jain, Rajeev; Jadon, N; Radhapyari, K

    2010-10-01

    Adsorption and electrochemical reduction of pyrantel pamoate are studied in Britton Robinson buffer medium at hanging mercury drop electrode (HMDE) by Adsorptive Stripping Voltammetric technique. The peak current shows a linear dependence with the drug concentration over the range 250 ng mL(-1) to 64 microg mL(-1). Applicability to assay the drug in urine samples is illustrated in the concentration range 5-20 microg mL(-1).

  7. Determination of cobalt and nickel in biological materials using catalytic adsorptive stripping voltammetry

    OpenAIRE

    Bobrowski, Andrzej; Zarębski, Jerzy; Królicka, Agnieszka

    2012-01-01

    The paper discusses the utilisation of the catalytic adsorptive stripping voltammetric method for the simultaneous determination of Co and Ni in biological materials such as hair, oyster tissue, bovine liver and oriental tobacco leaves. For this purpose the most sensitive and selective catalytic-adsorptive system with nioxime and nitrite has been selected. The optimal parameters, including concentration of the supporting electrolyte, pH and accumulation time and potential, have be...

  8. Determination of vanillin in commercial food product by adsorptive stripping voltammetry using a boron-doped diamond electrode.

    Science.gov (United States)

    Yardım, Yavuz; Gülcan, Mehmet; Şentürk, Zühre

    2013-12-01

    A method for the determination of food additive vanillin was developed by adsorptive stripping voltammetry. Its determination was carried out at the anodically pre-treated boron-doped diamond electrode in aqueous solutions. Using square-wave stripping mode, the compound yielded a well-defined voltammetric response in phosphate buffer, pH 2.5 at +1.14 V (vs. Ag/AgCl) (a pre-concentration step being carried out at open-circuit condition for 60s). A linear calibration graph was obtained in the concentration range of 0.5-15.0 μg mL(-1) (3.3×10(-6)-9.8×10(-5) mol L(-1)) with a detection limit of 0.024 μg mL(-1) (1.6×10(-7) mol L(-1)). As an example, the practical applicability of the proposed method was tested for the determination of this flavouring agent in commercial pudding powder of Keshkule (Turkish milk pudding with almond flour).

  9. Nanocomposite electrodes made of carbon nanofibers and black wax. Anodic stripping voltammetry of zinc and lead.

    Science.gov (United States)

    van Dijk, N; Fletcher, S; Madden, C E; Marken, F

    2001-11-01

    Nanocomposite electrodes offer exciting new possibilities in electroanalytical chemistry. In this preliminary study, nanocomposite electrodes made of carbon nanofibers and black wax were characterized and investigated as novel substrates for metal deposition and stripping processes. Carbon nanofibers were grown from ethylene-hydrogen gas mixtures over Fe-Ni-Cu (85:10:5) nanoparticle catalysts at 600 degrees C and then embedded in Apiezon black wax under vacuum at 140 degrees C. The resulting nanocomposite electrodes showed (i) good conductivity, (ii) a wide potential window in aqueous solutions, (iii) low background currents, (iv) near steady state voltammetric responses with substantial Faradaic currents and (v) sharply peaked fast scan metal stripping responses. Zinc is a notoriously difficult metal to determine in aqueous solutions, because its deposition and stripping are accompanied by hydrogen evolution at extreme negative potentials. It therefore provided a challenging test for our new nanocomposite electrode. Although numerous complications associated with the hydrogen evolution process could not be eliminated, remarkably clear voltammograms could be obtained even at scan rates of 40 V s(-1).

  10. Cyclopentanone thiosemicarbazone, a new complexing agent for copper determination in biological samples by adsorptive stripping voltammetry.

    Science.gov (United States)

    Mahajan, Rakesh Kumar; Walia, T P S; Sumanjit; Lobana, T S

    2006-03-01

    A selective and sensitive stripping voltammetric method for the determination of trace amounts of copper(II) with cyclopentanone thiosemicarbazone (CPTSC) is presented. The method is based on the adsorptive accumulation of the resulting copper-CPTSC complex on a hanging mercury drop electrode, followed by the stripping voltammetric measurements at the reduction current of the adsorbed complex at -0.37 V vs. Ag/AgCl. The optimal conditions for the stripping analysis of copper include pH 9.3, deposition time of 120 s, and a deposition potential of -0.1 V (vs. Ag/AgCl). The peak current is linearly proportional to the copper concentration over a range 3.14 x 10(-9) M to 1.57 x 10(-6) M with a limit of detection of 1.57 x 10(-9) M. The technique has been applied to the determination of copper in biological samples, like urine and whole blood.

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

    Science.gov (United States)

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

    2011-09-09

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

  12. Simple and rapid determination of trace iodide by cathodic stripping voltammetry.

    Science.gov (United States)

    Yang, Lingxi; Zou, Lina; Li, Gaiping; Ye, Baoxian

    2016-01-15

    This work establishes a highly sensitive and simple stripping voltammetric method for the direct determination of trace iodide. In the presence of abounding bromide and appropriate amount of cetylpyridine bromide (CPB), the iodine was accumulated on the glassy carbon electrode surface as ion association complex (CPBI2Br). After accumulation for a period of time, a linear sweep potential with negative scanning was applied and the I2 in CPBI2Br was reduced again into the solution. Under the optimization conditions, the stripping signals (peak current) were linear relationship with iodide concentration in range of 3.81×10(-3)µg/mL to 0.114 μg/mL and 0.127μg/mL to 2.54μg/mL, with a detection limit of 1.02ng/mL (S/N=3) for a accumulation time of 180s. Determination of trace iodine in pharmaceutical sample, kelp and table salt were performed with high accuracy and satisfactory recovery results. Copyright © 2015 Elsevier B.V. All rights reserved.

  13. Square wave adsorptive cathodic stripping voltammetry automated by sequential injection analysis Potentialities and limitations exemplified by the determination of methyl parathion in water samples.

    Science.gov (United States)

    dos Santos, Luciana B O; Masini, Jorge C

    2008-01-14

    This paper describes the development and evaluation of a sequential injection method to automate the determination of methyl parathion by square wave adsorptive cathodic stripping voltammetry exploiting the concept of monosegmented flow analysis to perform in-line sample conditioning and standard addition. Accumulation and stripping steps are made in the sample medium conditioned with 40 mmolL(-1) Britton-Robinson buffer (pH 10) in 0.25 molL(-1) NaNO3. The homogenized mixture is injected at a flow rate of 10 microLs(-1) toward the flow cell, which is adapted to the capillary of a hanging drop mercury electrode. After a suitable deposition time, the flow is stopped and the potential is scanned from -0.3 to -1.0V versus Ag/AgCl at frequency of 250 Hz and pulse height of 25 mV. The linear dynamic range is observed for methyl parathion concentrations between 0.010 and 0.50 mgL(-1), with detection and quantification limits of 2 and 7 microgL(-1), respectively. The sampling throughput is 25 h(-1) if the in line standard addition and sample conditioning protocols are followed, but this frequency can be increased up to 61 h(-1) if the sample is conditioned off-line and quantified using an external calibration curve. The method was applied for determination of methyl parathion in spiked water samples and the accuracy was evaluated either by comparison to high performance liquid chromatography with UV detection, or by the recovery percentages. Although no evidences of statistically significant differences were observed between the expected and obtained concentrations, because of the susceptibility of the method to interference by other pesticides (e.g., parathion, dichlorvos) and natural organic matter (e.g., fulvic and humic acids), isolation of the analyte may be required when more complex sample matrices are encountered.

  14. Trace vanadium analysis by catalytic adsorptive stripping voltammetry using mercury-coated micro-wire and polystyrene-coated bismuth film electrodes

    Energy Technology Data Exchange (ETDEWEB)

    Dansby-Sparks, Royce; Chambers, James Q. [Department of Chemistry, University of Tennessee, Knoxville, TN 37996-1600 (United States); Xue Ziling, E-mail: xue@ion.chem.utk.edu [Department of Chemistry, University of Tennessee, Knoxville, TN 37996-1600 (United States)

    2009-06-08

    An electrochemical technique has been developed for ultra-trace (ng L{sup -1}) vanadium (V) measurement. Catalytic adsorptive stripping voltammetry for V analysis was developed at mercury-coated gold micro-wire electrodes (MWEs, 100 {mu}m) in the presence of gallic acid (GA) and bromate ion. A potential of -0.275 V (vs Ag/AgCl) was used to accumulate the complex in acetate buffer (pH 5.0) at the electrode surface followed by a differential pulse voltammetric scan. Parameters affecting the electrochemical response, including pH, concentration of GA and bromate, deposition potential and time have been optimized. Linear response was obtained in the 0-1000 ng L{sup -1} range (2 min deposition), with a detection limit of 0.88 ng L{sup -1}. The method was validated by comparison of results for an unknown solution of V by atomic absorption measurement. The protocol was evaluated in a real sample by measuring the amount of V in river water samples. Thick bismuth film electrodes with protective polystyrene films have also been made and evaluated as a mercury free alternative. However, ng L{sup -1} level detection was only attainable with extended (10 min) deposition times. The proposed use of MWEs for the detection of V is sensitive enough for future use to test V concentration in biological fluids treated by the advanced oxidation process (AOP).

  15. Trace vanadium analysis by catalytic adsorptive stripping voltammetry using mercury-coated micro-wire and polystyrene-coated bismuth film electrodes.

    Science.gov (United States)

    Dansby-Sparks, Royce; Chambers, James Q; Xue, Zi-Ling

    2009-06-08

    An electrochemical technique has been developed for ultra-trace (ng L(-1)) vanadium (V) measurement. Catalytic adsorptive stripping voltammetry for V analysis was developed at mercury-coated gold micro-wire electrodes (MWEs, 100 microm) in the presence of gallic acid (GA) and bromate ion. A potential of -0.275 V (vs Ag/AgCl) was used to accumulate the complex in acetate buffer (pH 5.0) at the electrode surface followed by a differential pulse voltammetric scan. Parameters affecting the electrochemical response, including pH, concentration of GA and bromate, deposition potential and time have been optimized. Linear response was obtained in the 0-1000 ng L(-1) range (2 min deposition), with a detection limit of 0.88 ng L(-1). The method was validated by comparison of results for an unknown solution of V by atomic absorption measurement. The protocol was evaluated in a real sample by measuring the amount of V in river water samples. Thick bismuth film electrodes with protective polystyrene films have also been made and evaluated as a mercury free alternative. However, ng L(-1) level detection was only attainable with extended (10 min) deposition times. The proposed use of MWEs for the detection of V is sensitive enough for future use to test V concentration in biological fluids treated by the advanced oxidation process (AOP).

  16. Determination of iodide and total iodine in estuarine waters by cathodic stripping voltammetry using a vibrating silver amalgam microwire electrode.

    Science.gov (United States)

    Espada-Bellido, Estrella; Bi, Zhaoshun; Salaün, Pascal; van den Berg, Constant M G

    2017-11-01

    Iodide in natural waters is an important nutrient to aquatic organisms and its determination is of relevance to marine aquaculture. For this reason it is of interest to have a simple analytical method for determination of iodide in water samples. Iodide in seawater can be determined electrochemically by cathodic stripping voltammetry (CSV) with a mercury drop electrode which has environmental drawbacks. In an attempt to minimise the use of mercury in voltammetry, a vibrating silver amalgam microwire electrode is used here for the determination by CSV of iodide speciation in natural waters including seawater. Microwire electrodes were made from silver wires (diameter: 12.5µm) and electrochemically coated with mercury. The electrode surface was stable for extended periods of analyses (at least one week) and was then replaced. The optimised conditions include a pH 8, a frequency of 500Hz and a deposition time of 60s, among others. The microwire was reactivated between scans using a conditioning potential at -3 V for 1s. The detection limit for iodide in seawater was found to be 0.7nM I(-) at a deposition time of 60s. The response increased linearly with the concentration of iodide in seawater up to 100nM I(-). The method was successfully applied to various samples from the estuary of the river Mersey (Liverpool Bay). An existing procedure for iodine speciation was modified to enable determination of iodate and total iodine as well as iodide in estuarine waters. Copyright © 2017 Elsevier B.V. All rights reserved.

  17. Determination of tryptophan and histidine by adsorptive cathodic stripping voltammetry using H-point standard addition method.

    Science.gov (United States)

    Ensafi, Ali A; Hajian, R

    2006-11-24

    A sequential method is proposed for the determination of tryptophane and histidine by adsorptive cathodic stripping voltammetry using standard addition and H-point standard addition method (HPSAM). The complexes of copper(II) with the amino acids were accumulated onto the surface of a hanging mercury drop electrode for 60s. Then the preconcentrated complexes were reduced by square wave voltammetry and the peak currents were measured. The effect of various parameters such as pH, concentration of copper, accumulation potential, accumulation time and scan rate on the sensitivity were studied by one-at-a time and artificial neural network. Under the optimized conditions, the peak currents at about +0.05 to -0.30 V is proportional to the concentration of tryptophan and histidine over the concentration ranges of 5-220 and 100-1200 nM, respectively. Optimization of the parameters by one-at-a time showed that at accumulation potential of 0.10 V (versus Ag/AgCl reference electrode) the peak current is proportional only to the concentration of tryptophan and histidine does not have any contribution to the current. The optimization results by artificial neural network showed that at accumulation potential of -0.06 V (versus Ag/AgCl) the peak current is proportional to the both concentrations of tryptophan and histidine. Therefore, the method of H-point standard addition has been used for resolving overlap voltamograms for determination of histidine in the present of tryptophane. The method was successfully applied to the determination of tryptophan and histidine in synthetic and real samples.

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

    Energy Technology Data Exchange (ETDEWEB)

    Guerreiro, Gabriela V.; Zaitouna, Anita J.; Lai, Rebecca Y., E-mail: rlai2@unl.edu

    2014-01-31

    Graphical abstract: -- Highlights: •An electrochemical Hg(II) sensor based on T–Hg(II)–T sensing motif was fabricated. •A methylene blue-modified DNA probe was used to fabricate the sensor. •Sensor performance was evaluated using ACV, CV, SWV, and DPV. •The sensor behaves as a “signal-off” sensor in ACV and CV. •The sensor behaves as either a “signal-on” or “signal-off” sensor in SWV and DPV. -- Abstract: Here we report the characterization of an electrochemical mercury (Hg{sup 2+}) sensor constructed with a methylene blue (MB)-modified and thymine-containing linear DNA probe. Similar to the linear probe electrochemical DNA sensor, the resultant sensor behaved as a “signal-off” sensor in alternating current voltammetry and cyclic voltammetry. However, depending on the applied frequency or pulse width, the sensor can behave as either a “signal-off” or “signal-on” sensor in square wave voltammetry (SWV) and differential pulse voltammetry (DPV). In SWV, the sensor showed “signal-on” behavior at low frequencies and “signal-off” behavior at high frequencies. In DPV, the sensor showed “signal-off” behavior at short pulse widths and “signal-on” behavior at long pulse widths. Independent of the sensor interrogation technique, the limit of detection was found to be 10 nM, with a linear dynamic range between 10 nM and 500 nM. In addition, the sensor responded to Hg{sup 2+} rather rapidly; majority of the signal change occurred in <20 min. Overall, the sensor retains all the characteristics of this class of sensors; it is reagentless, reusable, sensitive, specific and selective. This study also highlights the feasibility of using a MB-modified probe for real-time sensing of Hg{sup 2+}, which has not been previously reported. More importantly, the observed “switching” behavior in SWV and DPV is potentially generalizable and should be applicable to most sensors in this class of dynamics-based electrochemical biosensors.

  19. Pulse radiolysis and cyclic voltammetry studies of redox properties of phenothiazine radicals

    Energy Technology Data Exchange (ETDEWEB)

    Madej, Edyta [Gray Cancer Institute, PO Box 100, Mount Vernon Hospital, Northwood, Middlesex HA6 2JR (United Kingdom)]. E-mail: madej@gci.ac.uk; Wardman, Peter [Gray Cancer Institute, PO Box 100, Mount Vernon Hospital, Northwood, Middlesex HA6 2JR (United Kingdom)

    2006-09-15

    One-electron transfer equilibria between seven phenothiazines were characterized by pulse radiolysis, producing radical-cations via oxidation by Br{sub 2} {sup .-} or (SCN){sub 2} {sup .-} radicals. The reduction potentials of the phenothiazine radicals were determined by cyclic voltammetry. As an independent check, the redox equilibrium between one phenothiazine and the redox indicator ABTS was investigated. The data establish phenothiazines as useful indicators for radical redox properties. However, there are potential problems of aggregation, additional reactions with Br{sup -}/Br{sub 2} {sup .-} and reactivity of the radicals towards buffers or other nucleophiles.

  20. Compositional analysis of electrodeposited bismuth telluride thermoelectric thin films using combined electrochemical quartz crystal microgravimetry--stripping voltammetry.

    Science.gov (United States)

    Ham, Sunyoung; Jeon, Soyeon; Lee, Ungki; Park, Minsoon; Paeng, Ki-Jung; Myung, Noseung; Rajeshwar, Krishnan

    2008-09-01

    Bismuth telluride (Bi 2Te 3 ) is a benchmark material for thermoelectric power generation and cooling applications. Electrodeposition is a versatile technique for preparing thin films of this material; however, it affords films of variable composition depending on the preparation history. A simple and rapid assay of electrodeposited films, therefore, has both fundamental and practical importance. In this study, a new protocol for the electroanalysis of Bi 2Te 3 thin films is presented by combining the two powerful and complementary techniques of electrochemical quartz crystal microgravimetry (EQCM) and stripping voltammetry. First, any free (and excess) tellurium in the electrodeposited film was reduced to soluble Te ( 2- ) species by scanning to negative potentials in a 0.1 M Na 2SO 4 electrolyte, and the accompanying frequency increase (mass loss) was used to determine the content of free tellurium. The film was again subjected to cathodic stripping in the same medium (to generate Bi (0) and soluble Te (2-) from the Bi 2 Te 3 film component of interest), and the EQCM frequency change was used to determine the content of chemically bound Te in the Bi 2Te 3 thin film and thereby the compound stoichiometry. Finally, the EQCM frequency change during Bi oxidation to Bi (3+) and the difference between total Bi and Bi in Bi 2Te 3 resulted in the assay of free (excess) Bi in the electrodeposited film. Problems associated with the chemical/electrochemical stability of the free Bi species were circumvented by a flow electroanalysis approach. Data are also presented on the sensitivity of electrodeposited Bi 2Te 3 film composition to the electrodeposition potential. This newly developed method can be used for the compositional analysis of other thermoelectric thin-film material candidates in general.

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

    Science.gov (United States)

    Jiang, Chuanjia; Hsu-Kim, Heileen

    2014-11-01

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

  2. Determination of Se(IV) in natural waters by adsorptive stripping voltammetry of 5-nitropiazselenol.

    Science.gov (United States)

    Ashournia, Mehdi; Aliakbar, Alireza

    2010-02-15

    The high tendency of 5-nitropiazselenol for self-accumulation on thin mercury film electrode was used innovatively for determination of Se(IV) in natural waters. 5-Nitropiazselenol was formed by reaction between Se(IV) and 4-nitro-1,2-phenylenediamine in acidic solution and self-accumulation process was carried out directly from reaction media. The adsorbed 5-nitropiazselenol was stripped in HCl solution by DP cathodic potential scan. All parameters influencing the measurement were optimized and evaluated. Detection limit of this method is 0.06 ng mL(-1). Interferences of various cations and anions were studied. The adsorption tendency of some other piazselenols made by some aromatic ortho-diamines was also investigated. The problems arising from applying potential during accumulation process in natural waters analysis were discussed. This method was applied for determination of Se(IV) in natural waters collected from some internationally registrated lagoons south of Caspian Sea. The obtained results were compared with the results of ICP-AES and DPCSV after electrochemical preconcentration.

  3. Flow electrochemical analyses of zinc by stripping voltammetry on graphite felt electrode.

    Science.gov (United States)

    Feier, B; Floner, D; Cristea, C; Bodoki, E; Sandulescu, R; Geneste, F

    2012-08-30

    A flow sensor for trace analysis of zinc, using graphite felt as working electrode is reported here. A flow cell, well-adapted to 3-D porous electrodes and capable to do both the preconcentration step at a cathodic potential and the stripping of the zinc was successfully developed. It was demonstrated that this cell allows to obtain better electrochemical signals for Zn(2+) compared to a standard three-electrodes cell and that the percolation during accumulation increases the kinetics of electrodeposition. The influence on Zn(2+) signal of the deposition potential, the time of deposition and the flow rate was studied. The resulting sensor shows a linear response towards Zn(2+) with a linear range of 10(-6)-10(-4)M and a limit of detection of 5×10(-7) M for an analysis time of 5 min. The interferences study showed that the Cr(3+), Pb(2+), Cd(2+) ions have a small effect on the Zn electrochemical signal, whereas Fe(3+), Cu(2+), Co(2+) and Ni(2+) ions strongly influence it. The electrode was tested on real samples (tap water spiked with Zn(2+), food supplement) with a good recovery by applying the standard addition method. Copyright © 2012 Elsevier B.V. All rights reserved.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2011-09-09

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

  5. Adsorptive stripping voltammetry of nickel with 1-nitroso-2-napthol using a bismuth film electrode.

    Science.gov (United States)

    Segura, Rodrigo; Pradena, Milenco; Pinto, Deny; Godoy, Fernando; Nagles, Edgar; Arancibia, Verónica

    2011-10-15

    A sensitive procedure is presented for the voltammetric determination of nickel. The procedure involves an adsorptive accumulation of nickel 1-nitroso-2-napthol (NN) complex on a bismuth film electrode prepared ex situ by electrodeposition. The most suitable operating conditions and parameters such as pH, ligand concentration (C(NN)), adsorptive potential (E(ads)), adsorptive time (t(ads)), scan rate and others were selected and the determination of nickel in aqueous solutions using the standard addition method was possible. The adsorbed Ni-NN complex gives a well defined cathodic stripping peak current at -0.70 V, which was used for the determination of nickel in the concentration range of 10.0-70.0 μg L(-1) (pH 7.5; C(NN) 6.5 μmol L(-1); E(ads) -0.30 V; t(ads) 60s) with a detection limit of 0.1 μg L(-1). The relative standard deviation for a solution containing 10.0 μg L(-1) of Ni(II) was 3.5% (n=4). The proposed method was validated determining Ni(II) in certified reference waste water (SPS-WW1) and Certified Reference Water for Trace Elements (TMDA 51.3) with satisfactory results. Then lake water samples were analyzed. Copyright © 2011. Published by Elsevier B.V.

  6. Trace metal characterization and speciation in geothermal effluent by multiple scanning anodic stripping voltammetry and atomic absorption analysis

    Energy Technology Data Exchange (ETDEWEB)

    Kowalski, B.R.

    1979-05-25

    Recent studies have shown geothermal power plants to have a significant environmental impact on the ground water of the area. The heavy metals arsenic and mercury are special problems, as both are concentrated by flora and fauna exposed to the effluent waters. Because the toxicity of these and other metallic pollutants present in geothermal effluent depends on the chemical form, or speciation, of the particular metal, any serious study of the environmental impact of a geothermal development should include studies of trace metal speciation, in addition to trace metal concentration. This proposal details a method for determining metal speciation in dilute waters. The method is based on ion-exchange and backed by atomic absorption spectrometry and multiple scanning anodic stripping voltammetry. Special laboratory studies will be performed on mercury, arsenic and selenium speciation in synthetic geothermal water. The method will be applied to three known geothermal areas in Washington and Oregon, with emphasis on the speciation of mercury, arsenic and selenium in these waters. The computer controlled electrochemical instrumentation was built and tested. Using this instrumentation, a new experimental procedure was developed to determine the chemical form (speciation) of metal ions in very dilute solutions (ng/ml). This method was tested on model systems including Pb, Cd, and As with C1/sup -/, CO/sub 3//sup 2 -/ and glycine ligands. Finally, the speciation of lead in a geothermal water was examined and the PbC1/sup +/ complex was observed and quantified.

  7. Preparation and Evaluation of Acetabularia-Modified Carbon Paste Electrode in Anodic Stripping Voltammetry of Copper and Lead Ions

    Directory of Open Access Journals (Sweden)

    Muhammad Raziq Rahimi Kooh

    2013-01-01

    Full Text Available Seaweed is well known about for potential in chelating heavy metals. In this study, carbon paste electrodes were fabricated with siphonous seaweed Acetabularia acetabulum as the modifiers to sense lead (II and copper (II by square-wave anodic stripping voltammetry. Various scan rates and deposition potentials were measured to obtain the optimal peak current for Pb(II and Cu(II. Optimum conditions of Acetabularia-CPE for sensing Pb(II were at the scan rate of 75 mV/s and deposition potential of −800 mV, while for Cu(II sensing were at 100 mV/s and −300 mV, respectively. The electrodes were characterized by the duration of accumulation time, preconcentration over a range of standards, supporting electrolyte, and standard solutions of various pH values. Interference studies were carried out. Both Zn(II and Cu(II were found to interfere with Pb(II sensing, whereas only Zn(II causes interference with Cu(II sensing. The electrode was found to have good regeneration ability via electrochemical cleaning. Preliminary testing of complex samples such as NPK fertilisers, black soil, and sea salt samples was included.

  8. Redox magnetohydrodynamic enhancement of stripping voltammetry: toward portable analysis using disposable electrodes, permanent magnets, and small volumes.

    Science.gov (United States)

    Weston, Melissa C; Anderson, Emily C; Arumugam, Prabhu U; Narasimhan, Padhmodhbhava Yoga; Fritsch, Ingrid

    2006-12-01

    The use of redox magnetohydrodynamics (MHD) to enhance the anodic stripping voltammetry (ASV) response of heavy metals has been investigated, with respect to achieving portability: disposable electrodes consisting of screen-printed carbon (SPC) on a low temperature co-fired ceramic (LTCC) substrate, small volumes, and permanent magnets. The analytes tested (Cd(2+), Cu(2+), and Pb(2+)) were codeposited on SPC with Hg(2+) to form a Hg thin film electrode. High concentrations of Fe(3+) were used to produce a high cathodic current which generates a significant Lorentz force in the presence of a magnetic field. This Lorentz force induces solution convection during the deposition step, enhancing the mass transport of analytes to the electrode and increasing their preconcentrated quantity in the mercury thin film. Therefore, larger ASV peaks and improved sensitivities are obtained, compared to analyses performed without a magnet. The effects on ASV signal of varying Hg(2+) concentration (0.10 and 1.0 mM), deposition time (10-600 s), and electrode surface roughness were investigated. In addition, analyses were performed using a real lake water matrix. By using the disposable LTCC-SPC working electrodes in small volumes (150 microL) and with small permanent magnets (0.78 T), peak areas were increased by 75% when compared to the signal obtained in the absence of a magnetic field. A limit of detection of 25 nM for Cd(2+) was observed with only a 1 min preconcentration time.

  9. Simultaneous determination of trace uranium(VI) and zinc(II) by adsorptive cathodic stripping voltammetry with aluminon ligand.

    Science.gov (United States)

    Cha, K W; Park, C I; Park, S H

    2000-09-05

    Uranium(VI) complexed with aluminon (3-[bis(3-carboxy-4-hydroxy-phenyl)methylene]-6-oxo-1,4-cyclohexadiene-1-carboxylic acid triammonium salt) was determined by adsorptive cathodic stripping voltammetry (ACSV) using a hanging mercury drop electrode. Trace uranium(VI) and zinc(II) can be simultaneously determined in a single scan in the presence of aluminon and urea. Optimal conditions were found to be: accumulation time; 180-200 s, accumulation potential; 50 mV versus Ag/AgCl, scan rate; 40 mV s(-1), supporting electrolyte; 0.1 M sodium acetate buffer at pH 6.5-7.0, and concentration of aluminon; 1x10(-6) M. The linear range of uranium(VI) and zinc(II) were observed over the concentration range 2-33 and 30-120 ng ml(-1), respectively. The detection limit (S/N=3) are 0.2 ng ml(-1) (uranium) and 30 ng ml(-1) (zinc). A good reproducibility shows RSDs of 2.5-4.0% (n=10). The procedure offers high selectivity, with the presence of urea masking some metal ions.

  10. A study of the determination of the hypertensive drug captopril by square wave cathodic adsorptive stripping voltammetry.

    Science.gov (United States)

    Ioannides, X; Economou, A; Voulgaropoulos, A

    2003-09-19

    In this work, the determination of captopril (CPL) was studied by square wave cathodic adsorptive stripping voltammetry (SWCAdSV) on a hanging mercury drop electrode (HMDE). CPL was adsorptively preconcentrated on the mercury surface as a sparingly soluble mercury salt under stirring of the solution and then the accumulated species was reduced by a cathodic square wave voltammetric scan. The reduction current was related to the CPL concentration in the sample. The chemical and instrumental parameters affecting the response were investigated and optimized for the CPL determination. The calibration curve was linear from 0.5 to 180 microg l(-1) of CPL (depending on the preconcentration time), the limit of detection at a S/N ratio of 3 was 0.5 microg l(-1) with 300 s of preconcentration and the relative standard deviation was 3.2% at the 20 microg l(-1) level (with 120 s of preconcentration, n=8). The method was applied to the determination of CPL in two pharmaceutical formulations with recoveries of 97.9 and 98.8%. Finally, the potential for applying the proposed method to the determination of CPL in biological media is briefly discussed.

  11. Unprecedented stable aqueous semiquinone methide radical formation interferes with adsorptive cathodic stripping voltammetry of cobalt methyl thymol blue.

    Science.gov (United States)

    Niztayev, Alidin N; Hagen, Wilfred R

    2005-09-15

    A putatively highly sensitive and selective method for the determination of cobalt in aqueous samples by catalytic adsorptive cathodic stripping voltammetry using methyl thymol blue (MTB) as the ligand has been documented [A. Safavi, E. Shams, Talanta 51 (2000) 1117] and its underlying mechanism has been briefly explored [A. Safavi, E. Shams, Electroanalysis 14 (2002) 708]. In an attempt to adapt the method for application in metalloprotein analysis we obtained erratic results, which were traced down to the redox non-innocence of the free ligand in the potential range prescribed for the metal analysis. On the hanging mercury drop electrode free methyl thymol blue is reversibly one-electron reduced to the semiquinone form with E(m,7.0)=-482mV versus NHE at 22 degrees C, and the radical is subsequently quasi-reversibly one-electron reduced to the quinol form with E(m,7) approximately -0.9V. This observation invalidates the use of MTB in electrochemical analysis of metal ions. This is also the first observation ever of a stable quinone methide radical in aqueous solution.

  12. Direct determination of cadmium and lead in pharmaceutical ingredients using anodic stripping voltammetry in aqueous and DMSO/water solutions.

    Science.gov (United States)

    Rosolina, Samuel M; Chambers, James Q; Lee, Carlos W; Xue, Zi-Ling

    2015-09-17

    A new electrochemical method has been developed to detect and quantify the elemental impurities, cadmium(II) (Cd(2+)) and lead(II) (Pb(2+)), either simultaneously or individually in pharmaceutical matrices. The electro-analytical approach, involving the use of anodic stripping voltammetry (ASV) on an unmodified glassy carbon electrode, was performed in both aqueous and in a 95/5 dimethyl sulfoxide (DMSO)/water solutions, without acid digestion or dry ashing to remove organic matrices. Limits of detection (LODs) in the μg L(-1) [or parts per billion (ppb), mass/volume] range were obtained for both heavy metals - in the presence and absence of representative pharmaceutical components. To the best of our knowledge, the work demonstrates the first analysis of heavy metals in DMSO/water solutions through ASV. The strong reproducibility and stability of the sensing platform, as well as obviation of sample pretreatment show the promise of utilizing ASV as a sensitive, robust, and inexpensive alternative to inductively-coupled-plasma (ICP)-based approaches for the analysis of elemental impurities in, e.g., pharmaceutical-related matrices.

  13. Glyphosate detection with ammonium nitrate and humic acids as potential interfering substances by pulsed voltammetry technique.

    Science.gov (United States)

    Martínez Gil, Pablo; Laguarda-Miro, Nicolas; Camino, Juan Soto; Peris, Rafael Masot

    2013-10-15

    Pulsed voltammetry has been used to detect and quantify glyphosate on buffered water in presence of ammonium nitrate and humic substances. Glyphosate is the most widely used herbicide active ingredient in the world. It is a non-selective broad spectrum herbicide but some of its health and environmental effects are still being discussed. Nowadays, glyphosate pollution in water is being monitored but quantification techniques are slow and expensive. Glyphosate wastes are often detected in countryside water bodies where organic substances and fertilizers (commonly based on ammonium nitrate) may also be present. Glyphosate also forms complexes with humic acids so these compounds have also been taken into consideration. The objective of this research is to study the interference of these common pollutants in glyphosate measurements by pulsed voltammetry. The statistical treatment of the voltammetric data obtained lets us discriminate glyphosate from the other studied compounds and a mathematical model has been built to quantify glyphosate concentrations in a buffer despite the presence of humic substances and ammonium nitrate. In this model, the coefficient of determination (R(2)) is 0.977 and the RMSEP value is 2.96 × 10(-5) so the model is considered statistically valid.

  14. Assay of dipyridamole in human serum using cathodic adsorptive square-wave stripping voltammetry.

    Science.gov (United States)

    Ghoneim, M M; Tawfik, A; Radi, A

    2002-09-01

    A rapid and sensitive square-wave voltammetric procedure was optimized for the determination of dipyridamole after its adsorption preconcentration onto a hanging mercury drop electrode. The peak current of the first of the two peaks developed for this drug in Britton-Robinson buffer at pH 8.0 has been considered for the present analytical study. An accumulation potential of -1.0 V versus Ag/AgCl/KCl(s), pulse amplitude a =100 mV, scan increment Delta E =10 mV, and frequency f =120 Hz were the optimal experimental parameters. Dipyridamole can be determined in the concentration range of 9.0 x 10(-9) to 5.0 x 10(-6) M using accumulation times of 30-300 s. A detection limit of 4.0 x 10(-11) M was achieved after a 300 s accumulation time. Applicability to serum samples was illustrated. The average recoveries for dipyridamole spiked to serum at 0.25-4.50 micro g ml(-1) were 96.0-102.0%, and the higher standard deviation was 2.9%. A detection limit of 0.06 micro g mL(-1) of serum was obtained.

  15. Highly sensitive determination of mercury using copper enhancer by diamond electrode coupled with sequential injection–anodic stripping voltammetry

    Energy Technology Data Exchange (ETDEWEB)

    Chaiyo, Sudkate [Department of Chemistry, Faculty of Science, Srinakharinwirot University (Thailand); Chailapakul, Orawon [Department of Chemistry, Faculty of Science, Chulalongkorn University (Thailand); Center for Petroleum, Petrochemicals, and Advanced Materials, Chulalongkorn University (Thailand); Siangproh, Weena, E-mail: weena@swu.ac.th [Department of Chemistry, Faculty of Science, Srinakharinwirot University (Thailand)

    2014-12-10

    Highlights: • Highly sensitive determination of Hg(II) using SI–ASV-BDD was achieved. • Electrochemical detection of Hg(II) using Cu(II) enhancer was accomplished. • LOD and LOQ were found to be very low at 40.0 ppt and 135.0 ppt. • This method was successfully applied for determination of Hg(II) in real samples. - Abstract: A highly sensitive determination of mercury in the presence of Cu(II) using a boron-doped diamond (BDD) thin film electrode coupled with sequential injection–anodic stripping voltammetry (SI–ASV) was proposed. The Cu(II) was simultaneously deposited with Hg(II) in a 0.5 M HCl supporting electrolyte by electrodeposition. In presence of an excess of Cu(II), the sensitivity for the determination of Hg(II) was remarkably enhanced. Cu(II) and Hg(II) were on-line deposited onto the BDD electrode surface at −1.0 V (vs. Ag/AgCl, 3 M KCl) for 150 s with a flow rate of 14 μL s{sup −1}. An anodic stripping voltammogram was recorded from −0.4 V to 0.25 V using a frequency of 60 Hz, an amplitude of 50 mV, and a step potential of 10 mV at a stopped flow. Under the optimal conditions, well-defined peaks of Cu(II) and Hg(II) were found at −0.25 V and +0.05 V (vs. Ag/AgCl, 3 M KCl), respectively. The detection of Hg(II) showed two linear dynamic ranges (0.1–30.0 ng mL{sup −1} and 5.0–60.0 ng mL{sup −1}). The limit of detection (S/N = 3) obtained from the experiment was found to be 0.04 ng mL{sup −1}. The precision values for 10 replicate determinations were 1.1, 2.1 and 2.9% RSD for 0.5, 10 and 20 ng mL{sup −1}, respectively. The proposed method has been successfully applied for the determination of Hg(II) in seawater, salmon, squid, cockle and seaweed samples. A comparison between the proposed method and an inductively coupled plasma optical emission spectrometry (ICP-OES) standard method was performed on the samples, and the concentrations obtained via both methods were in agreement with the certified values of Hg

  16. Applicability of 2-hydroxybenzaldehyde benzoylhydrazone in the determination of trace metals by adsorptive cathodic stripping voltammetry: relevancy of simultaneous determinations.

    Science.gov (United States)

    Espada-Bellido, Estrella; Galindo-Riaño, M Dolores; Aouarram, Abdellah; García-Vargas, Manuel

    2009-07-01

    The applicability of 2-hydroxybenzaldehyde benzoylhydrazone (2-HBBH) for determining Cd(II), Cu(II), Pb(II) and Bi(III) ions by adsorptive cathodic stripping voltammetry was studied. The sensitivity of metal reduction peak currents was highly enhanced with the addition of 2-HBBH to metallic solutions, showing the adsorptive characteristics of the complexes. Variable factors affecting the response (mainly: the influences of pH, supporting electrolyte and deposition potential on selectivity and sensitivity) were investigated. Limits of detection suitable for trace analysis were obtained: 0.28 microg L(-1) for Cd(II) at pH 10; 0.026 microg L(-1) for Pb(II) at pH 9; 0.285 microg L(-1) for Bi(III) at pH 8 and 0.051 microg L(-1) for Cu(II) at pH 9.5. Simultaneous determinations of two groups of elements, consisting of Cd(II)-Pb(II)-Cu(II) and Cd(II)-Pb(II)-Bi(III), at pH 9.5 and 9, respectively, were described with good resolution and sensitivities. Metals were quantified at concentrations in the range from 0.5 to 14 microg L(-1). The RSD at a concentration level of 5 microg L(-1) of metal was 4.28% for Cd(II), 2.99% for Pb(II), 4.82% for Bi(III) and 1.35% for Cu(II). The method was applied to the simultaneous determination of metals in certified reference water (TMDA-62) and in synthetic water samples with satisfactory results.

  17. Determination of chromium in estuarine waters by catalytic cathodic stripping voltammetry using a vibrating silver amalgam microwire electrode.

    Science.gov (United States)

    Espada-Bellido, Estrella; Bi, Zhaoshun; van den Berg, Constant M G

    2013-02-15

    Chromium (Cr(VI)) in water can be determined by adsorptive catalytic cathodic stripping voltammetry in the presence of diethylenetriaminepentaacetic acid (DTPA) and nitrate on the hanging mercury drop electrode (HMDE). Predominately Cr(VI) is detected and the water is UV-digested to convert all Cr to Cr(VI) prior to analysis. We develop here an alternative to the HMDE by using a silver amalgam electrode based on a vibrating microwire. The microwire electrodes were 12.5 μm in diameter and electrochemically coated with mercury, and were stable for a week. Conditions were re-optimised, and we used a DTPA concentration of 5mM, 30 mM acetate pH buffer (pH 5.5 in seawater and pH 5.8 in pure water), and 1.5M nitrate solution. The microwire was reactivated prior to each scan by applying a negative potential (-3V) for 2s which removed all deposited Cr. The detection limit for chromium in pH buffer was found to be 0.2 nM Cr(VI) and in seawater 0.3 nM Cr(VI) at a deposition time of 30s. The response increased linearly with the concentration of Cr(VI) up to 60 nM Cr(VI) in seawater. The limit of detection is less good than using the HMDE, but the linear range is good and the microwire electrode could form the basis of apparatus for flow-analysis. The method was successfully tested on water samples from the estuary of the river Mersey (Liverpool Bay) giving chromium concentrations between 1.48 nM and 2.29 nM. Copyright © 2012 Elsevier B.V. All rights reserved.

  18. Determination of Sb(III) using an ex-situ bismuth screen-printed carbon electrode by adsorptive stripping voltammetry.

    Science.gov (United States)

    Rojas-Romo, Carlos; Serrano, Núria; Ariño, Cristina; Arancibia, Verónica; Díaz-Cruz, José Manuel; Esteban, Miquel

    2016-08-01

    The determination of Sb(III) on an ex-situ bismuth screen-printed carbon electrode (ex-situ BiSPCE) by means of adsorptive stripping voltammetry (AdSV) using quercetin-5'-sulfonic acid as chelating agent was optimized. The effect of different experimental parameters such pH, ligand concentration (CQSA), accumulation potential (Eacc) and accumulation time (tacc) were studied to obtain a wide linear range, the highest sensitivity and the lowest detection limit. Ex-situ BiSPCE was analytically compared with a sputtered bismuth screen-printed electrode (BispSPE) under optimal conditions. The obtained analytical parameters suggest that ex-situ BiSPCE behaves much better than BispSPE and the first was selected for this study. Optimal parameters were pH=4.6; CQSA=10.0 to 20.0×10(-6)molL(-1); Eacc=-0.5V and tacc=60s. Peak area is proportional to Sb(III) concentration up to 100.0μgL(-1) (tacc 60s) and 45.0μgL(-1) (tacc 120s) range, with detection limits of 1.2μgL(-)(1) (tacc 60s) and 0.8μgL(-1) (tacc 120s). The relative standard deviation for a Sb(III) solution (20.0μgL(-1)) was 3.9% for ten successive assays. Thus, the effect of various interfering metal ions was studied and the methodology was validated using a spiked groundwater reference material with very satisfactory results.

  19. Polarographic behaviour of loratadine and its direct determination in pharmaceutical formulation and human plasma by cathodic adsorptive stripping voltammetry.

    Science.gov (United States)

    Ghoneim, M M; Mabrouk, M M; Hassanein, A M; Tawfik, A

    2001-07-01

    The polarographic behaviour of the antihistaminic drug loratadine has been investigated in B.R. buffer solution of different pH values. Contradictory to that mentioned before in a previously published work, loratadine is electro-active at the mercury electrode. In B.R. buffer solution of pH values > or =6 it is reduced via a single 2-electrons irreversible wave corresponding to saturation of carbon-nitrogen double bond of the pyridine ring. The electrode reaction pathway was proposed and discussed. A sensitive differential pulse stripping voltammetric method based on controlled adsorptive accumulation of loratadine on a hanging mercury drop electrode has been developed for its direct determination at nanomolar concentrations without nitration of the drug. The optimized conditions for the direct cathodic adsorptive stripping voltammetric determination of the drug are: 0.1 M sodium hydroxide solution as a supporting electrolyte, accumulation potential, -1.2 V; accumulation time, 30 s; scan rate, 2-5 mV x s(-1) and pulse amplitude 100 mV. The proposed procedure was applied for the assay of loratadine in pharmaceutical formulation and human plasma. The average recoveries were 99.32-99.44 and 100.33-102.99% with the RSD 0.27-0.42 and 0.39-0.90% in pharmaceutical formulation and human plasma, respectively. The limits of detection of 1.60x10(-7) and 1.25x10(-7) M loratadine were found in pharmaceutical formulation and human plasma, respectively.

  20. Poly(ester sulphonic acid) coated mercury thin film electrodes: characterization and application in batch injection analysis stripping voltammetry of heavy metal ions.

    Science.gov (United States)

    Brett, C M; Fungaro, D A

    2000-01-10

    Mercury-thin film electrodes coated with a thin film of poly(ester sulphonic acid) (PESA) have been investigated for application in the analysis of trace heavy metals by square wave anodic stripping voltammetry using the batch injection analysis (BIA) technique. Different polymer dispersion concentrations in water/acetone mixed solvent are investigated and are characterised by electrochemical impedance measurements on glassy carbon and on mercury film electrodes. The influence of electrolyte anion, acetate or nitrate, on polymer film properties is demonstrated, acetate buffer being shown to be preferable for stripping voltammetry applications. Although stripping currents are between 30 and 70% less at the coated than at bare mercury thin film electrodes, the influence of model surfactants on stripping response is shown to be very small. The effect of the composition of the modifier film dispersion on calibration plots is shown; however, detection limits of around 5 nM are found for all modified electrodes tested. This coated electrode is an alternative to Nafion-coated mercury thin film electrodes for the analysis of trace metals in complex matrices, particularly useful when there is a high concentration of non-ionic detergents.

  1. Determination of antioxidant activity of spices and their active principles by differential pulse voltammetry.

    Science.gov (United States)

    Palma, Alberto; Ruiz Montoya, Mercedes; Arteaga, Jesús F; Rodríguez Mellado, Jose M

    2014-01-22

    The anodic oxidation of mercury in the presence of hydrogen peroxide in differential pulse voltammetry (DPV) was used to determine the antioxidant (AO) character of radical scavengers. Hydroperoxide radical is formed at the potentials of the oxidation peak on mercury electrodes, such radical reacting with the antioxidants in different extension. The parameter C10 (antioxidant concentration at which the peak area decreases by 10%) is used to measure the scavenging activity of the individual antioxidants. To establish the scavenging activity of antioxidant mixtures as a whole, the parameter, μ10 as the reverse of V10, V10 being the volume necessary to decrease the peak area in DPV by 10%, was selected. Higher μ10 values correspond to higher scavenging activity. The studies have been extended to aqueous extracts of some species. The results may be useful in explaining the effect of spices in vitro and in vivo studies.

  2. Direct determination of tellurium and its redox speciation at the low nanogram level in natural waters by catalytic cathodic stripping voltammetry.

    Science.gov (United States)

    Biver, Marc; Quentel, François; Filella, Montserrat

    2015-11-01

    Tellurium is one of the elements recently identified as technologically critical and is becoming a new emergent contaminant. No reliable method exists for its determination in environmental samples such as natural waters. This gap is filled by the method described here; it allows the rapid detection of trace concentrations of Te(IV) and Te(VI) in surface waters by differential pulse cathodic stripping voltammetry. It is based on the proton reduction catalysed by the absorption of Te(IV) on the mercury electrode. Under our conditions (0.1 mol L(-1) HCl) a detection limit of about 5 ng L(-1) for a deposition time of 300 s is achieved. Organic matter does not represent a problem at low concentrations; higher concentrations are eliminated by adsorptive purification. Tellurium occurs primarily as Te(IV) and Te(VI) in natural waters. Thus, determining total Te requires the reduction of Te(VI) that it is not electroactive. A number of reduction procedures have been carefully evaluated and a method based on the addition of TiCl3 to the acidified samples has been proven to reduce Te(VI) at the trace level to Te(IV) reliably and quantitatively. Therefore, the procedure described allows the direct determination of total Te and its redox speciation. It is flexible, reliable and cost effective compared to any possible alternative method based on the common preconcentration-ICPMS approach. It is readily implementable as a routine method and can be deployed in the field with relative ease.

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

    Science.gov (United States)

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

    2013-08-06

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

  4. Direct Determination of Zinc, Cadmium, Lead, Copper Metal in Tap Water of Delhi (India by Anodic Stripping Voltammetry Technique

    Directory of Open Access Journals (Sweden)

    Raj J.

    2013-04-01

    Full Text Available Salts of Zinc, Cadmium, Lead and Copper are taken incidentally or accidently and has become of great toxicological importance having toxic effect. In the present study direct determination of Zn, Cd, Pb and Cu metal was carried out from tap water of Delhi (India using differential pulse anodic stripping Voltammeter (DPASV at Hanging mercury dropping electrode (HMDE.Determination of Zn, Cd, Pb, Cu was done using Ammonium acetate buffer (pH 4.6 with a sweep rate (scan rate of 59.5 mV/s and pulse amplitude 50mV by HMDE by standard addition method. The solution was stirred during pre-electrolysis at -1150mV (vs. Ag/AgCl for 90 seconds and the potential was scanned from -1150V to +100V (vs..Ag/AgCl. As a result the minimum level of Zn, Cd, Pb, Cu was Zero and the concentration observed in the tap water sample of Delhi (India was determined as 0.174 mg/L-1, 0.001 mg/L-1, 0.002 mg/L-1, 0.011 mg/L-1 respectively.

  5. Mapping Activity Variations for Ru2O3 in Lunar Volcanic Green Glass Analogs Using Differential Pulse Voltammetry

    Science.gov (United States)

    Malum, K. M.; Colson, R. O.; Sawarynski, M.

    2001-01-01

    Using differential pulse voltammetry, we are mapping variations in activities for NiO and Ru2O3 as a function of compositional variation for compositions centered around an Apollo 15 green glass analog. Additional information is contained in the original extended abstract.

  6. Extraction of arsenic as the diethyl dithiophosphate complex with supercritical fluid and quantitation by cathodic stripping voltammetry.

    Science.gov (United States)

    Arancibia, Verónica; López, Alex; Zúñiga, M Carolina; Segura, Rodrigo

    2006-02-28

    The separation of arsenic based on in situ chelation with ammonium diethyl dithiophosphate (ADDTP) has been carried out using methanol-modified supercritical CO(2). Aliquots of extract were added to an electroanalytical cell and arsenic was determined by square wave cathodic stripping voltammetry (SWCSV) at a hanging mercury drop electrode (HMDE). Quantitative extractions of As(DDTP)(3) were achieved when the experiments were carried out at a pressure of 2500psi, a temperature of 90 degrees C, 2.0mL of methanol, 20.0min of static extraction and 5.0min of dynamic extraction in the presence of 18mg of ADDTP. Analysis of arsenic was made using 150mgL(-1) of Cu(II) in 1M HCl solution as supporting electrolyte in the presence of ADDTP as ligand. Preconcentration was carried out by deposition at a potential of -0.50V and the intermetallic compound Cu(x)As(y) was reduced at a potential of -0.77 to -0.82V, depending on ligand concentration. The results showed that the presence of ligand plays an important role, increasing the method's sensitivity and preventing the oxidation of As(III). The calibration graph of the As(DDTP)(3) solution was linear from 0.8 to 12.5mugL(-1) of arsenic (LOD 0.5mugL(-1), R=0.9992, t(acc)=60s). The method was validated using carrot pulp spiked with arsenic solution. This method was applied to the determination of arsenic in samples of carrots, beets and irrigation water. Arsenic in beets was: skin 4.10+/-0.18mgkg(-1); pulp 3.83+/-0.19mgkg(-1) and juice 0.71+/-0.09mgL(-1); arsenic in carrots was: skin 2.15+/-0.09mgkg(-1); pulp 0.59+/-0.11mgkg(-1) and juice 0.71+/-0.03mgL(-1). Arsenic in water were: Chiu-Chiu 0.08mgL(-1), Inacaliri 1.12mgL(-1), and Salado river 0.17+/-0.07mgL(-1).

  7. Differential Pulse Anodic Stripping Voltammetric Determination of Lead with Heparin Modified Electrode

    Institute of Scientific and Technical Information of China (English)

    LI,Nian-Bing(李念兵); DUAN,Jian-Ping(段建平); CHEN,Guo-Nan(陈国南)

    2004-01-01

    A novel differential pulse anodic stripping voltammetry for the determination of trace amounts of lead, using a biomacromolecule heparin drop-coated modified glassy carbon electrode, has been described. Pb2+ was deposited on the surface of a heparin-modified electrode at - 1.0 V (vs. SCE) via forming Pb2+-heparin and subsequent reduction at the electrode. In the following step, Pb-heparin was oxidized, and voltammograms were recorded by scanning the potential in a positive direction. Conditions were optimized with respect to the pH of the medium, the mass of drop-coated heparin, accumulation potential and accumulation time. The peak current was proportional to the Pb2+ concentration in the range of 2.0× 10-9 to 7.0× 10-7 mol/L, The detection limit was 3.0× 10-10 mol/L.The relative standard deviation was 4.83% for 1.0× 10-8mol/L Pb2- (n= 10). The developed method has been applied to the determination of Pb2- in water samples with satisfactory results.

  8. Nonlinear Characteristics of an Intense Laser Pulse Propagating in Partially Stripped Plasmas

    Institute of Scientific and Technical Information of China (English)

    HU Qiang-Lin; LIU Shi-Bing; CHEN Tao; JIANG Yi-Jian

    2005-01-01

    The nonlinear optic characteristics of an intense laser pulse propagating in partially stripped plasmas are investigated analytically. The phase and group velocity of the laser pulse propagation as well as the three general expressions governing the nonlinear optic behavior, based on the photon number conservation, are obtained by considering the partially stripped plasma as a nonlinear optic medium. The numerical result shows that the presence of the bound electrons in partially stripped plasma can significantly change the propagating property of the intense laser pulse.

  9. Sensitive quantitation of Ochratoxin A in cocoa beans using differential pulse voltammetry based aptasensor.

    Science.gov (United States)

    Mishra, Rupesh K; Hayat, Akhtar; Catanante, Gaëlle; Istamboulie, Georges; Marty, Jean-Louis

    2016-02-01

    In this work, we propose for the first time a sensitive Ochratoxin A (OTA) detection in cocoa beans using competitive aptasensor by differential pulse voltammetry (DPV). In the proposed method, biotin labeled and free OTA competed to bind with immobilized aptamer onto the surface of a screen printed carbon electrode (SPCE), and percentage binding was calculated. The detection was performed after adding avidin-ALP to perform avidin-biotin reaction; the signal was generated through a suitable substrate 1-naphthyl phosphate (1-NP), for alkaline phosphatase (ALP). The cocoa samples were extracted and purified using molecular imprinted polymer (MIP) columns specifically designed for OTA. The developed aptasensor showed a good linearity in the range 0.15-5 ng/mL with the limit of detection (LOD) 0.07 ng/mL and 3.7% relative standard deviation (RSD). The aptasensor displayed good recovery values in the range 82.1-85% with 3.87% RSD, thus, demonstrated the efficiency of proposed aptasensor for such matrices.

  10. The determination of heavy metals in human gallstone by anodic stripping voltammetry; Analyse des metaux lourds contenus dans les calculs de la vesicule biliaire

    Energy Technology Data Exchange (ETDEWEB)

    Bouropoulos, N.; Koutsoukos, P.G.; Karavias, D. [Patras Univ. (Greece). Dept. of Inorganic Chemistry

    1996-04-01

    The accumulation of heavy metals in human tissues is indicative of exposure to toxic substances and analysis for their concentration levels in pathological situations may be correlated with the respective problems. In this work, anodic stripping voltammetry was applied to the analysis of the heavy metal content of human gallstones extracted surgically from patients coming from the region of south-western Greece. The stones were analysed for lead, copper cadmium zinc. The results obtained did not show any correlation of the analytical concentration of the heavy metals with the cholesterol or bilirubin content of the stones. Copper was found to be present in high concentrations while the mole fractions of cadmium and lead in the stones showed a linear log-log relationship with the total heavy metal concentration. The simplicity of the instrumentation involved, the extremely high sensitivity of the method and the high accuracy obtained make anodic stripping voltammetry a useful tool for the further investigation of the role of heavy metals in the pathogenesis of gallstones. (authors) 15 refs.

  11. Improving Reproducibility of Lab-on-a-Chip Sensor with Bismuth Working Electrode for Determining Zn in Serum by Anodic Stripping Voltammetry

    Science.gov (United States)

    Pei, Xing; Kang, Wenjing; Yue, Wei; Bange, Adam; Heineman, William R.; Papautsky, Ian

    2014-01-01

    This work reports on the continuing development of a lab-on-a-chip electrochemical sensor for determination of zinc in blood serum using square wave anodic stripping voltammetry. The microscale sensor consists of a three electrode system, including an environmentally friendly bismuth working electrode, an integrated silver/silver chloride reference electrode, and a gold auxiliary electrode. The sensor demonstrates a linear response in 0.1 M acetate buffer at pH 6 for zinc concentrations in the 1–30 μM range. By optimizing bismuth film deposition and better control of the fabrication process, repeatability of the sensor was improved, reducing variability from 42% to <2%. Through optimization of electrolyte and stripping voltammetry parameters, limit of detection was greatly improved to 60 nM. The optimized sensor was also able to measure zinc in the extracted blood serum. Ultimately, with integrated sample preparation, the sensor will permit rapid (min) measurements of zinc from a sub-mL sample (a few drops of blood) for clinical applications. PMID:24729629

  12. Electrochemical determination of resveratrol in dietary supplements at a boron-doped diamond electrode in the presence of hexadecyltrimethylammonium bromide using square-wave adsorptive stripping voltammetry

    Directory of Open Access Journals (Sweden)

    Yardim Yavuz

    2017-01-01

    Full Text Available A sensitive electroanalytical methodology for the determination of resveratrol is presented for the first time using adsorptive stripping voltammetry at a bare boron-doped diamond (BDD electrode. In cyclic voltammetry, resveratrol shows one irreversible and an adsorption-controlled oxidation peak at a BDD electrode. The voltammetric results indicated that in the presence of hexadecyl trimethyl ammonium bromide, the BDD electrode remarkably enhanced the oxidation of resveratrol, which leads to an improvement in the peak current with a shift of the peak potential to more positive values. Using the square-wave stripping mode, the compound yielded a well-defined voltammetric response in 0.1 M nitric acid solution containing 100 μmol L-1 hexadecyl trimethyl ammonium bromide at 0.74 V (vs. Ag/AgCl, after 60 s accumulation at the open-circuit condition. A linear calibration graph was obtained in the concentration range 0.025 to 60.0 μg mL-1, with a detection limit of 0.0063 μg mL-1. The applicability of the proposed method was verified by analysis of resveratrol in commercial dietary supplements.

  13. Investigation of the reduction process of dopamine using paired pulse voltammetry

    Science.gov (United States)

    Kim, Do Hyoung; Oh, Yoonbae; Shin, Hojin; Blaha, Charles D.; Bennet, Kevin E.; Lee, Kendall H.; Kim, In Young; Jang, Dong Pyo

    2014-01-01

    The oxidation of dopamine (DA) around +0.6V potential in anodic sweep and its reduction around −0.1V in cathodic sweep at a relatively fast scanning rate (300 V/s or greater) have been used for identification of DA oxidation in fast-scan cyclic voltammetry (FSCV). However, compared to the oxidation peak of DA, the reduction peak has not been fully examined in analytical studies, although it has been used as one of the representative features to identify DA. In this study, the reduction process of DA was investigated using paired pulse voltammetry (PPV), which consists of two identical triangle-shaped waveforms, separated by a short interval at the holding potential. Especially, the discrepancies between the magnitude of the oxidation and reduction peaks of DA were investigated based on three factors: (1) the instant desorption of the DA oxidation product (dopamine-o-quinone: DOQ) after production, (2) the effect of the holding potential on the reduction process, and (3) the rate-limited reduction process of DA. For the first test, the triangle waveform FSCV experiment was performed on DA with various scanrates (from 400 to 1000 V/s) and durations of switching potentials of the triangle waveform (from 0.0 to 6.0 ms) in order to vary the duration between the applied oxidation potential at +0.6V and the reduction potential at −0.2V. As a result, the ratio of reduction over oxidation peak current response decreased as the duration became longer. To evaluate the effect of holding potentials during the reduction process, FSCV experiments were conducted with holding potential from 0.0V to −0.8V. We found that more negative holding potentials lead to larger amount of reduction process. For evaluation of the rate-limited reduction process of DA, PPV with a 1Hz repetition rate and various delays (2, 8, 20, 40 and 80ms) between the paired scans were utilized to determine how much reduction process occurred during the holding potential (−0.4V). These tests showed that

  14. Investigation of the reduction process of dopamine using paired pulse voltammetry.

    Science.gov (United States)

    Kim, Do Hyoung; Oh, Yoonbae; Shin, Hojin; Blaha, Charles D; Bennet, Kevin E; Lee, Kendall H; Kim, In Young; Jang, Dong Pyo

    2014-03-15

    The oxidation of dopamine (DA) around +0.6V potential in anodic sweep and its reduction around -0.1V in cathodic sweep at a relatively fast scanning rate (300 V/s or greater) have been used for identification of DA oxidation in fast-scan cyclic voltammetry (FSCV). However, compared to the oxidation peak of DA, the reduction peak has not been fully examined in analytical studies, although it has been used as one of the representative features to identify DA. In this study, the reduction process of DA was investigated using paired pulse voltammetry (PPV), which consists of two identical triangle-shaped waveforms, separated by a short interval at the holding potential. Especially, the discrepancies between the magnitude of the oxidation and reduction peaks of DA were investigated based on three factors: (1) the instant desorption of the DA oxidation product (dopamine-o-quinone: DOQ) after production, (2) the effect of the holding potential on the reduction process, and (3) the rate-limited reduction process of DA. For the first test, the triangle waveform FSCV experiment was performed on DA with various scanrates (from 400 to 1000 V/s) and durations of switching potentials of the triangle waveform (from 0.0 to 6.0 ms) in order to vary the duration between the applied oxidation potential at +0.6V and the reduction potential at -0.2V. As a result, the ratio of reduction over oxidation peak current response decreased as the duration became longer. To evaluate the effect of holding potentials during the reduction process, FSCV experiments were conducted with holding potential from 0.0V to -0.8V. We found that more negative holding potentials lead to larger amount of reduction process. For evaluation of the rate-limited reduction process of DA, PPV with a 1Hz repetition rate and various delays (2, 8, 20, 40 and 80ms) between the paired scans were utilized to determine how much reduction process occurred during the holding potential (-0.4V). These tests showed that

  15. Catalytic hydrogen evolution in cathodic stripping voltammetry on a mercury electrode in the presence of cobalt(II) ion and phenylthiourea or thiourea.

    Science.gov (United States)

    Spătaru, N; Bănica, F G

    2001-11-01

    The system Co(II)-phenylthiourea (PTU)-borax buffer was investigated by cathodic stripping voltammetry (CSV) at a hanging mercury drop electrode. The results of the voltammetric measurements showed that the presence of both PTU and Co(II) gives rise to a new irreversible peak at about -1.5 V. Based upon our previous results obtained in the study of other sulfur compounds and the sulfide ion itself, the peak was ascribed to the catalytic hydrogen evolution superimposed on the reduction of the coordinated Co(II) ion. The catalyst itself is a Co(II) complex with the sulfide ion produced by the decomposition of the analyte during the deposition step. The influence of PTU and cobalt concentration, accumulation conditions and stripping parameters was investigated and complementary data on thiourea are included. The results showed that the measurement of the catalytic hydrogen evolution peak current can be used as a basis for a simple, accurate and rapid method for the determination of PTU within the concentration range 10-100 nM. The catalytic method is relatively free of interferences and could be a suitable alternative for cases in which the stripping peak due to mercury ion reduction in the accumulated mercury compound is disturbed by some interference.

  16. Determination of Cd, Pb and Cu in Mandovi estuary by differential pulse anodic stripping voltammetry

    Digital Repository Service at National Institute of Oceanography (India)

    George, M.D.; Sawkar, K.; Reddy, C.V.G.

    0-60% for Pb and 0-80% for Cu. Compared to the reported values from other estuaries, Mandovi estuarine waters have registered a higher concentration of the metals. These high concentrations, to a large extent, are considered to be the effect...

  17. Voltammetric Study and Determination of Phenylephrine Hydrochloride at INP-Nafion-Modified CPE Sensor Employing Differential Pulse Voltammetry

    Directory of Open Access Journals (Sweden)

    Zeinab Pourghobadi

    2014-03-01

    Full Text Available In this study, describes the voltammetric oxidation and determination of phenylephrine (PHE hydrochloride at a new chemically modified electrode. Iron nanoparticle (INPs was dispersed in Nafion solution to obtain a INP-Nafion-modified CPE for the voltammetric analysis of PHE .The electrochemical behaviour of PHE on INP-Nafion-modified CPE was studied, using cyclic voltammetry as a diagnostic technique. The effects of amount of INPs-Nafion dispersion, pH, and scan rate on the response of modified electrode for the oxidation of PHE were investigated. Using differential pulse voltammetry (DPV, the modified electrode indicated a dynamic linear range for quantitative determination of PHE in the range of 5 μM−130 μM, and the detection limit was estimated to be 0.76 μM. The method was developed for the determination of PHE in pharmaceutical samples with satisfactory results.

  18. Simultaneous voltammetric determination of morphine and noscapine by adsorptive differential pulse stripping method and least-squares support vector machines.

    Science.gov (United States)

    Niazi, Ali; Ghasemi, Jahanbakhsh; Zendehdel, Mojgan

    2007-11-30

    An adsorptive differential pulse stripping method for the simultaneous determination of morphine and noscapine is proposed. The procedure involves an adsorptive accumulation of morphine and noscapine on a hanging mercury drop electrode (HMDE), followed by oxidation of adsorbed morphine and noscapine by voltammetric scan using differential pulse modulation. The optimum experimental conditions are: pH 10.0, accumulation potential of -100 mV versus Ag/AgCl, accumulation time of 150 s, scan rate of 40 mV s(-1) and pulse height of 100 mV. Morphine and noscapine peak currents were observed in same potential region at about +0.25 V. The simultaneous determination of morphine and noscapine by using voltammetry is a difficult problem in analytical chemistry, due to voltammogram interferences. The resolution of mixture of morphine and noscapine by the application of least-squares support vector machines (LS-SVM) was performed. The linear dynamic ranges were 0.01-3.10 and 0.015-2.75 microg mL(-1) and detection limits were 3 and 7 ng mL(-1) for morphine and noscapine, respectively. The capability of the method for the analysis of real samples was evaluated by the determination of morphine and noscapine in addict's human plasma with satisfactory results.

  19. Functionalized Nanoporous Track-Etched b-PVDF Membrane Electrodes for Heavy Metal Determination by Square-Wave Anodic Stripping Voltammetry

    Directory of Open Access Journals (Sweden)

    Bessbousse H.

    2013-04-01

    Full Text Available Track-etched functionalized nanoporous β-PVDF membrane electrodes, or functionalized membrane electrodes (FMEs, are electrodes made from track-etched, poly(acrylic acid (PAA functionalized nanoporous β-poly(vinylidene fluoride (β-PVDF membranes with thin porous Au films sputtered on each side as electrodes. To form the β-PVDF nanoporous membranes, β-PVDF films are irradiated by swift heavy ions. After irradiation, radical tracks are stable in the membranes. Chemical etching removes some of the radical tracks revealing nanopores. Radicals, remaining in the pores, initiate radio grafting of PAA from the pore walls of the nanoporous β-PVDF. PAA is a cation exchange polymer that adsorbs metal ions, such as Pb2+, from aqueous solutions thus concentrating the ions into the membrane. After a calibrated time the FME is transferred to an electrochemical cell for square-wave anodic stripping voltammetry analysis.

  20. Trace and selective determination of cobalt(II in water and salt samples using cathodic adsorptive stripping voltammetry in the presence of pyrogallol red

    Directory of Open Access Journals (Sweden)

    Hasanpour Foroozan

    2013-01-01

    Full Text Available A sensitive and selective procedure is presented for voltammetric determination of cobalt. The procedure involves an adsorptive accumulation of cobalt pyrogallol red (PGR complex on stationary mercury drop electrode, followed by cathodic stripping voltammetry measurement of reduction current of adsorbed complex at -1.17 V (vs. Ag/AgCl. The optimum conditions for determination of cobalt include pH 11.0, 35 μM pyrogallol red, an accumulation potential of -0.9 V (vs. Ag/AgCl and scan rate 80 mVs-1. The peak current is proportional to the concentration of cobalt over the concentration range of 5.0 to 280 ng mL-1 with a detection limit of 1 ng mL-1 with an accumulation time of 140 s. The method was applied for the determination of cobalt in analytical grade NaCl and water samples.

  1. Determination of picomolar levels of platinum in estuarine waters: a comparison of cathodic stripping voltammetry and isotope dilution-inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Obata, Hajime; Yoshida, Tetsuaki; Ogawa, Hiroshi

    2006-10-27

    A comparative study to determine picomolar concentrations of platinum in natural waters was performed using two different analytical techniques. Results obtained by cathodic stripping voltammetry (CSV) were compared with those obtained by isotope dilution-inductively coupled plasma mass spectrometry (ID-ICPMS) combined with anion exchange resin column extraction method. Using successive UV irradiations with low-pressure mercury (L-Hg) lamp for 4h prior to CSV analysis, the results of both methods were comparable. Without adequate photolytic decomposition, the results obtained using CSV were generally lower than those obtained using ID-ICPMS in the estuarine waters around Tokyo Bay. This difference implies the presence of organically complexed Pt species in the estuarine waters. The Pt enrichment in the middle of the Tokyo Bay estuaries probably reflects the anthropogenic release of Pt from highly populated areas in Tokyo.

  2. Direct simultaneous determination of Co, Cu, Fe, Ni and V in pore waters by means of adsorptive cathodic stripping voltammetry with mixed ligands.

    Science.gov (United States)

    Santos-Echeandía, Juan

    2011-07-15

    An analytical procedure is proposed for the direct simultaneous determination in a single scan of Co, Cu, Fe, Ni and V in sediment pore waters by means of adsorptive cathodic stripping voltammetry (ACSV) with mixed ligands (DMG and catechol). Optimum conditions for the determination of these five elements were studied. Detection limits of the technique depended upon the reproducibility of the procedure blank, and were found to be 0.04 nM Co, 0.09 nM Cu, 1.29 nM Fe, 0.46 nM Ni and 2,52 nMV making the method suitable for the direct simultaneous determination of these five metals in pore waters, estuarine waters and probably coastal waters. Copyright © 2011 Elsevier B.V. All rights reserved.

  3. Determination of brilliant blue FCF in the presence and absence of erythrosine and quinoline yellow food colours by cathodic stripping voltammetry.

    Science.gov (United States)

    Florian, M; Yamanaka, H; Carneiro, P A; Zanoni, M Valnice Boldrin

    2002-09-01

    A study of the voltammetric behaviour of the food colours brilliant blue FCF (C.I. 42090), erythrosine (C.I. 45430) and quinoline yellow (C.I. 47005) in the pH range 2-10 have been carried out by cathodic#10; stripping voltammetry. At pH 4.5 (acetate buffer) with an accumulation potential of 0 V and accumulation time of 30s, the voltammograms presented well-defined reduction peaks at potential - 0.76 V for brilliant blue FCF, - 0.85 V for quinoline yellow and - 0.54 V for erythrosine. Linear calibration graphs were obtained from 8 to 80 microg l(-1) brilliant blue, from 4 to 43 microg l(-1) quinoline yellow and from 10 to 70 microg l(-1) erythrosine. The method has been successfully applied to identify and quantify binary mixtures of these dyes and applied for determining brilliant blue FCF in commercial food products.

  4. On-site fuel electroanalysis: determination of lead, copper and mercury in fuel bioethanol by anodic stripping voltammetry using screen-printed gold electrodes.

    Science.gov (United States)

    Almeida, Eduardo S; Richter, Eduardo M; Munoz, Rodrigo A A

    2014-07-21

    The potential application of commercial screen-printed gold electrodes (SPGEs) for the trace determination of lead, copper, and mercury in fuel bioethanol is demonstrated. Samples were simply diluted in 0.067 mol L(-1) HCl solution prior to square-wave anodic stripping voltammetry (SWASV) measurements recorded with a portable potentiostat. The proposed method presented a low detection limit (<2 μg L(-1)) for a 240 s deposition time, linear range between 5 and 300 μg L(-1), and adequate recovery values (96-104%) for spiked samples. This analytical method shows great promise for on-site trace metal determination in fuel bioethanol once there is no requirement for sample treatment or electrode modification.

  5. Mercury(II) trace detection by a gold nanoparticle-modified glassy carbon electrode using square-wave anodic stripping voltammetry including a chloride desorption step.

    Science.gov (United States)

    Laffont, Laure; Hezard, Teddy; Gros, Pierre; Heimbürger, Lars-Eric; Sonke, Jeroen E; Behra, Philippe; Evrard, David

    2015-08-15

    Gold nanoparticles (AuNPs) were deposited on a glassy carbon (GC) substrate by constant potential electrolysis and characterized by cyclic voltammetry in H2SO4 and field emission gun scanning electron microscopy (FEG-SEM). The modified AuNPs-GC electrode was used for low Hg(II) concentration detection using a Square Wave Anodic Stripping Voltammetry (SWASV) procedure which included a chloride desorption step. The comparison of the obtained results with our previous work in which no desorption step was used showed that this latter step significantly improved the analytical performances, providing a three time higher sensitivity and a limit of detection of 80pM for 300s preconcentration, as well as a lower average standard deviation. The influence of chloride concentration on the AuNPs-GC electrode response to Hg(II) trace amounts was also studied and its optimal value confirmed to be in the 10(-2)M range. Finally, the AuNPs-GC electrode was used for the determination of Hg(II) in a natural groundwater sample from south of France. By using a preconcentration time of 3000s, a Hg(II) concentration of 19±3pM was found, which compared well with the result obtained by cold vapor atomic fluorescence spectroscopy (22±2pM).

  6. Determination of oleuropein using multiwalled carbon nanotube modified glassy carbon electrode by adsorptive stripping square wave voltammetry.

    Science.gov (United States)

    Cittan, Mustafa; Koçak, Süleyman; Çelik, Ali; Dost, Kenan

    2016-10-01

    A multi-walled carbon nanotube modified glassy carbon electrode was used to prepare an electrochemical sensing platform for the determination of oleuropein. Results showed that, the accumulation of oleuropein on the prepared electrode takes place with the adsorption process. Electrochemical behavior of oleuropein was studied by using cyclic voltammetry. Compared to the bare GCE, the oxidation peak current of oleuropein increased about 340 times at MWCNT/GCE. Voltammetric determination of oleuropein on the surface of prepared electrode was studied using square wave voltammetry where the oxidation peak current of oleuropein was measured as an analytical signal. A calibration curve of oleuropein was performed between 0.01 and 0.70µM and a good linearity was obtained with a correlation coefficient of 0.9984. Detection and quantification limits of the method were obtained as 2.73 and 9.09nM, respectively. In addition, intra-day and inter-day precision studies indicated that the voltammetric method was sufficiently repeatable. Finally, the proposed electrochemical sensor was successfully applied to the determination of oleuropein in an olive leaf extract. Microwave-assisted extraction of oleuropein had good recovery values between 92% and 98%. The results obtained with the proposed electrochemical sensor were compared with liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis.

  7. Application of normal pulse voltammetry to the kinetic study of formic acid oxidation on a carbon supported Pd electrocatalyst

    Science.gov (United States)

    Wang, Yujiao; Wu, Xiaochen; Wu, Bing; Gao, Ying

    The kinetic parameters of formic acid oxidation on a carbon supported Pd electrode, such as the charge transfer coefficient (α) and apparent diffusion coefficient (D) are obtained by applying the technique of normal pulse voltammetry. The standard rate constant (k 0) of formic acid oxidation on a Pd/C electrode is estimated. The results show that formic acid oxidation is more sensitive to temperature at relatively high potential because the activation energy is significantly increased as the potential rose above 0.6 V.

  8. Application of experimental design on determination of aluminum content in saline samples by adsorptive cathodic stripping voltammetry

    OpenAIRE

    YILMAZ, Sinan; Öztürk, Betül; ÖZDEMİR, Durmuş

    2013-01-01

    Adsorptive cathodic stripping voltammetric determination of aluminum at ng mL-1 levels in salt samples based on the metal complexation with Calcon (1-(2-hydroxynaphthylazo)-2 naphthol-4-sulfonic acid) and the subsequent adsorptive deposition onto a hanging mercury drop electrode was studied. Central composite design was used as a design method. Several chemical and instrumental parameters (pH, ligand concentration, deposition time, deposition potential, and complexing time) were invo...

  9. Kinetic and equilibrium studies for the adsorption process of cadmium(II) and copper(II) onto Pseudomonas aeruginosa using square wave anodic stripping voltammetry method

    Energy Technology Data Exchange (ETDEWEB)

    Kong Bo; Tang Biyu; Liu Xiaoying; Zeng Xiandong; Duan Haiyan [State Key Laboratory of Chemo/Biosensing and Chemometrics, College of Chemistry and Chemical Engineering, Hunan University, Hunan, Changsha 410082 (China); Luo Shenglian, E-mail: kongbo2136@163.com [State Key Laboratory of Chemo/Biosensing and Chemometrics, College of Chemistry and Chemical Engineering, Hunan University, Hunan, Changsha 410082 (China); Wei Wanzhi [State Key Laboratory of Chemo/Biosensing and Chemometrics, College of Chemistry and Chemical Engineering, Hunan University, Hunan, Changsha 410082 (China)

    2009-08-15

    A novel method for the simultaneous determination of cadmium(II) and copper(II) during the adsorption process onto Pseudomonas aeruginosa was developed. The concentration of the free metal ions was successfully detected by square wave anodic stripping voltammetry (SWASV) on the mercaptoethane sulfonate (MES) modified gold electrode, while the P. aeruginosa was efficiently avoided approaching to the electrode surface by the MES monolayer. And the anodic stripping peaks of Cd{sup 2+} and Cu{sup 2+} appear at -0.13 and 0.34 V respectively, at the concentration range of 5-50 {mu}M, the peak currents of SWASV present linear relationships with the concentrations of cadmium and copper respectively. As the determination of Cd{sup 2+} and Cu{sup 2+} was in real time and without pretreatment, the kinetic characteristics of the adsorption process were studied and all the corresponding regression parameters were obtained by fitting the electrochemical experimental data to the pseudo-second-order kinetic model. Moreover, Langmuir and Freundlich models well described the biosorption isotherms. And there were some differences in the amount of metal ion adsorbed at equilibrium (q{sub e}) and other kinetics parameters when the two ions coexisted were compared with the unaccompanied condition, which were also discussed in this paper. The proposed electrode system provides excellent platform for the simultaneous determination of trace metals in complex biosorption process.

  10. Selective determination of trace copper(II) by cathodic adsorptive stripping voltammetry with a naphthol-derivative Schiff's base.

    Science.gov (United States)

    Shamsipur, Mojtaba; Saeidi, Mahboubeh; Sharghi, Hashem; Naeimi, Hossein

    2003-01-01

    A selective and sensitive stripping voltammetric method for the determination of trace amounts of copper(II) with a recently synthesized naphthol-derivative Schiff's base (2,2'-[1,2-ethanediylbis(nitriloethylidyne)]bis(1-naphthalene)) is presented. The method is based on adsorptive accumulation of the resulting copper-Schiff's base complex on a hanging mercury drop electrode, followed by the stripping voltammetric measurement at the reduction current of adsorbed complex at -0.15 V (vs. Ag/AgCl). The optimal conditions for the stripping analysis of copper include pH 5.5 to 6.5, 8 microM Schiff's base and an accumulation potential of -0.05 V (vs. Ag/AgCI). The peak current is linearly proportional to the copper concentration over a range 2.3-50.8 ng ml(-1) with a limit of detection of 1.9 ng ml(-1). The accumulation time and RSD are 90 s and (3.2-3.5)%, respectively. The method was applied to the determination of copper in some analytical grade salts, tap water, human serum and sheep's liver.

  11. In situ microliter-droplet anodic stripping voltammetry of copper stained on the gold label after galvanic replacement reaction enlargement for ultrasensitive immunoassay of proteins.

    Science.gov (United States)

    Qin, Xiaoli; Xu, Aigui; Wang, Linchun; Liu, Ling; Chao, Long; He, Fang; Tan, Yueming; Chen, Chao; Xie, Qingji

    2016-05-15

    We report a new protocol for ultrasensitive electrochemical sandwich-type immunosensing, on the basis of signal amplification by gold-label/copper-staining, galvanic replacement reactions (GRRs), and in situ microliter-droplet anodic stripping voltammetry (ASV) after an enhanced cathodic preconcentration of copper. First, a sandwich-type immuno-structure is appropriately assembled at a glassy carbon electrode. Second, copper is selectively stained on the catalytic surfaces of second antibody-conjugated Au nanoparticles through CuSO4-ascorbic acid redox reaction, and the GRRs between HAuCl4 and the stained copper are used to amplify the quantity of copper. Finally, the corresponding antigen is determined based on simultaneous chemical-dissolution/cathodic-preconcentration of copper for in-situ ASV analysis directly at the immunoelectrode. Cyclic voltammetry, electrochemical impedance spectroscopy, quartz crystal microbalance and scanning electron microscopy are used for film characterization and/or process monitoring. Under optimized conditions, ultrasensitive analyses of human immunoglobulin G (IgG) and human carbohydrate antigen 125 (CA125) are achieved. The limits of detection are 0.3 fg mL(-1) (equivalent to 7 IgG molecules in the 6 μL sample employed) for IgG (S/N=3) and 1.3 nU mL(-1) for CA125 (S/N=3), respectively, which are amongst the best reported to date for the two proteins. The theoretical feasibility of such a single-molecule-level amperometric immunoassay is also discussed based on the immunological reaction thermodynamics. Copyright © 2016 Elsevier B.V. All rights reserved.

  12. The redox thermodynamics and kinetics of flavonoid rutin adsorbed at glassy carbon electrodes by stripping square wave voltammetry

    Energy Technology Data Exchange (ETDEWEB)

    Aragao Catunda, Francisco Eduardo; Araujo, Marcelo Francisco de [Departamento de Quimica, Instituto de Ciencias Exactas, Universidad Federal Rural do Rio de Janeiro, BR 465 KM 07, 23890-000, Seropedica, RJ (Brazil); Granero, Adrian Marcelo; Arevalo, Fernando Javier [Departamento de Quimica, Facultad de Ciencias Exactas, Fisico-Quimicas y Naturales, Universidad Nacional de Rio Cuarto, Agencia Postal No 3 - (5800), Rio Cuarto (Argentina); Carvalho, Mario Geraldo de [Departamento de Quimica, Instituto de Ciencias Exactas, Universidad Federal Rural do Rio de Janeiro, BR 465 KM 07, 23890-000, Seropedica, RJ (Brazil); Zon, Maria Alicia, E-mail: azon@exa.unrc.edu.ar [Departamento de Quimica, Facultad de Ciencias Exactas, Fisico-Quimicas y Naturales, Universidad Nacional de Rio Cuarto, Agencia Postal No 3 - (5800), Rio Cuarto (Argentina); Fernandez, Hector, E-mail: hfernandez@exa.unrc.edu.ar [Departamento de Quimica, Facultad de Ciencias Exactas, Fisico-Quimicas y Naturales, Universidad Nacional de Rio Cuarto, Agencia Postal No 3 - (5800), Rio Cuarto (Argentina)

    2011-11-30

    Highlights: > Adsorptive accumulation of rutin is studied at glassy carbon (GC) electrodes. > The Frumkin adsorption isotherm described the specific interaction. > Gibbs free energy of adsorption and the interaction parameter were determined. > Thermodynamics and kinetics of the surface redox process were characterized by SWV. > Detection limit for rutin was 2 x 10{sup -8} mol dm{sup -3} (12 ppb). - Abstract: The adsorptive accumulation of rutin (RU) at glassy carbon (GC) electrodes in 10% ethanol + 90% 1 mol dm{sup -3} HClO{sub 4} aqueous solution is studied by using cyclic (CV) and square wave (SWV) voltammetries. The Frumkin adsorption isotherm best described the specific interaction of rutin with carbon electrodes. By fitting the experimental data, values of -31.9 kJ mol{sup -1} and 0.54 {+-} 0.02 were obtained for the Gibbs free energy of adsorption and the interaction parameter, respectively. SWV fully characterized the thermodynamics and kinetics of the surface redox process, using a combination of the 'quasi-reversible maximum' and the 'splitting of SW peaks' methods. Average values of 0.644 {+-} 0.003 V and 0.44 {+-} 0.02 were obtained for the formal potential and the anodic transfer coefficient, respectively. Moreover, a formal rate constant of 6.1 x 10{sup 2} s{sup -1} was obtained. SWV was also employed to generate calibration curves. The lowest concentration of RU experimentally measured for a signal-to-noise ratio of 3:1 was 2 x 10{sup -8} mol dm{sup -3} (12 ppb).

  13. Adsorptive stripping differential pulse voltammetric determination of venlafaxine and desvenlafaxine employing Nafion-carbon nanotube composite glassy carbon electrode

    Energy Technology Data Exchange (ETDEWEB)

    Sanghavi, Bankim J. [Department of Chemistry, University of Mumbai, Vidyanagari, Santacruz (East), Mumbai 400 098, Maharashtra (India); Srivastava, Ashwini K., E-mail: aksrivastava@chem.mu.ac.i [Department of Chemistry, University of Mumbai, Vidyanagari, Santacruz (East), Mumbai 400 098, Maharashtra (India)

    2011-04-15

    A Nafion-carbon nanotube-modified glassy carbon electrode (NAF-CNT-GCE) was developed for the determination of venlafaxine (VF) and desvenlafaxine (DVF). The electrochemical behavior of both these molecules was investigated employing cyclic voltammetry (CV), chronocoulometry (CC), electrochemical impedance spectroscopy (EIS) and adsorptive stripping differential pulse voltammetry (AdSDPV). The surface morphology of the electrodes has been studied by means of scanning electron microscopy (SEM). These studies revealed that the oxidation of VF and DVF is facilitated at NAF-CNT-GCE. After optimization of analytical conditions employing this electrode at pH 7.0 in Britton-Robinson buffer (0.05 M) for VF and pH 5.0 in acetate buffer (0.1 M) for DVF, the peak currents for both the molecules were found to vary linearly with their concentrations in the range of 3.81 x 10{sup -8}-6.22 x 10{sup -5} M for VF and 5.33 x 10{sup -8}-3.58 x 10{sup -5} M for DVF. The detection limits (S/N = 3) of 1.24 x 10{sup -8} and 2.11 x 10{sup -8} M were obtained for VF and DVF, respectively, using AdSDPV. The prepared modified electrode showed several advantages, such as simple preparation method, high sensitivity, very low detection limits and excellent reproducibility. The proposed method was employed for the determination of VF and DVF in pharmaceutical formulations, urine and blood serum samples.

  14. Complexation-Based Detection of Nickel(II at a Graphene-Chelate Probe in the Presence of Cobalt and Zinc by Adsorptive Stripping Voltammetry

    Directory of Open Access Journals (Sweden)

    Keagan Pokpas

    2017-07-01

    Full Text Available The adsorptive stripping voltammetric detection of nickel and cobalt in water samples at metal film electrodes has been extensively studied. In this work, a novel, environmentally friendly, metal-free electrochemical probe was constructed for the ultra-trace determination of Ni2+ in water samples by Adsorptive Cathodic Stripping Voltammetry (AdCSV. The electrochemical platform is based on the adsorptive accumulation of Ni2+ ions directly onto a glassy carbon electrode (GCE modified with dimethylglyoxime (DMG as chelating agent and a Nafion-graphene (NGr nanocomposite to enhance electrode sensitivity. The nafion-graphene dimethylglyoxime modified glassy carbon electrode (NGr-DMG-GCE shows superior detection capabilities as a result of the improved surface-area-to-volume ratio and enhanced electron transfer kinetics following the incorporation of single layer graphene, while limiting the toxic effects of the sensor by removal of the more common mercury, bismuth and lead films. Furthermore, for the first time the NGr-DMG-GCE, in the presence of common interfering metal ions of Co2+ and Zn2+ demonstrates good selectivity and preferential binding towards the detection of Ni2+ in water samples. Structural and morphological characterisation of the synthesised single layer graphene sheets was conducted by Raman spectrometry, HRTEM and HRSEM analysis. The instrumental parameters associated with the electrochemical response, including accumulation potential and accumulation time were investigated and optimised in addition to the influence of DMG and graphene concentrations. The NGr-DMG-GCE demonstrated well resolved, reproducible peaks, with RSD (% below 5% and a detection limit of 1.5 µg L−1 for Ni2+ reduction at an accumulation time of 120 s., the prepared electrochemical sensor exhibited good detection and quantitation towards Ni2+ detection in tap water samples, well below 0.1 mg L−1 set by the WHO and EPA standards. This comparable to the South

  15. Complexation-Based Detection of Nickel(II) at a Graphene-Chelate Probe in the Presence of Cobalt and Zinc by Adsorptive Stripping Voltammetry.

    Science.gov (United States)

    Pokpas, Keagan; Jahed, Nazeem; Baker, Priscilla G; Iwuoha, Emmanuel I

    2017-07-25

    The adsorptive stripping voltammetric detection of nickel and cobalt in water samples at metal film electrodes has been extensively studied. In this work, a novel, environmentally friendly, metal-free electrochemical probe was constructed for the ultra-trace determination of Ni(2+) in water samples by Adsorptive Cathodic Stripping Voltammetry (AdCSV). The electrochemical platform is based on the adsorptive accumulation of Ni(2+) ions directly onto a glassy carbon electrode (GCE) modified with dimethylglyoxime (DMG) as chelating agent and a Nafion-graphene (NGr) nanocomposite to enhance electrode sensitivity. The nafion-graphene dimethylglyoxime modified glassy carbon electrode (NGr-DMG-GCE) shows superior detection capabilities as a result of the improved surface-area-to-volume ratio and enhanced electron transfer kinetics following the incorporation of single layer graphene, while limiting the toxic effects of the sensor by removal of the more common mercury, bismuth and lead films. Furthermore, for the first time the NGr-DMG-GCE, in the presence of common interfering metal ions of Co(2+) and Zn(2+) demonstrates good selectivity and preferential binding towards the detection of Ni(2+) in water samples. Structural and morphological characterisation of the synthesised single layer graphene sheets was conducted by Raman spectrometry, HRTEM and HRSEM analysis. The instrumental parameters associated with the electrochemical response, including accumulation potential and accumulation time were investigated and optimised in addition to the influence of DMG and graphene concentrations. The NGr-DMG-GCE demonstrated well resolved, reproducible peaks, with RSD (%) below 5% and a detection limit of 1.5 µg L(-1) for Ni(2+) reduction at an accumulation time of 120 s., the prepared electrochemical sensor exhibited good detection and quantitation towards Ni(2+) detection in tap water samples, well below 0.1 mg L(-1) set by the WHO and EPA standards. This comparable to the South

  16. Microanalysis of oligodeoxynucleotides by cathodic stripping voltammetry at amalgam-alloy surfaces in the presence of copper ions.

    Science.gov (United States)

    Hason, Stanislav; Vetterl, Vladimír

    2006-05-15

    The application of gold amalgam-alloy electrode (AuAE) for a sensitive voltammetric detection of different oligodeoxynucleotides (ODNs) containing the purine units within the ODN-chains in the presence of copper is described. The detection of ODNs is based on the following procedure: (i) the first step includes an acidic hydrolysis of the ODN (ahODN) samples performing the release of the purine bases from ODN-chain; (ii) the second step includes an electrochemical accumulation of the complex of the purine base residues released from ODN-chain with copper ions Cu(I) (ahODN-Cu(I) complex) at the potential of reduction of copper ions Cu(II) on the amalgam-alloy electrode surfaces; (iii) finally followed the cathodic stripping of the electrochemically accumulated ahODN-Cu(I) complex from the electrode surface. The proposed electrochemical method was used for: (a) detection of different ODN lengths containing only adenine units (the number of adenine units within the ODN-chains was changed from 10 to 80), and (b) determination of the number of purine units within the 30-mer ODNs containing a random sequence segments involving both the purine and pyrimidine units. The intensity of the cathodic stripping current density peak (j(CSP)) of the electrochemically accumulated ahODN-Cu(I) complex increased linearly with the increasing number of purine units within the ODN-chains. We observed a good correlation between the percentage content of purine units to the whole length of different 30-mer ODNs and the percentage content of the intensity of the j(CSP) of the electrochemically accumulated 30-mer ahODN-Cu(I) complexes. The detection of acid hydrolysed 80-mer (A(80)) in the bulk solution and in a 20-mul volume is possible down to 200pM and 2nM at the AuAE, respectively. For the shortest 10-mer (A(10)) a detectable value of 5nM in the bulk solution on the AuAE was observed. The sensitive detection of different ODNs containing the purine units in their chains in the presence of

  17. Determination of Xanthine in the Presence of Hypoxanthine by Adsorptive Stripping Voltammetry at the Mercury Film Electrode

    Science.gov (United States)

    Farias, Percio Augusto Mardini; Castro, Arnaldo Aguiar

    2014-01-01

    A stripping method for the determination of xanthine in the presence of hypoxanthine at the submicromolar concentration levels is described. The method is based on controlled adsorptive accumulation at the thin-film mercury electrode followed by a fast linear scan voltammetric measurement of the surface species. Optimum experimental conditions were found to be the use of 1.0 × 10−3 mol L−1 NaOH solution as supporting electrolyte, an accumulation potential of 0.00 V for xanthine and −0.50 V for hypoxanthine–copper, and a linear scan rate of 200 mV second−1. The response of xanthine is linear over the concentration ranges of 20–140 ppb. For an accumulation time of 30 minutes, the detection limit was found to be 36 ppt (2.3 × 10−10 mol L−1). Adequate conditions for measuring the xanthine in the presence of hypoxanthine, copper and other metals, uric acid, and other nitrogenated bases were also investigated. The utility of the method is demonstrated by the presence of xanthine associated with hypoxanthine, uric acid, nitrogenated bases, ATP, and ssDNA. PMID:24940040

  18. Application of adsorptive stripping voltammetry to the simultaneous determination of bismuth and copper in the presence of nuclear fast red.

    Science.gov (United States)

    Gholivand, M B; Romiani, A A

    2006-06-30

    A sensitive and selective method for the simultaneous determination of copper and bismuth by adsorptive stripping was developed using nuclear fast red (2-anthracenesulfonic acid, 4-amino-9,10-dihydro-1,3-dihydroxy-9,10-dioxo-, monosodium salt) as selective complexing agent onto hanging mercury drop electrode. In a single scan both metals gave peaks that were distinctly separated by 85 mV allowing their determination in the presence of each other. Optimal analytical conditions were found to be: nuclear fast red concentration of 80 microM, pH of 2.8 and adsorptive potential of -300 mV versus Ag/AgCl. With accumulation time of 180s the peaks currents are proportional to concentration of copper and bismuth over the 1-100 and 5-60 ng mL(-1) range with detection limits of 0.2 and 1.2 ng mL(-1), respectively. The procedure was applied to simultaneous determination of copper and bismuth in some real samples.

  19. Application of anodic stripping voltammetry for zinc, copper, and cadmium quantification in the aqueous humor: implications of pseudoexfoliation syndrome.

    Science.gov (United States)

    Panteli, Vassiliki S; Kanellopoulou, Dimitra G; Gartaganis, Sotirios P; Koutsoukos, Petros G

    2009-12-01

    Anodic stripping voltammetric (ASV) procedure, using mercury film electrode, was optimized and applied to determine the concentrations of zinc, cadmium, and copper in the aqueous humor. Concentration levels as low as 1 ppb of the test metals was possible to be detected using short electrolysis times (120 s) and microquantities of aqueous humor (up to 35 μL). As a first application of the voltammetric analysis of trace metals in the aqueous humor, the role of the three selected trace elements in the pseudoexfoliation (PEX) syndrome was examined. Samples from aqueous humor were collected during cataract extraction from patients with and without PEX. The zinc and copper concentration levels in the aqueous humor did not show statistically significant difference in the study and control group. Cadmium was detected in a small number of samples, without however statistical differences between the two groups. ASV proved to be a highly precise and sensitive tool for the quantification of heavy metal ions in aqueous humor. Further studies may lead to useful conclusions for the role of zinc, copper, or cadmium in PEX syndrome.

  20. Determination of the antibiotic drug pefloxacin in bulk form, tablets and human serum using square wave cathodic adsorptive stripping voltammetry.

    Science.gov (United States)

    Beltagi, A M

    2003-04-10

    A simple, rapid, reliable and fully validated square wave cathodic adsorptive stripping voltammetric procedure has been developed for the determination of the antibiotic pefloxacin drug in bulk form, tablets and human serum, based on its electrochemical reduction at a hanging mercury drop electrode. The Britton-Robinson buffer of pH 7.0 was found to be reasonable as a supporting electrolyte for assay of the drug. Pefloxacin drug, at the optimized conditions, showed a single 2-electron well-defined peak at -1.07 V (versus Ag/AgCl/KCl(s)) using an accumulation potential of -0.40 V. This peak may be attributed to the reduction of the C=O group. A mean recovery of 99.54%+/-0.23 and a detection limit of 1.65 x 10(-10) M pefloxacin were achieved. After being validated, the proposed procedure was successfully applied for the determination of the drug in tablets and human serum with mean recoveries of 99.57+/-0.48 and 98.55+/-0.78%, respectively. A detection limit of 4.50 x 10(-10) M was achieved for the determination of the drug in human serum. Results of the proposed procedure were comparable with those obtained by reported methods.

  1. Determination of selenium(IV) by catalytic stripping voltammetry with an in situ plated bismuth-film electrode.

    Science.gov (United States)

    Long, Jiajie; Nagaosa, Yukio

    2007-11-01

    A very sensitive and simple method is presented for the determination of Se(IV) by Osteryang square-wave cathodic stripping voltammery (OSWCSV). The method is based on the reduction of Se(IV) with Bi(III) onto an edge-plane type of pyrolytic graphite substrate, followed by a cathodic potential scan. OSWCSV studies indicate that the reduced selenium produced a distinct catalytic hydrogen wave at -1150 mV vs. Ag/AgCl. The peak height of the catalytic hydrogen wave was directly proportional to the initial Se(IV) concentration in the ranges of 0.1 - 1.0 and 1.0 - 20.0 microg L(-1) (correlation coefficients 0.9800 and 0.9901, respectively) when the optimized parameters were used. A 3sigma detection limit of 0.025 microg L(-1)0 Se(IV) was obtained at 30 s deposition time. The relative standard deviation was 4.0% on replicate runs (n = 12) for the determinations of 0.10 microg L(-1) Se(IV). Analytical results of natural water samples demonstrate that the proposed method is applicable to speciation analysis of Se(IV) and Se(VI).

  2. Determination of buprenorphine by differential pulse voltammetry on carbon paste electrode using SDS as an enhancement factor.

    Science.gov (United States)

    Behpour, Mohsen; Valipour, Akram; Keshavarz, Mahin

    2014-09-01

    In the present study, a facile electrochemical approach is proposed for the determination of buprenorphine (BPR) in the presence of sodium dodecyl sulfate (SDS). SDS was applied for amplification of oxidation signal. Carbon paste electrode (CPE) used as working electrode and cyclic voltammetry (CV), differential pulse voltammetry (DPV) and electrochemical impedance spectroscopy (EIS) were carried out in phosphate buffer solution (pH3.0). Under optimal experimental conditions, the oxidation current increased with the addition of BPR in the sample and two dynamic ranges obtained from 4.00 nM to 0.126 μM and from 0.126 to 0.317 μM by DPV and exhibited a low detection limit (LOD) of 1.33 nM (S/N=3). This offered method has been used for the determination of BPR in the real samples and has validated with the recovery test for BPR spiked urine samples. The result demonstrated that this method is a simple, sensitive, rapid, low-cost, and stable method for BPR detection.

  3. Determination of propylthiouracil in pharmaceuticals by differential pulse voltammetry using a cathodically pretreated boron-doped diamond electrode

    Energy Technology Data Exchange (ETDEWEB)

    Sartori, Elen Romao [Universidade Estadual de Londrina, PR (Brazil). Dept. de Quimica; Trench, Aline Barrios; Rocha-Filho, Romeu C.; Fatibello-Filho, Orlando, E-mail: bello@ufscar.br [Universidade Federal de Sao Carlos (UFSCAR), SP (Brazil). Dept. de Quimica

    2013-09-15

    A simple procedure is described for the determination of propylthiouracil (PTU) by differential pulse voltammetry (DPV) using a cathodically pretreated boron-doped diamond (BDD) electrode. Cyclic voltammetry studies indicate that the oxidation of PTU is irreversible at a peak potential of 1.42 V (vs. Ag/AgCl (3.0 mol L{sup -1} KCl)) in a Britton-Robinson (BR) buffer solution (pH 2.0). Under optimized conditions, the obtained analytical curve was linear (r = 0.9985) for the PTU concentration range of 1.0 to 29.1 {mu}mol L{sup -1} in a BR buffer solution (pH 2.0), with a detection limit of 0.90 {mu}mol L{sup -1}. The proposed method was successfully applied in the determination of PTU in pharmaceutical samples, with results in agreement at a 95% confidence level with those obtained using an official titration method. (author)

  4. Cd, Pb and Cu in spring waters of the Sibylline Mountains National Park (Central Italy, determined by square wave anodic stripping voltammetry

    Directory of Open Access Journals (Sweden)

    Truzzi C.

    2013-04-01

    Full Text Available Square wave anodic stripping voltammetry (SWASV was used to determine Cd, Pb and Cu in spring waters of the Sibylline Mountains National Park, Central Italy. Samples were collected from three different areas of the Park (Mount Bove North, Mount Bove South and Springs of River Nera during the period 2004-2011. Physical-chemical parameters were also determined to obtain a general characterization of the waters. Very low metal concentrations were observed (i.e., Cd 1.3±0.4 ng L-1, Pb 13.8±5.6 ng L-1, Cu 157±95 ng L-1, well below the legal limits and also below the medians of known Italian and European data. Comparing the three areas it was noted that waters from the area of the Nera Springs are the poorest in heavy metals and the richest in minerals, that conversely the waters of Mt. Bove North are the richest in heavy metals and the poorest in mineral salts, and finally that intermediate values both for heavy metals and mineral salts were observed for the waters of Mt. Bove South.

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

    Science.gov (United States)

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

    2017-04-15

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

  6. Ultramicroband array electrode. 1. Analysis of mercury in contaminated soils and flue gas exposed samples using a gold-plated iridium portable system by anodic stripping voltammetry.

    Science.gov (United States)

    Xiao, Li; Dietze, William; Nyasulu, Frazier; Mibeck, Blaise A F

    2006-07-15

    The applicability of a gold-plated iridium Nano-Band array ultramicroelectrode (6 microm by 0.2 microm, 64-microm interspacing, 100 electrode bands) in the analysis of mercury using a portable system is demonstrated by anodic stripping voltammetry in real-life samples. Optimized measurement parameters, 0.1 M HCl electrolyte, plating potential of 0 mV, and staircase scan mode were identified. The dynamic linear range is 10-180 ppb at 5-s deposition time with 1.5 microC of gold plated. The experimental detection limit for Hg2+ in 0.1 M HCl was 0.5 ppb at a deposition time of 4 min and a scan rate of 10 V/s. Real-life samples, such as flue gas exposed samples from flue gas simulators could be analyzed within 5 min using the method of standard additions. We identified a field-portable extraction procedure for soil samples using 1:1 concentrated HNO3/30% H2O2 mixture, compatible with ASV and the iridium electrode. The detection limit for soils is 1 ppm. The results obtained using ASV are in good agreement with reference values using cold vapor atomic absorption for the sample matrixes studied here. To our knowledge, this is the first mercury application using a reusable iridium array ultramicroelectrode. The portable potentiostat is less than 500 g, and together with the portable digestion method, makes the Nano-Band Explorer system field applicable.

  7. Optimization Central Composite Design for The Simultaneous Determination of Cd(II Ions in Fruit and Vegetable Samples by Adsorptive Stripping Voltammetry

    Directory of Open Access Journals (Sweden)

    Deswati

    2016-06-01

    Full Text Available This work describes a procedure for the simultaneous determination of cadmium in fruit and vegetable samples using adsorptive stripping voltammetry of complexes with calcon at a hanging mercury drop electrode (HMDE has been optimized using central composite design (CCD. The selection of the experimental conditions was made using experimental of the influence of several parameters were studied : variations of calcon concentration, pH, accumulation potential and accumulation time. The design experiment was a central composite design with 4 factors/variables, 3 levels and 31 treatment combinations. From analysis of variance, it was decided to accept the second-order model and the independent variable, concluded that a significant effect on the response variable (peak current. Based on data analysis with central composite design, the determination of cadmium obtained optimum conditions were : calcon concentration 0.8435 mM, pH 8.0047, accumulation potential -0.6346 Volt and accumulation time 81.85 seconds with a maximum peak current 61.8146 nA. At the optimum condition were obtained relative standard deviation 0.84%, recovery 98.88%, the linear range up to 110 µg/L, limit of detection 1.009 µg/L and LOQ 3.363 µg/L. The procedure was successfully applied to the determination of cadmium in fruit and vegetable samples without prior treatment.

  8. Determination of mercury in hair by square-wave anodic stripping voltammetry at a rotating gold disk electrode after microwave digestion.

    Science.gov (United States)

    East, Gaston A; Marinho, Epitácio P

    2005-03-01

    A simple and reliable method for the determination of mercury in hair on a rotating gold disk electrode using subtractive anodic stripping voltammetry without removal of oxygen is reported. Voltammetric and microwave parameters were optimized to obtain the best analytical results. Parameters such as supporting electrolyte concentration, influence of chloride in the Hg peak, deposition potential, scan rate, accumulation time, rotation rate, square-wave amplitude, and electrode conditioning were studied. Pressurized microwave-assisted digestion of hair, suitable for the accurate voltammetric determination of Hg, was evaluated using six acid mixtures and several time-power programs. Under the optimized conditions, no interference by copper, cadmium, lead, nickel, manganese, iron, or zinc was found at concentrations corresponding to their occurrence in normal hair. A calibration plot between 6,67 and 46,69 microg/L was linear, with r(2) better than 0.999. The detection limit for a deposition time of 60 s at 254 g was calculated as 1.92 nM (3omega). Validation of the method was demonstrated with the use of a certified reference sample of hair. Eight real samples of hair (four unexposed children and four exposed persons) were also analyzed.

  9. Determination of palladium(II) with alpha-(2-benzimidazolyl)-alpha',alpha''-(N-5-nitro-2-pyridylhydrazone)-toluene by adsorptive cathodic stripping voltammetry.

    Science.gov (United States)

    Kim, Sung-Ii; Cha, Ki-Won

    2002-06-10

    The determination of palladium(II) complexed with alpha-(2-benzimidazolyl)-alpha',alpha''-(N-5-nitro-2-pyridylhydrazone)-Toluene (BINPHT) was investigated by adsorptive cathodic stripping voltammetry using hanging mercury drop electrode. Palladium(II) in the sample solution can be determined in BINPHT and ethylenediaminetetraacetic acid (EDTA). Accumulation is achieved by adsorption of Pd(II)-BINPHT complex on a hanging mercury drop electrode. Optimal conditions were found to be: supporting electrolyte; 0.01 M sodium acetate buffer at pH 5.0, accumulation potential; -590 mV versus Ag/AgCl, accumulation time; 180 s, scan rate; 50 mV s(-1), concentration of BINPHT; 2x10(-5) M. The linear range of Pd(II) was observed over the concentration range 20-100 ng ml(-1) The detection limit (S/N=3) is 2 ng ml(-1). A good reproductivity shows RSD of 2.0% (n=7). This procedure offers high selectivity with the presence of EDTA masking some metallic ions. River water sample spiking with palladium was determined.

  10. Microdetermination of human serum albumin by differential pulse voltammetry at a L-cysteine modified silver electrode

    Indian Academy of Sciences (India)

    Liyuan Lu; Yanqin Zi; Hongling Wang

    2008-07-01

    A simple and highly sensitive electrochemical method for the determination of human serum albumin (HSA) using differential pulse voltammetry (DPV), based on a silver electrode modified with a self-assembled monolayer of L-cysteine, was developed. L-cysteine can be modified onto a silver electrode by covalent bonding through the sulfur to give stable and long-lived chemical electrodes. This electrode showed good sensitivity, selectivity, reproducibility and time stability in the determination of trace amounts of HSA by DPV technique. The detection limit can be as low as 4 × 10-17 mol/L. The optimum conditions for the determination were carefully investigated. This method had been applied to the determination of HSA in human serum samples. The results were in agreement with those given in standard method.

  11. Study on Water—Soluble Organic Reducing Substances.I.Determination of Organic Reducing Substances by Differential Pulse Voltammetry

    Institute of Scientific and Technical Information of China (English)

    WUYOU-XIAN; DINGCHANG-PU

    1991-01-01

    A new method was proposed for study of organic reducing substances in soils.According to the theoretical relationship between the voltammetric behaviors and reduction-oxidation reaction of reducing substances,the working conditions of differential pulse voltammetry (d.p.v.)for determining the organic reducing substances produced during the processes of the anaerobic decomposition of plant materials were established with a glass carbon electrode as working electrode,1M Ag-AgCl electrode with large area as reference electrode,0.2M NH4Ac as supporting from -0.5 to +1.2 voltage(vs.M Ag-AgCl).The peak current proportional to the concentration of reducing substances,and the characteristic peak potential of each organic reducing substance were regarded as the quantitative and qualitative base,respectively.These results obtained under the conditions mentioned above directly reflect both the reducing intensity and capacity of the organic reducing system in soils.

  12. Differential pulse cathodic stripping voltammetric determination of uranium with arsenazo-III at the hanging mercury dropping electrode

    Energy Technology Data Exchange (ETDEWEB)

    Kadi, M.W.; El-Shahawi, M.S. [Chemistry Dept., King Abdulaziz Univ., Jeddah (Saudi Arabia)

    2009-07-01

    An accurate, inexpensive and less laborious controlled adsorptive accumulation of uranium(VI)-arsenazo-III on a hanging mercury drop electrode (HMDE) has been developed for uranium(VI) determination. The method is based upon the collection of uranium(VI)-arsenazo-III complex at pH 5-6 at the HMDE and subsequent direct stripping measurement of the element in the nanomolar concentration level. The cathodic peak current (i{sub p,c}) of the adsorbed complex ions of uranium(VI) was measured at -0.35 V vs. Ag/AgCl reference electrode by differential pulse cathodic stripping voltammetry (DP-CSV), proceeded by an accumulation period of 150s2.5 in Britton-Robinson buffer of pH 5. The plot of the resulting i{sub p,c} vs. uranium(VI) concentration was linear in the range 2.1 x 10{sup -9} to 9.60 x 10{sup -7} mol L{sup -1} uranium(VI) and tended to level off at above 9.6 x 10{sup -7} mol L{sup -1}. The limits of detection and quantification of uranium(VI) were found to be 4.7 x 10{sup -10} and 1.5 x 10{sup -9} mol L{sup -1}, respectively. A relative standard deviation of {+-}2.39% (n = 5) at 8.5 x 10{sup -7} mol L{sup -1} uranium(VI) was obtained. The method was validated by comparing the results with that obtained by ICP-MS method with RSD less than {+-}3.3%. The method was applied successfully for the analysis of uranium in certified reference material (IAEA soil-7), and in phosphate fertilizers. (orig.)

  13. Amperometric detection of gold by differential pulse voltammetry using a DNA biosensor

    Institute of Scientific and Technical Information of China (English)

    GAN Ning; WANG Zhiying; XU Weiming; PAN Jianguo

    2007-01-01

    A DNA biosensor with [Ru(DA-bpy)3]Cl2(DA-bpy:4,4'-diamino-2,2'-bipyridine) (RuL) as the electrochemical probe was prepared on pyrolytic graphite electrode (PGE) through the supramolecular interaction between RuL complex and DNA template. Cyclic voltammetry of RuL-DNA film showed a pair of stable and reversible peaks corresponding to the Ru(Ⅲ)/Ru(Ⅱ) redox potential of-0.165 V versus Ag|AgCl in pH 7.4 0.1 mol· L-1 Tris-HCl. The electron transfer was expected across the double-strand DNA by an "electron tunneling" mechanism. When the DNA biosensor was immerged in gold (Ⅲ) buffer solution, the current peak signal (Ⅰ) of the RuL-DNA supramolecular depressed and △Ⅰ was linear in the concentration range of Au ion from 1 × 10-7 to 2 × 10-5 mol·L-1 with a regression coefficient of 0.9879. The detection limit was 5 × 10-8 mol·L-1. The developed procedures were applied to the analysis of synthetic samples of real materials with good sensitivity and selectivity.

  14. Electrochemical Investigation of Coenzyme Q10 on Silver Electrode in Ethanol Aqueous Solution and Its Determination Using Differential Pulse Voltammetry.

    Science.gov (United States)

    Li, Dan; Deng, Wei; Xu, Hu; Sun, Yinxing; Wang, Yuhong; Chen, Shouhui; Ding, Xianting

    2016-08-01

    The electrochemistry reduction of coenzyme Q10 (CoQ10) on silver electrodes has been investigated in mixed solvent containing 95 vol. % ethanol and 5 vol. % water. A combination of cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) is employed to explore the mechanism of redox processes of CoQ10 in the presence and absence of oxygen, respectively. It has been proved that the redox reaction of CoQ10 is highly dependent on the oxygen in the solution compared with that of CoQ0, which may be attributed to the isoprenoid side chain effect of CoQ10 Moreover, the effects of experimental variables such as electrolyte component, pH, temperature, and sonication time on the amperometric and potentiometric responses of CoQ10 are presented. The differential pulse voltammetry method has been developed for the quantification of the CoQ10 in the complex samples. Under the optimum conditions, the method is linear over the concentration range of 1.00 × 10(-7) to 1.00 × 10(-3) mol/L (8.63 × 10(-2) to 8.63 × 10(2) mg/kg). The limit of detection (3σ/k) is 3.33 × 10(-8) mol/L (2.88 × 10(-2) mg/kg). The recoveries of the spiked samples are between 91% and 108%. The presented method can be applied to the analysis of CoQ10 in real samples without any pretreatment.

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

    Directory of Open Access Journals (Sweden)

    Ali F. Alghamdi

    2017-09-01

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

  16. Is microwave digestion using TFM vessels a suitable preparation method for Pt determination in biological samples by adsorptive cathodic stripping voltammetry?

    Science.gov (United States)

    Haus, Nadine; Eybe, Tanja; Zimmermann, Sonja; Sures, Bernd

    2009-03-02

    The occurrence of Pt in environmental matrices is increasing since the introduction of automobile catalytic converters. Given that Pt is bioavailable and causes biological effects in plants and animals, respective biomonitoring programs are in high demand. But the analytical methods for conducting such programs have not yet been sufficiently established. Therefore, a study was carried out to develop a microwave digestion of biological samples, which allows a rapid determination of Pt by adsorptive cathodic stripping voltammetry. A high pressure microwave system was used and the digestion was performed in HNO(3) and HCl. After digestion the HNO(3) was evaporated with a microwave assisted vacuum concentration set. The study resulted in a procedural detection limit of 37.5 ng L(-1) and a relative standard deviation of 18%. A recovery study resulted in a Pt loss below 5%. The microwave assisted evaporation of HNO(3) performed satisfactorily and up to 500 mL of the sample solution could be used for the voltammetric measurements without any effect on the peak heights. A direct comparison of Pt concentrations conducted after microwave digestion and digestion by high pressure ashing showed similar values. However, these promising results were not persistent throughout the repeated analysis using the same Teflon vessels. The vessels did not endure the harsh conditions and due to aging processes the Pt loss consistently increased until Pt determination in environmental relevant concentrations became impossible. Quartz vessels could not be employed as an alternative to the Teflon vessels, due to a lack of compatibility with the vacuum concentration system. Consequently, the results of this paper show that there is a need for further development of more resistant Teflon materials.

  17. Simultaneous determination of three 5-nitroimidazoles in foodstuffs by differential pulse voltammetry and chemometrics

    Institute of Scientific and Technical Information of China (English)

    Yi Gui; Yong Nian Ni; Serge Kokot

    2011-01-01

    The voltammetric behaviour of three 5-nitroimidazoles, metronidazole, tinidazole and ornidazole, was investigated, and a method was developed for the simultaneous determination of these compounds, based on their reduction at a hanging mercury drop electrode (HMDE) in pH 8.95 buffer with differential pulse voltammetric (DPV) approach. Well defined voltammetric waves with peak potentials of -692, -640 and -652 mV were observed for these compounds, respectively. It is difficult to determine them individually from their mixtures without preseparation, for their voltammetric peaks overlapped seriously, so the chemometrics were used to resolve the overlapped voltammogram and quantify the mixtures. The proposed method was successfully applied to the determination of three 5-nitroimidazoles in milk and honey samples.

  18. Does morphine enhance the release of 5-hydroxytryptamine in the rat spinal cord? An in vivo differential pulse voltammetry study.

    Science.gov (United States)

    Chiang, C Y; Xiang, X K

    1987-05-19

    Differential pulse voltammetry used in combination with an electrochemically treated carbon fiber electrode allowed the detection of 5-hydroxyindoles (5-HI) in the dorsal horn of the urethane-anesthetized rat. Voltammograms were recorded every 3 min for up to 4 h. One component of the signal, peak 3, corresponding to 5-HI and uric acid was first identified separately in vitro as well as in vivo, and then further examined by means of systemic L- and D-trytophan administration and by local application of uricase, respectively. It was found that the height of peak 3 was unaffected by systemic morphine. Even following pretreatment with probenecid, the height of peak 3 was increased only 8.6-13.7% over that with saline, by morphine given either intraperitoneally or intracerebrally into the nucleus raphe magnus. However, these increments of peak 3 were not statistically significant. These findings suggest that the serotonin descending system is unlikely to play an important role in morphine analgesia.

  19. Simultaneous determination of paracetamol and ibuprofen in pharmaceutical samples by differential pulse voltammetry using a boron-doped diamond electrode

    Energy Technology Data Exchange (ETDEWEB)

    Lima, Amanda B.; Guimaraes, Carlos F.R.C.; Verly, Rodrigo M.; Silva, Leonardo M. da [Universidade Federal dos Vales do Jequitinhonha e Mucuri (UFVJM), Diamantina, MG (Brazil). Departamento de Quimica; Torres, Livia M.F.C.; Carvalho Junior, Alvaro D.; Santos, Wallans T. P. dos, E-mail: wallanst@ufvjm.edu.br [Universidade Federal dos Vales do Jequitinhonha e Mucuri (UFVJM), Diamantina, MG (Brazil). Departamento de Farmacia

    2014-03-15

    This work presents a simple, fast and low-cost methodology for the simultaneous determination of paracetamol (PC) and ibuprofen (IB) in pharmaceutical formulations by differential pulse voltammetry using a boron-doped diamond (BDD) electrode. A well-defined oxidation peak was observed using the BDD electrode for each analyte (0.85 V for PC and 1.72 V for IB (vs. Ag/AgCl)) in 0.1 mol L{sup -1} H{sub 2}SO{sub 4} solution containing 10% (v/v) of ethanol. Calibration curves for the simultaneous determination of PC and IB showed a linear response for both drugs in a concentration range of 20 to 400 μmol L{sup -1} (r{sup 2} = 0.999), with a detection limit of 7.1 μmol L{sup -1} for PC and 3.8 μmol L{sup -1} for IB. The addition-recovery studies in samples were about 100% and the results were validated by chromatographic methods. (author)

  20. Unveiling One-Dimensional Supramolecular Structures Formed Through π-π Stacking of Phenothiazines by Differential Pulse Voltammetry.

    Science.gov (United States)

    Carvalho, Fernando R; Zampieri, Eduardo H; Caetano, Wilker; Silva, Rafael

    2017-03-09

    Organic based nanomaterials can be self-assembled by strong and directional intermolecular forces as π-π interactions are. Experimental information about the stability, size and geometry of those formed structures are very limited for species which easily aggregates even at very low concentration. Differential pulse voltammetry can unveil the formation, growth and also the stability window of ordered one-dimensional, lamellar, self-aggregates formed by supramolecular π stacking of phenothiazines at micromolar (10-6 mol·L-1) concentration. The self-diffusion features of the species at different concentration were determined by DPV and used to probe the π staking process through the concept of the frictional resistance. It is observed that toluidine blue and methylene blue start to self-aggregate around 9 µmol·L-1 and the self-aggregation process occurs by one-dimensional growth as the concentration of the phenothiazines is increased up to around 170 µmol·L-1 for toluidine blue O and 200 µmol·L-1 for methylene blue. At higher concentration the aggregation process leads to structures with lower anisometry.

  1. Double preconcentration of trace amounts of cadmium in nail samples and measurement by differential pulse voltammetry.

    Science.gov (United States)

    Shahi, Somayeh; Nateghi, Mohammad Reza

    2015-04-01

    Cadion was coated on carbon powder and used as a solid phase for selective extraction and preconcentration of cadmium ions. Complexed cadmium ions were eluted from solid phase by 5 mL, nitric acid (2.0 M) with the flow rate of 2 mL min(-1).The resulted solution was used for accumulation of the cadmium metal at the surface of the carbon paste electrode at -1.3 V reduction potential. Finally, cadmium was reoxidized and the differential pulse voltammogram recorded at the potential range of -0.55 to -0.2 V. Calibration graph was plotted in the concentration range of 0.5-50 μg L(-1) of cadmium. Detection limit 0.06 μg L(-1) was calculated based on the 3 Sb/m. The RSD was 9.13 % (n = 4) for cadmium concentration of 10 μg L(-1) with preconcentration factor of 100. Method was successfully used for the determination of cadmium in finger nail samples and after spiking the samples, the recoveries were evaluated >96 %.

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

    Science.gov (United States)

    Economou, Anastasios; Voulgaropoulos, Anastasios

    2003-01-01

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

  3. Nonlinear Dynamics of Ultrashort Long-Range Surface Plasmon Polariton Pulses in Gold Strip Waveguides

    DEFF Research Database (Denmark)

    Lysenko, Oleg; Bache, Morten; Olivier, Nicolas

    2016-01-01

    We study experimentally and theoretically nonlinear propagation of ultrashort long-range surface plasmon polaritons in gold strip waveguides. The nonlinear absorption of the plasmonic modes in the waveguides is measured with femtosecond pulses revealing a strong dependence of the third......-order nonlinear susceptibility of the gold core on the pulse duration and layer thickness. A comprehensive model for the pulse duration dependence of the third-order nonlinear susceptibility is developed on the basis of the nonlinear Schrödinger equation for plasmonic mode propagation in the waveguides....... The model accounts for the intrinsic delayed (noninstantaneous) nonlinearity of free electrons of gold as well as the thickness of the gold film and is experimentally verified. The obtained results are important for the development of active plasmonic and nanophotonic components....

  4. Study of the short-term release of the ionic fraction of heavy metals from dental amalgam into synthetic saliva, using anodic stripping voltammetry with microelectrodes.

    Science.gov (United States)

    Sanna, Gavino; Pilo, Maria I; Piu, Paola C; Spano, Nadia; Tapparo, Andrea; Campus, Guglielmo G; Seeber, Renato

    2002-11-12

    The present paper describes a fast and reproducible procedure, employing differential pulse stripping analysis technique with graphite microelectrodes, for the quantitative evaluation of the ionic fraction of heavy metals (namely Hg, Cu, and Zn) released from dental amalgams into synthetic saliva during 6-90 h contact between amalgam and saliva, after completion of the dental restoration (short-term release). The Zn(2+) concentration was evaluated by linear calibration, whereas Cu(2+) and Hg(2+) contents were estimated by the standard additions method. While the concentration of Zn(2+) ion does not increase significantly anymore after a 6-h contact (values from 288+/-12 to 346+/-12 mugdm(-3) at time of contact from 6 to 90 h, respectively), in the same time interval the concentration of both Cu(2+) and Hg(2+) ions progressively increases (from 38+/-6 to 197+/-4 mugdm(-3) and from 15+/-3 to 101+/-2 mugdm(-3), respectively). The results of the release tests reveal that Hg concentration is at the highest level of risk (HBM III), as identified by the three human biomonitoring categories suggested by the Institut für Wasser-, Boden- und Lufthygiene des Umweltbundesamtes (Germany) for the estimation of potential harmful effects on health due to exposure to heavy metals.

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

    Science.gov (United States)

    Pomeroy, R. S.; And Others

    1989-01-01

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

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

    Science.gov (United States)

    Pomeroy, R. S.; And Others

    1989-01-01

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

  7. Direct Quantification of Cd(2+) in the Presence of Cu(2+) by a Combination of Anodic Stripping Voltammetry Using a Bi-Film-Modified Glassy Carbon Electrode and an Artificial Neural Network.

    Science.gov (United States)

    Zhao, Guo; Wang, Hui; Liu, Gang

    2017-07-03

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

  8. 差分脉冲伏安法测定卡托普利%Determination of Captopril by Using Differential Pulse Voltammetry

    Institute of Scientific and Technical Information of China (English)

    杜虹; 刘会; 赵常志

    2011-01-01

    A simple and sensitive electrochemical method was described by using differential pulse voltammetry for the determination of captopril (CPT). The method was based on the adsorption and oxidation of CPT at a gold electrode. The electrochemical behavior of CPT on the electrode was investigated with cyclic voltammetry and differential pulse voltammetry. Under the optimized experimental conditions, the voltammetric response was proportional to the concentration of CPT over the range from 0.217 to 3.04 mg/L with a correlation coefficient of 0. 9991, and the detection limit was estimated to be 0. 152 mg/L at a signal/noise ratio of 3. The relative standard deviation was less than 2.41% (n=5) and the recovery was in the range of 96.5%~101% for the determination of CPT in pharmaceutical samples.%本文基于金电极表面对巯基化合物的吸附作用,提出了一种简便灵敏的测定抗高血压药物卡托普利的新方法.研究了卡托普利在金电极上的伏安响应,优化了差分脉冲伏安法测定卡托普利的实验条件.研究结果表明:在0.217~3.04 mg/L的范围内,卡托普利的氧化峰电流与其浓度呈良好的线性关系,检出限为0.152 mg/L.测定药物中卡托普利的相对标准偏差小于2.41%,加标回收率为96.5%~101%.

  9. Determination of Silver(I) by Differential Pulse Voltammetry Using a Glassy Carbon Electrode Modified with Synthesized N-(2-Aminoethyl)-4,4′-Bipyridine

    Science.gov (United States)

    Radulescu, Maria-Cristina; Chira, Ana; Radulescu, Medeea; Bucur, Bogdan; Bucur, Madalina Petruta; Radu, Gabriel Lucian

    2010-01-01

    A new modified glassy carbon electrode (GCE) based on a synthesized N-(2-aminoethyl)-4,4′-bipyridine (ABP) was developed for the determination of Ag(I) by differential pulse voltammetry (DPV). ABP was covalently immobilized on GC electrodes surface using 4-nitrobenzendiazonium (4-NBD) and glutaraldehyde (GA). The Ag(I) ions were preconcentrated by chemical interaction with bipyridine under a negative potential (−0.6 V); then the reduced ions were oxidized by differential pulse voltammetry and a peak was observed at 0.34 V. The calibration curve was linear in the concentration range from 0.05 μM to 1 μM Ag(I) with a detection limit of 0.025 μM and RSD = 3.6%, for 0.4 μM Ag(I). The presence of several common ions in more than 125-fold excess had no effect on the determination of Ag(I). The developed sensor was applied to the determination of Ag(I) in water samples using a standard addition method. PMID:22163530

  10. Determination of Silver(I by Differential Pulse Voltammetry Using a Glassy Carbon Electrode Modified with Synthesized N-(2-Aminoethyl-4,4'-Bipyridine

    Directory of Open Access Journals (Sweden)

    Gabriel Lucian Radu

    2010-12-01

    Full Text Available A new modified glassy carbon electrode (GCE based on a synthesized N-(2-aminoethyl-4,4'-bipyridine (ABP was developed for the determination of Ag(I by differential pulse voltammetry (DPV. ABP was covalently immobilized on GC electrodes surface using 4-nitrobenzendiazonium (4-NBD and glutaraldehyde (GA. The Ag(I ions were preconcentrated by chemical interaction with bipyridine under a negative potential (−0.6 V; then the reduced ions were oxidized by differential pulse voltammetry and a peak was observed at 0.34 V. The calibration curve was linear in the concentration range from 0.05 μM to 1 μM Ag(I with a detection limit of 0.025 μM and RSD = 3.6%, for 0.4 μM Ag(I. The presence of several common ions in more than 125-fold excess had no effect on the determination of Ag(I. The developed sensor was applied to the determination of Ag(I in water samples using a standard addition method.

  11. Simultaneous determination of Mn(II), Cu(II) and Fe(III) as 2-(5'-bromo-2'-pyridylazo)-5-diethylaminophenol complexes by adsorptive cathodic stripping voltammetry at a carbon paste electrode.

    Science.gov (United States)

    Ghoneim, Enass M

    2010-07-15

    A simple and precise square-wave adsorptive cathodic stripping voltammetry (SW-AdCSV) method has been described for simultaneous determination of Mn(II), Cu(II) and Fe(III) in water samples using a carbon paste electrode. In 0.1 mol L(-1) acetate buffer (pH 5) containing 50 micromol L(-1) of 2-(5'-bromo-2'-pyridylazo)-5-diethylaminophenol (5-Br-PADAP), Mn(II), Cu(II) and Fe(III) were simultaneously determined as metal-complexes with 5-Br-PADAP following preconcentration onto the carbon paste electrode by adsorptive accumulation at +1.0V (vs. Ag/AgCl/3M KCl). Insignificant interference from various cations (K(+), Na(+), Mg(2+), Ca(2+), Al(3+), Bi(3+), Sb(3+), Se(4+), Zn(2+), Ni(2+), Co(2+), Cd(2+), Pb(2+), V(5+), Ti(4+) and NH(4)(+)), anions (HCO(3)(-), Cl(-), NO(3-), SO(4)(2-) and PO(4)(3-)) and ascorbic acid was noticed. Limits of detection of 0.066, 0.108 and 0.093 microg L(-1) and limits of quantitation of 0.22, 0.36 and 0.31 microg L(-1) Mn(II), Cu(II) and Fe(III), respectively, were achieved by the described method. The described stripping voltammetry method was successfully applied for simultaneous determination of Mn(II), Cu(II) and Fe(III) in ground, tap and bottled natural water samples. Copyright 2010 Elsevier B.V. All rights reserved.

  12. Cyclic Voltammetry.

    Science.gov (United States)

    Evans, Dennis H.; And Others

    1983-01-01

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

  13. Cyclic Voltammetry.

    Science.gov (United States)

    Evans, Dennis H.; And Others

    1983-01-01

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

  14. Highly sensitive and selective determination of pyrazinamide at poly-L-methionine/reduced graphene oxide modified electrode by differential pulse voltammetry in human blood plasma and urine samples.

    Science.gov (United States)

    Cheemalapati, Srikanth; Devadas, Balamurugan; Chen, Shen-Ming

    2014-03-15

    In this current study we used electrochemically active film which contains poly-L-methionine (PMET) and electrochemically reduced graphene oxide (ERGO) on glassy carbon electrode (GCE) for pyrazinamide (PZM) detection. The electrocatalytic response of analyte at PMET/ERGO/GCE film was measured using both cyclic voltammetry (CV) and differential pulse voltammetry (DPV). In addition, electrochemical impedance studies revealed that the smaller R(ct) value observed at PMET/ERGO film modified GCE which authenticates its good conductivity and faster electron transfer rate. The prepared PMET/ERGO/GCE film exhibits excellent DPV response towards PZM and the reduction peak current increased linearly with respect to PZM concentration in the linear range between 0.4 μM to 1129 μM with a sensitivity of 0.266 μA μM(-1) cm(-2). Real sample studies were carried out in human blood plasma and urine samples, which offered good recovery and revealed the promising practicality of the sensor for PZM detection. The proposed sensor displayed a good selectivity, repeatability, sensitivity with appreciable consistency and good reproducibility. In addition, the proposed electrochemical sensor showed good results towards the commercial pharmaceutical PZM samples.

  15. Determination of Total Germanium in Chinese Herbal Remedies by Square-Wave Catalytic Adsorptive Cathodic Stripping Voltammetry at an Improved Bismuth Film Electrode

    Directory of Open Access Journals (Sweden)

    Shangwei Zhong

    2013-01-01

    Full Text Available A catalytic adsorptive cathodic stripping voltammetric method on an improved bismuth film electrode (BiFE for the determination of trace germanium in the presence of pyrogallol has been investigated. A well-defined and sensitive stripping peak of Ge(IV-pyrogallol complex was observed at −0.79 V (versus SCE in a 0.1 M acetate buffer solution (pH 4.8 at a deposition potential of −0.34 V. The reduction current is catalytically enhanced by adding KBrO3. The experimental variables and potential interference were studied. Compared with the BiFE plated in the solution prepared based on HAc-NaAc without trisodium citrate, the improved BiFE electrodeposited in the solution of HAc-NaAc containing trisodium citrate displayed a better electroanalytical performance for the determination of germanium(IV. Under the optimized conditions, the detection limit of Ge(IV was 60 ng L−1, and the relative standard deviation (RSD was 3.73% at 5 μg L−1 level (n=9. This method was successfully applied to determine the total germanium in several Chinese herbal remedies.

  16. Design of heavy metal detector for anodic stripping voltammetry%水质阳极伏安法重金属检测仪设计

    Institute of Scientific and Technical Information of China (English)

    郑英; 王迷迷; 李香菊; 张立珍

    2015-01-01

    This paper designs an instrument for the detection of heavy metals in water by anodic voltammetry.In this paper,we analyze the principle of the detection,design the hardware circuit,the software programming and the prototype.The instrument can detect the concentration of copper,lead,cadmium, zinc and other heavy metals in the water environment,and the measurement data is stored and printed.The system has the advantages of good sensitivity,high efficiency,high efficiency,high information storage capacity, friendly man-machine interface and so on.%本文设计一种采用阳极伏安法对水环境重金属进行检测的仪器.本文分析了伏安法检测原理,设计了硬件电路,软件编程并制作样机.通过该仪器能够检测水环境中的铜、铅、镉、锌等多种重金属的浓度,并对测量数据进行存储和打印.通过对多种重金属进行测试验证,该系统具有灵敏度好、效率高、信息存储量大,友好的人机界面等特点,具有良好的重金属检测功能.

  17. A Simple, Fast, and Inexpensive Simultaneous Determination of Trace Bismuth(III) and Lead(II) in Water Samples by Adsorptive Stripping Voltammetry

    Science.gov (United States)

    Adamczyk, Marzena

    2017-01-01

    A simple, fast, and inexpensive voltammetric method for the simultaneous determination of trace bismuth(III) and lead(II) using (Hg(Ag)FE) as a working electrode was optimized. For adsorptive stripping voltammetric determination of Bi(III) and Pb(II) in a single scan, the cupferron was applied as a complexing agent. Experimental conditions under which these elements can be simultaneously detected include 0.1 mol L−1 acetate buffer (pH = 4.6), 1 × 10−4 mol L−1 cupferron, accumulation potential −0.05 V, and accumulation time 30 s. The experiments were performed without deaeration of the solutions. The calibration graph was linear from 2 × 10−9 mol L−1 to 1 × 10−7 mol L−1 for the simultaneous presence of bismuth and lead. The detection limits for preconcentration time of 30 s were 6.7 × 10−10 mol L−1 and 8.8 × 10−10 mol L−1 for bismuth and lead, respectively. The application of this procedure was tested by analyzing certified reference material (SPS-WW1 Wastewater) and Lake Zemborzyce water (eastern areas of Poland).

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

    Science.gov (United States)

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

    2017-05-01

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

  19. Simultaneous determination of Cd(II) and Cu(II) using stripping voltammetry in groundwater, soil and Alhagi maurorum plants in industrial and urban areas in Northern Border, Saudi Arabia with luminol as a chelating agent.

    Science.gov (United States)

    Al-Hossainy, Ahmed Farouk

    2015-01-01

    The cathodic stripping voltammetry of Cu(II) and Cd(II) speciation was re-optimized by using luminol (Lu) in groundwater, soil and Alhagi maurorum plants, finding differences with the pre-existing method and a different interpretation for the electroactive species. The main findings are that optimum sensitivity is obtained at 0.3-142.5 ng/mL and 0.065-60.0 ng/mL for copper and cadmium, respectively, that the complexes responsible for adsorption on the electrode are CuLu and CdLu, and that the sensitivity of the method is much improved in the absence of dissolved oxygen. The limit of detection of the method was 0.011 ± 0.001 ng/mL for Cu(II) and 0.013 ± 0.001 ng/mL for Cd(II). The interference of some common ions: Cr(III), Fe(III), Zn(II), Ni(II), Co(II) and Mo(II) was studied. It was concluded that application of this method for the determination of Cu(II) and Cd(II) in groundwater, soil and Alhagi maurorum plants led to satisfactory results.

  20. The automatic heavy metals monitoring system of water based on linear sweep stripping voltammetry%基于溶出伏安法的水质重金属自动监测系统

    Institute of Scientific and Technical Information of China (English)

    赵学亮; 史云

    2011-01-01

    An automatic monitoring system is developed for detecting heavy metals in water, based on linear sweep stripping voltammetry. Automatic determination of trace lead, zinc, arsenic and antimony are realized. The hardware and software design is introduced. Meanwhile, the recognition and correction method of false point, quantitative analysis method and parameter configuration of accumulation potential etc are introduced in detail. The result of experimental test shows that the system features lower detection limit, quick response and high automation etc, and has wide application prospect.%基于线性扫描溶出伏安法研制了一套水质重金属自动监测系统,实现了水中铅、锌、砷、锑重金属元素的自动监测.介绍了系统的硬、软件设计,详细阐述了数据采集中虚假点识别和纠正算法、定量分析方法和富集电位等参数的配置.实验表明,该仪器具有检出限低、响应快、自动化程度高等优点,具有一定应用前景.

  1. Simultaneous determination of mycophenolate mofetil and its active metabolite, mycophenolic acid, by differential pulse voltammetry using multi-walled carbon nanotubes modified glassy carbon electrode.

    Science.gov (United States)

    Madrakian, Tayyebeh; Soleimani, Mohammad; Afkhami, Abbas

    2014-09-01

    A highly sensitive electrochemical sensor for the simultaneous determination of mycophenolate mofetil (MPM) and mycophenolic acid (MPA) was fabricated by multi-walled carbon nanotubes modified glassy carbon electrode (MWCNTs/GCE). The electrochemical behavior of these two drugs was studied at the modified electrode using cyclic voltammetry and adsorptive differential pulse voltammetry. MPM and MPA were oxidized at the GCE during an irreversible process. DPV analysis showed two oxidation peaks at 0.87V and 1.1V vs. Ag/AgCl for MPM and an oxidation peak at 0.87V vs. Ag/AgCl for MPA in phosphate buffer solution of pH5.0. The MWCNTs/GCE displayed excellent electrochemical activities toward oxidation of MPM and MPA relative to the bare GCE. The experimental design algorithm was used for optimization of DPV parameters. The electrode represents linear responses in the range 5.0×10(-6) to 1.6×10(-4)molL(-1) and 2.5×10(-6)molL(-1) to 6.0×10(-5)molL(-1) for MPM and MPA, respectively. The detection limit was found to be 9.0×10(-7)molL(-1) and 4.0×10(-7)molL(-1) for MPM and MPA, respectively. The modified electrode showed a good sensitivity and stability. It was successfully applied to the simultaneous determination of MPM and MPA in plasma and urine samples.

  2. Assessment of accuracy and precision in speciation analysis by competitive ligand equilibration-cathodic stripping voltammetry (CLE-CSV) and application to Antarctic samples

    Energy Technology Data Exchange (ETDEWEB)

    Monticelli, Damiano, E-mail: damiano.monticelli@uninsubria.it [Dipartimento di Scienze Chimiche e Ambientali, Universita degli Studi dell' Insubria - sede di Como, via Valleggio 11 22100 Como (Italy); Dossi, Carlo; Castelletti, Alessio [Dipartimento di Scienze Chimiche e Ambientali, Universita degli Studi dell' Insubria - sede di Como, via Valleggio 11 22100 Como (Italy)

    2010-08-24

    The analytical performances of Competitive Ligand Equilibration with Cathodic Stripping Voltammetric detection of the labile fraction (CLE-CSV) were assessed. This speciation method enables the concentration of natural ligand(s) and their conditional stability constants for the complexation of the investigated metal to be determined through thermodynamic considerations. Literature data were discussed and general trends in the precision of the determined parameters identified: ligand concentrations were affected, on average, by a 10% relative percentage standard deviation (RSD%), whereas conditional stability constants showed much lower precision, with an average RSD% of 50%. New experimental data were collected to obtain a complete assessment of accuracy and precision attainable for the determination of strong ligands at the ultra trace level, enabling the whole protocol to be evaluated. Firstly, the side reaction coefficient alpha for the formation of the complex between the added ligand and the investigated metal ({alpha}{sub CuL}) was determined. The method was subsequently applied to the analysis of solution containing ligand at trace levels (5-50 nM) with known complexing characteristics. Copper was used as the model metal ion and ethylenediaminetetraacetic acid (EDTA) and diethylenetriaminepentaacetic acid (DTPA) as the model ligands. Results evidenced that the CLE-CSV protocol is not affected by systematic errors in the determination of both ligand concentration and the conditional stability constants. Good precision is obtained for ligand concentrations, with an average relative standard deviation (RSD%) of 5%; an average RSD% of 23% was calculated for the conditional stability constants. Including the contribution of the uncertainty in the value of {alpha}{sub CuL} in the evaluation of the uncertainty in the latter parameter increased the RSD% up to 40%. The CLE-CSV protocol was subsequently applied to the detection of strong ligands in water samples

  3. Assessment of accuracy and precision in speciation analysis by competitive ligand equilibration-cathodic stripping voltammetry (CLE-CSV) and application to Antarctic samples.

    Science.gov (United States)

    Monticelli, Damiano; Dossi, Carlo; Castelletti, Alessio

    2010-08-24

    The analytical performances of Competitive Ligand Equilibration with Cathodic Stripping Voltammetric detection of the labile fraction (CLE-CSV) were assessed. This speciation method enables the concentration of natural ligand(s) and their conditional stability constants for the complexation of the investigated metal to be determined through thermodynamic considerations. Literature data were discussed and general trends in the precision of the determined parameters identified: ligand concentrations were affected, on average, by a 10% relative percentage standard deviation (RSD%), whereas conditional stability constants showed much lower precision, with an average RSD% of 50%. New experimental data were collected to obtain a complete assessment of accuracy and precision attainable for the determination of strong ligands at the ultra trace level, enabling the whole protocol to be evaluated. Firstly, the side reaction coefficient alpha for the formation of the complex between the added ligand and the investigated metal (alpha(CuL)) was determined. The method was subsequently applied to the analysis of solution containing ligand at trace levels (5-50 nM) with known complexing characteristics. Copper was used as the model metal ion and ethylenediaminetetraacetic acid (EDTA) and diethylenetriaminepentaacetic acid (DTPA) as the model ligands. Results evidenced that the CLE-CSV protocol is not affected by systematic errors in the determination of both ligand concentration and the conditional stability constants. Good precision is obtained for ligand concentrations, with an average relative standard deviation (RSD%) of 5%; an average RSD% of 23% was calculated for the conditional stability constants. Including the contribution of the uncertainty in the value of alpha(CuL) in the evaluation of the uncertainty in the latter parameter increased the RSD% up to 40%. The CLE-CSV protocol was subsequently applied to the detection of strong ligands in water samples collected in

  4. Determination of Trace Amounts of Gold in Environmental Samples by Adsorptive Stripping Voltammetry of Its Complex with Rhodamine Using Osc-Pls

    Directory of Open Access Journals (Sweden)

    A. Akrami

    2012-11-01

    Full Text Available The multivariate calibration method was applied for the determination of trace amounts of gold based on a hanging mercury drop electrode (HMDE in the presence of rhodanine, followed by reduction of adsorbed gold by voltammetric scan using differential pulse modulation The optimum experimental conditions are: rhodanine concentration of 0.20 mg mL-1, pH 5.0, accumulation potential of -600 mV versus Ag/AgCl, accumulation time of 100 sec, scan rate of 30 mV s-1 and pulse height of 100 mV. The calibration matrix for partial least squares (PLS regression was designed with 9 samples. Orthogonal signal correction (OSC is a preprocessing technique used for removing the information unrelated to the target variables based on constrained principal component analysis. OSC is a suitable preprocessing method for PLS calibration without loss of prediction capacity using electrochemical method. The RMSEP for gold determination with PLS and OSC-PLS were 8.51 and 1.94, respectively. This procedure allows the determination of gold in synthetic and real samples with good reliability of the determination. 

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

    Science.gov (United States)

    Asadpour-Zeynali, Karim; Mollarasouli, Fariba

    2017-06-15

    This work introduces a new electrochemical sensor based on polyvinyl pyrrolidone capped CoFe2O4@CdSe core-shell modified electrode for a rapid detection and highly sensitive determination of rifampicin (RIF) by square wave adsorptive stripping voltammetry. The new PVP capped CoFe2O4@CdSe with core-shell nanostructure was synthesized by a facile synthesis method for the first time. PVP can act as a capping and etching agent for protection of the outer surface nanoparticles and formation of a mesoporous shell, respectively. Another important feature of this work is the choice of the ligand (1,10-phenanthroline) for precursor cadmium complex that works as a chelating agent in order to increase optical and electrical properties and stability of prepared nanomaterial. The nanoparticles have been characterized by field emission scanning electron microscopy (FESEM), transmission electron microscope (TEM), energy dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), UV-vis, photoluminescence (PL) spectroscopy, FT-IR, and cyclic voltammetry techniques. The PL spectroscopy study of CoFe2O4@CdSe has shown significant PL quenching by the formation of CoFe2O4 core inside CdSe, this shows that CoFe2O4 NPs are efficient electron acceptors with the CdSe. It is clearly observed that the biosensor can significantly enhance electrocatalytic activity towards the oxidation of RIF, under the optimal conditions. The novelty of this work arises from the new synthesis method for the core-shell of CoFe2O4@CdSe. Then, the novel electrochemical biosensor was fabricated for ultra-trace level determination of rifampicin with very low detection limit (4.55×10(-17)M) and a wide linear range from 1.0×10(-16) to 1.0×10(-7)M. The fabricated biosensor showed high sensitivity and selectivity, good reproducibility and stability. Therefore, it was successfully applied for the determination of ultra-trace RIF amounts in biological and pharmaceutical samples with satisfactory recovery data.

  6. Determination of aluminium in water samples by adsorptive cathodic stripping voltammetry in the presence of pyrogallol red and a quaternary ammonium salt.

    Science.gov (United States)

    Arancibia, Verónica; Muñoz, Carolina

    2007-09-30

    A fast, sensitive and selective method for the determination of aluminium based on the reaction of the metal with pyrogallol red (PR) in the presence of tetrabutylammonium tetrafluoroborate (TBATFB) to form an Al(PR)(3)x9TBATFB complex which is adsorbed on the mercury electrode is presented. Under these conditions complexation of aluminium is rapid and no waiting period or heating of the sample is required. The reduction current of the accumulated complex is measured by scanning the potential in the cathodic direction. The variation of peak current with pH, adsorption time, adsorption potential, ligand and quaternary ammonium salt concentration, and some instrumental parameters, such as stirring rate in the accumulation stage, and step amplitude, pulse amplitude and step duration while obtaining the square wave voltamperograms were optimized. The best experimental parameters were pH 8.5, (NH(4)Ac-NH(3) buffer), C(PR)=25mumolL(-1), C(TBATFB) over 75mumolL(-1), t(ads)=60s, and E(ads)=-0.60V versus Ag/AgCl. A linear response is observed over the 0.0-30.0mugL(-1) concentration range, with a detection limit of 1.0mugL(-1). Reproducibility for 9.0mugL(-1) aluminium solution was 2.3% (n=6). Synthetic sea water and sea water reference material CRM-SW were used for validation measurements. Aluminium in urine samples of a volunteer who ingested 800mg of Al(OH)(3) was analyzed.

  7. Speciation analysis of aluminium(III) in natural waters and biological fluids by complexing with various catechols followed by differential pulse voltammetry detection.

    Science.gov (United States)

    Liu, Jian; Bi, Shuping; Yang, Li; Gu, Xiaodong; Ma, Pengju; Gan, Ning; Wang, Xianlong; Long, Xiufeng; Zhang, Fuping

    2002-12-01

    The biological effects of aluminium have received much attention in recent years. Speciation of Al is of basic relevance as it concerns its reactivity and bioavailability. A differential pulse voltammetry (DPV) procedure is proposed for speciation analysis of Al(III) in natural waters and biological fluids using six catechols (L-dopa, dopamine, epinephrine, norepinephrine, caffeic acid and o-benzenediol) as electroactive ligands. The decrease of the DPV anodic peak current for each catechol ligand is linear with the increase of Al concentration. This speciation analysis idea is based on the measurement of the complexation capacity, namely, different affinities of Al(III) for catechols and organic ligands under two pH conditions. The labile monomeric Al fraction (mainly inorganic aluminium) is determined at pH 4.6, while the total monomeric Al fraction is determined at pH 8.5. The principle for Al(III) speciation analysis by an electrochemical method is discussed. This sensitive and simple fractionation method is successfully applied to the speciation analysis of Al in natural waters and the results agree well with those of Driscoll's method. The speciation analysis of Al in biological fluids is also explored and the results are compared with those obtained by ultrafiltration and dialysis. Compared with other speciation protocols the electrochemical method possesses some remarkable advantages: rapidity, high sensitivity, cheap instrumentation and a simple operation procedure.

  8. Application of matrix solid-phase dispersion to the propham and maleic hydrazide determination in potatoes by differential pulse voltammetry and HPLC.

    Science.gov (United States)

    Arribas, Alberto Sánchez; Bermejo, Esperanza; Chicharro, Manuel; Zapardiel, Antonio

    2007-01-15

    The application of the matrix solid-phase dispersion (MSPD) process as sample treatment in connection with the electrochemical detection is studied for the first time. For this purpose, a novel methodology is introduced for the extraction of propham and maleic hydrazide herbicides from potatoes samples based in the MSPD process prior to their electrochemical detection. Potato samples disruption was done by blending them with C(8) bonded-phase and selective herbicide extraction was achieved by successive treatment of the blended with 50mM phosphate buffer pH 7.4 (for maleic hydrazide) and methanol (for propham). The extraction procedure efficiency was estimated using differential pulse voltammetry in potato samples spiked with the herbicides yielding recovery values of 98% and 68% for propham and maleic hydrazide, respectively. No significant adverse effect of the MSPD process was observed on the herbicides electrochemical signals. For comparison, recovery studies using HPLC with UV detection were carried out and a good correlation in the results obtained by using both techniques was observed.

  9. Platinum(II Complexes with Tetradentate Schiff Bases as Ligands: Synthesis, Characterization and Detection of DNA Interaction by Differential Pulse Voltammetry

    Directory of Open Access Journals (Sweden)

    Lijun Li

    2012-01-01

    Full Text Available Five sterically hindered platinum(II complexes with tetradentate schiff bases as ligands, [Pt(L] (L= N,N′-bisalicylidene-1,2-ethylenediamine (L1, N,N′-bisalicylidene-1,2-cyclohexanediamine (L2, N,N′-bis(5-hydroxyl-salicylidene-1,2-cyclohexanediamine (L3, N,N′-bisalicylidene-1,2-diphenyl-ethylenediamine (L4 and N,N′-bis(3-tert-butyl-5-methyl-salicylidene-1,2-diphenylethylenediamine (L5 have been synthesized and characterized by IR spectroscopy and elemental analysis. The sterical hindrance of antitumor drug candidates potentially makes them less susceptible to deactivation by sulphur containing proteins and helping to overcome resistance mechanisms. The interaction of these metal complexes with fish sperm single-stranded DNA (ssDNA was studied electrochemically based on the oxidation signals of guanine and adenine. Differential pulse voltammetry was employed to monitor the DNA interaction in solution by using renewable pencil graphite electrode. The results indicate that ligands with different groups can strongly affect the interaction between [Pt(L] complexes and ssDNA due to sterical hindrances and complex [Pt(L1] has the best interaction with DNA among the five complexes.

  10. Single-Use Disposable Electrochemical Label-Free Immunosensor for Detection of Glycated Hemoglobin (HbA1c) Using Differential Pulse Voltammetry (DPV).

    Science.gov (United States)

    Molazemhosseini, Alireza; Magagnin, Luca; Vena, Pasquale; Liu, Chung-Chiun

    2016-07-01

    A single-use disposable in vitro electrochemical immunosensor for the detection of HbA1c in undiluted human serum using differential pulse voltammetry (DPV) was developed. A three-electrode configuration electrochemical biosensor consisted of 10-nm-thin gold film working and counter electrodes and a thick-film printed Ag/AgCl reference electrode was fabricated on a polyethylene terephthalate (PET) substrate. Micro-fabrication techniques including sputtering vapor deposition and thick-film printing were used to fabricate the biosensor. This was a roll-to-roll cost-effective manufacturing process making the single-use disposable in vitro HbA1c biosensor a reality. Self-assembled monolayers of 3-Mercaptopropionic acid (MPA) were employed to covalently immobilize anti-HbA1c on the surface of gold electrodes. Electrochemical impedance spectroscopy (EIS) and X-ray photoelectron spectroscopy (XPS) confirmed the excellent coverage of MPA-SAM and the upward orientation of carboxylic groups. The hindering effect of HbA1c on the ferricyanide/ferrocyanide electron transfer reaction was exploited as the HbA1c detection mechanism. The biosensor showed a linear range of 7.5-20 µg/mL of HbA1c in 0.1 M PBS. Using undiluted human serum as the test medium, the biosensor presented an excellent linear behavior (R² = 0.999) in the range of 0.1-0.25 mg/mL of HbA1c. The potential application of this biosensor for in vitro measurement of HbA1c for diabetic management was demonstrated.

  11. Determination of Zinc(II) Ions Released into Artificial Digestive Juices from Culinary-Medicinal Button Mushroom, Agaricus bisporus (Agaricomycetidae), Biomass of In Vitro Cultures Using an Anodic Stripping Voltammetry Method.

    Science.gov (United States)

    Kala, Katarzyna; Muszynska, Bozena; Zajac, Magdalena; Krezalek, Remigiusz; Opoka, Wlodzimierz

    2016-01-01

    Zinc is one of those microelements that are essential for the proper functioning of the human body and must be supplemented in our food at a daily dose of 15 mg. It is well known that mushrooms accumulate elements; thus, in order to determine the extent of accumulation and the level of zinc released from mushrooms, in vitro cultures of Agaricus bisporus were established. The cultures were run on a modified Oddoux medium (a control culture) as well as on the same medium with the addition of zinc hydroaspartate (100 and 200 mg/L) and zinc sulfate (87.23 and 174.47 mg/L). These compounds were chosen to help estimate which form, organic or inorganic, results in a better assimilation of zinc(II) ions by biomass. As the next step, the level of zinc(II) ions released from the lyophilized biomass of in vitro cultures to the digestive juices, under thermal conditions of the human body (37°C), was determined. For this purpose, artificial digestive juices, imitating the composition of human digestive juices, were used. For determination of zinc(II) ions in the digestive tract, an anodic stripping voltammetry method was employed. The amount of zinc released into artificial saliva over 1 minute varied from 0.15 mg/100 g d.w. in the control culture to 2.35 mg/100 g d.w. in the biomass in the medium to which 200 mg/L zinc hydroaspartate had been added. Values were higher in gastric juice and depended on incubation time (2.66 to 30.63 mg/100 g d.w.). In intestinal juice, the highest value of the released zinc grew to 24.20 mg/100 g d.w. (biomass of A. bisporus in vitro cultures in medium with the addition of 200 mg/L zinc hydroaspartate). Total average amount of zinc released into artificial digestive juices was the highest (56.26 mg/100 g d.w.) from A. bisporus biomass of in vitro cultures in the medium to which 200 mg/L zinc hydroaspartate had been added.

  12. APPLICATION OF PRINCIPAL COMPONENTS ANALYSIS IN THE STUDY OF ADSORPTIVE VOLTAMMETRY OF METALICS IONS

    Directory of Open Access Journals (Sweden)

    Leandra de Oliveira Cruz da Silva

    2010-01-01

    Full Text Available The adsorptive stripping voltammetry with differential pulse cathodic through the use of a mixture of complexing agents dimethylglyoxime and oxine was used for an exploratory study simultaneously of ions cadmium, cobalt, copper, nickel, lead and zinc. Were obtained voltammograms of the 64 individual solutions used in planning and current data were submitted to principal component analysis (PCA, allowing to characterize the trends of the solutions of metal ions studied. The system can be described in eight principal components that explained 98.32% of variance. Since the first three principal components accumulated approximately 85.46% of the total variance.

  13. High-voltage isolation transformer for sub-nanosecond rise time pulses constructed with annular parallel-strip transmission lines.

    Science.gov (United States)

    Homma, Akira

    2011-07-01

    A novel annular parallel-strip transmission line was devised to construct high-voltage high-speed pulse isolation transformers. The transmission lines can easily realize stable high-voltage operation and good impedance matching between primary and secondary circuits. The time constant for the step response of the transformer was calculated by introducing a simple low-frequency equivalent circuit model. Results show that the relation between the time constant and low-cut-off frequency of the transformer conforms to the theory of the general first-order linear time-invariant system. Results also show that the test transformer composed of the new transmission lines can transmit about 600 ps rise time pulses across the dc potential difference of more than 150 kV with insertion loss of -2.5 dB. The measured effective time constant of 12 ns agreed exactly with the theoretically predicted value. For practical applications involving the delivery of synchronized trigger signals to a dc high-voltage electron gun station, the transformer described in this paper exhibited advantages over methods using fiber optic cables for the signal transfer system. This transformer has no jitter or breakdown problems that invariably occur in active circuit components.

  14. Trends in speciation analysis of some heavy metals in serum of patients with chronic hepatitis C and chronic hepatitis B using differential pulse adsorptive stripping voltammetric measurement and atomic absorption spectrophotometry.

    Science.gov (United States)

    Rashed, Mohamed Nageeb; Ahmed, Mahasen Mohamed; Al-Hossainy, Ahmed Farouk; Abd, Safaa Mahmoud

    2010-04-01

    The relationships between chronic liver diseases and trace heavy metal contents in blood are debatable and have not been understood clearly. The present study is undertaken to determine Co, Fe, and Ni concentrations in sera from viral hepatitis patients. In all eighty patients with chronic hepatitis (B, C) and 29 healthy individuals were chosen for this study. Donors were selected from different environmental areas, including Aswan, Kom Ombo, and Edfu as polluted areas, and Daraw as an unpolluted area. Co, Fe, and Ni concentrations in patient and healthy blood serum were measured by two different analytical techniques: differential pulse adsorptive stripping voltammetry (DPA(d)SV) and atomic absorption spectrophotometer (AAS). The results reveal that Fe is present in higher level in the blood serum of hepatitis patients than in the healthy control, whereas Co and Ni showed the opposite trend. Hepatitis patients from Edfu area exhibited higher Fe level in their serum than those from the other areas, while hepatitis patients and healthy control from Daraw area (free from pollution) exhibited the lowest metal values. Patients with hepatitis C show lower levels of Co, Ni, and Fe in their serum than those with hepatitis B. A comparative study was carried out between the results using DPA(d)SV and AAS techniques, which are in very good agreements. 2009 Elsevier GmbH. All rights reserved.

  15. Comparative evaluation of scanned stripping techniques: SSCP vs. SSV

    NARCIS (Netherlands)

    Town, R.M.; Leeuwen, van H.P.

    2006-01-01

    The characteristic features of scanned deposition potential curves constructed from stripping chronopotentiometry (SSCP) and various modes of stripping voltammetry (SSV) are critically evaluated. The strengths and weaknesses of each method for identification of metal ion speciation features and susc

  16. Application of neural networks to digital pulse shape analysis for an array of silicon strip detectors

    Energy Technology Data Exchange (ETDEWEB)

    Flores, J.L. [Dpto de Ingeniería Eléctrica y Térmica, Universidad de Huelva (Spain); Martel, I. [Dpto de Física Aplicada, Universidad de Huelva (Spain); CERN, ISOLDE, CH 1211 Geneva, 23 (Switzerland); Jiménez, R. [Dpto de Ingeniería Electrónica, Sist. Informáticos y Automática, Universidad de Huelva (Spain); Galán, J., E-mail: jgalan@diesia.uhu.es [Dpto de Ingeniería Electrónica, Sist. Informáticos y Automática, Universidad de Huelva (Spain); Salmerón, P. [Dpto de Ingeniería Eléctrica y Térmica, Universidad de Huelva (Spain)

    2016-09-11

    The new generation of nuclear physics detectors that used to study nuclear reactions is considering the use of digital pulse shape analysis techniques (DPSA) to obtain the (A,Z) values of the reaction products impinging in solid state detectors. This technique can be an important tool for selecting the relevant reaction channels at the HYDE (HYbrid DEtector ball array) silicon array foreseen for the Low Energy Branch of the FAIR facility (Darmstadt, Germany). In this work we study the feasibility of using artificial neural networks (ANNs) for particle identification with silicon detectors. Multilayer Perceptron networks were trained and tested with recent experimental data, showing excellent identification capabilities with signals of several isotopes ranging from {sup 12}C up to {sup 84}Kr, yielding higher discrimination rates than any other previously reported.

  17. Application of neural networks to digital pulse shape analysis for an array of silicon strip detectors

    Science.gov (United States)

    Flores, J. L.; Martel, I.; Jiménez, R.; Galán, J.; Salmerón, P.

    2016-09-01

    The new generation of nuclear physics detectors that used to study nuclear reactions is considering the use of digital pulse shape analysis techniques (DPSA) to obtain the (A,Z) values of the reaction products impinging in solid state detectors. This technique can be an important tool for selecting the relevant reaction channels at the HYDE (HYbrid DEtector ball array) silicon array foreseen for the Low Energy Branch of the FAIR facility (Darmstadt, Germany). In this work we study the feasibility of using artificial neural networks (ANNs) for particle identification with silicon detectors. Multilayer Perceptron networks were trained and tested with recent experimental data, showing excellent identification capabilities with signals of several isotopes ranging from 12C up to 84Kr, yielding higher discrimination rates than any other previously reported.

  18. Theoretical and experimental study of redox processes combined with adsorption phenomena under conditions of square-wave voltammetry

    OpenAIRE

    Gulaboski, Rubin

    2001-01-01

    Theoretical models of four electrode reactions coupled with adsorption phenomena under conditions of square-wave voltammetry are developed: simple surface redox reaction, surface catalytic reaction, cathodic stripping reaction of I order, and cathodic stripping reaction of II order.

  19. Characterization of silicon micro-strip sensors with a pulsed infra-red laser system for the CBM experiment at FAIR

    Energy Technology Data Exchange (ETDEWEB)

    Ghosh, Pradeep [Goethe University, Frankfurt am Main (Germany); GSI Helmholtz Center for Heavy Ion Research GmbH, Darmstadt (Germany); Eschke, Juergen [GSI Helmholtz Center for Heavy Ion Research GmbH, Darmstadt (Germany); Facility for Anti-proton and Ion Research, GmbH, Darmstadt (Germany); Collaboration: CBM-Collaboration

    2015-07-01

    The Silicon Tracking System (STS) of the CBM experiment at FAIR is composed of 8 tracking stations comprising of 1292 double-sided silicon micro-strip sensors. A Laser Test System (LTS) has been developed for the quality assurance of prototype sensors. The aim is to scan sensors with a pulsed infra-red laser driven by step motor to determine the charge sharing in-between strips and to measure qualitative uniformity of the sensor response over the whole active area. Several prototype sensors with strip pitch of 50 and 58 μm have been tested, as well as a prototype module with realistic mechanical arrangement of sensor and read-out cables. The LTS is designed to measure sensor response in an automatized procedure across the sensor with focused laser beam (spot-size ∼ 12 μm, wavelength = 1060 nm). The pulse with duration (∼ 10 ns) and power (∼ 5 mW) of the laser pulses is selected such, that the absorption of the laser light in the 300 μm thick silicon sensors produces a number of about 24000 electrons, which is similar to the charge created by minimum ionizing particles (MIP) in these sensors. Results from laser scans of prototype sensors and detector module are reported.

  20. Electrochemical reduction and cathodic stripping voltammetric determination of clotrimazole

    Directory of Open Access Journals (Sweden)

    Pereira Francisco C.

    2001-01-01

    Full Text Available The reduction of clotrimazole at a mercury electrode, in phosphate buffer, pH>6, involves a reversible one-electron process. The electrochemical process presents a large contribution from adsorption effects. For the differential pulse polarographic determination the addition of Triton X-100 is recommended. Clotrimazole can be determined by cathodic stripping voltammetry at 50 ng mL-1 level when pre-accumulated for 3 min at an accumulation potential of -0.20 V. The proposed method is applied successfully for the determination of clotrimazole in a commercial formulation.

  1. Affordable Cyclic Voltammetry

    Science.gov (United States)

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

    2009-01-01

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

  2. Affordable Cyclic Voltammetry

    Science.gov (United States)

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

    2009-01-01

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

  3. Voltammetry Method Evaluation

    Energy Technology Data Exchange (ETDEWEB)

    Hoyt, N. [Argonne National Lab. (ANL), Argonne, IL (United States); Pereira, C. [Argonne National Lab. (ANL), Argonne, IL (United States); Willit, J. [Argonne National Lab. (ANL), Argonne, IL (United States); Williamson, M. [Argonne National Lab. (ANL), Argonne, IL (United States)

    2016-07-29

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

  4. Cyclic Voltammetry Experiment.

    Science.gov (United States)

    Van Benschoten, James J.; And Others

    1983-01-01

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

  5. Cyclic Voltammetry Experiment.

    Science.gov (United States)

    Van Benschoten, James J.; And Others

    1983-01-01

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

  6. Determination of Salicylic Acid by Differential Pulse Voltammetry with an Electro-activated Glassy Carbon Electrode%电活化玻碳电极差分脉冲伏安法测定水杨酸的研

    Institute of Scientific and Technical Information of China (English)

    杜海军; 罗乐; 柳斌; 赵宇中; 李玉美; 谢兵

    2011-01-01

    The electrochemical behavior of salicylic acid ( SA ) on an electro-activated glassy carbon electrode ( EGCE) was studied by cyclic voltammetry(CV) and differential pulse voltammetry(DPV). The glassy carbon electrode ( GCE ) was activated in pH 7. 0 PBS buffer for 400 s by potentiostatic method at +1. 7 V. In 0. 2 mol ? L-1 NaOH solution, a well-defined oxidative peak of SA was observed at 0. 602 V(υs. Ag/AgCl) on the activated electrode. The anodic peak current increased linearly with scan rate from 0. 02 V ? S -1 to 0. 2 V ? S-1, revealing that the reaction was a absorption-controlled process. The experimental parameters were optimized and the correlation between peak current (Ipa) and concentration was studied by differential pulse voltammetry. Under the optimal conditions, the linear range for SA was in the range of 5. 0 x 10-6 -2. 0 x 10-3 mol ? L-1 with a correlation coefficient of 0. 986 3, and the detection limit(S/iV = 3) was 1. 2 x 10-7 mol ? L-1. The activated glassy carbon electrode showed the advantages of simple preparation procedure and good reproduc-ibility, and was applied in the determination of salicylic acid in pharmaceutical drugs with satisfactory results%采用循环伏安法和差分脉冲伏安法对水杨酸在电活化玻碳电极上的电化学行为进行研究.在pH7.0的PBS溶液中,将玻碳电极用恒电位法在+1.7V电位阳极氧化400 s.在0.2 mol·L- NaOH溶液中,水杨酸在0.602 V处有一良好的氧化峰,其氧化峰电流与扫描速率在0.02~0.2 V·s-1范围内呈良好线性关系,表明电极过程为受吸附控制的不可逆过程.差分脉冲伏安法的氧化峰电流(Ipa)与水杨酸的浓度在5.0×10-6~2.0×10-3 mol·L-1范围内呈良好的线性关系,相关系数为0.986 3,检出限为1.2×10-7mol· L-1.该方法操作简便,重复性较好,将其用于阿司匹林片剂中水杨酸含量的检测,结果满意.

  7. Electroanalytical determination of donepezil HCl in tablets and human serum by differential pulse and osteryoung square wave voltammetry at a glassy carbon electrode.

    Science.gov (United States)

    Golcu, A; Ozkan, S A

    2006-09-01

    Donepezil hydrochloride (DNP) is used for the treatment of mild to moderate dementia of the Alzheimer's type. The voltammetric behavior of DNP was studied at a glassy carbon electrode using cyclic, linear sweep, differential pulse (DPV) and square-wave (OSWV) voltammetric techniques. DNP exhibited irreversible anodic waves within the pH range 1.80 and 9.00 in different supporting electrolytes. The peak was characterized as being irreversible and diffusion-controlled. The possible mechanism of the oxidation process is discussed. The current-concentration plot was rectilinear over the range from 1 x 10(-6) to 1 x 10(-4) M in Britton-Robinson buffer at pH 7.0 with a correlation coefficient between 0.997 and 0.999 in supporting electrolyte and human serum samples using the DPV and SWV techniques. The repeatability and reproducibility of the methods for both media (supporting electrolyte and serum sample) were determined. Precision and accuracy of the developed methods were demonstrated by recovery studies. The standard addition method was used for the recovery studies. No electroactive interferences were found in biological fluids from endogenous substances or additives present in tablets. The methods developed were successfully applied to the determination of DNP in tablets and in spiked human serum.

  8. Pulse transient hot strip technique adapted for slab sample geometry to study anisotropic thermal transport properties of μm-thin crystalline films.

    Science.gov (United States)

    Ma, Y; Gustavsson, J S; Haglund, A; Gustavsson, M; Gustafsson, S E

    2014-04-01

    A new method based on the adaptation of the Pulse Transient Hot Strip technique to slab sample geometry has been developed for studying thermal conductivity and thermal diffusivity of anisotropic thin film materials (conductivity in the 0.01-100 W/mK range, deposited on thin substrates (i.e., wafers). Strength of this technique is that it provides a well-controlled thermal probing depth, making it possible to probe a predetermined depth of the sample layer and thereby avoiding the influence from material(s) deeper down in the sample. To verify the technique a series of measurements were conducted on a y-cut single crystal quartz wafer. A Hot Strip sensor (32-μm wide, 3.2-mm long) was deposited along two orthogonal crystallographic (x- and z-) directions and two independent pulse transients were recorded. Thereafter, the data was fitted to our theoretical model, and the anisotropic thermal transport properties were determined. Using a thermal probing depth of only 30 μm, we obtained a thermal conductivity along the perpendicular (parallel) direction to the z-, i.e., optic axis of 6.48 (11.4) W/mK, and a thermal diffusivity of 3.62 (6.52) mm(2)/s. This yields a volumetric specific heat of 1.79 MJ/mK. These values agree well with tabulated data on bulk crystalline quartz supporting the accuracy of the technique, and the obtained standard deviation of less than 2.7% demonstrates the precision of this new measurement technique.

  9. 掺杂硒碳糊电极阳极溶出法测定铋%Determination of bismuth at carbon paste electrodes doped with selenium by anodic stripping voltammetry

    Institute of Scientific and Technical Information of China (English)

    韦革; 魏小平; 李建平

    2011-01-01

    A new anodic stripping voltammetric method for the determination trace bismuth of was developed by using carbon paste electrodes doped with selenium as a working electrode. In 0.1 mol/L HC1, a sensitive oxidation peak of the Bi3+ were obtained with the peak potential of + 0.05 V (vs. Ag/AgCl). The oxidation peak current linearly changed with the logarithmic value of bismuth ion concentration in the range of 1.0 × 10-9 ~ 1. 0 × 10-5 mol/L. The detection limit was 1. 0 × 10 -10 mol/L. The method has been applied to the determination of the content of bismuth in water samples and the drugs of Bismuth Potassium Citrate Granules. The recoveries were found to be in the range of 93.3% ~ 105.4%. The proposed electrode is simple in fabrication, and cheap renewal in use. It is valuable in practical application.%建立了一种测定痕量铋的新方法,即利用掺杂硒碳糊电极作为工作电极的阳极溶出法.在0.1 mol/L的HCl底液中,Bi3+于+0.05V(vs.Ag/AgCl)出现灵敏的氧化溶出峰,铋离子的浓度在1.0×10-5~1.0×10-9 mol/L范围内其对数值lgc与铋的氧化峰电流值呈线性关系,检出限达1.0×10 -10 mol/L.本法已用于药物枸橼铋钾颗粒中铋含量的测定,回收率为95.5%~104.9%.

  10. Voltammetry of Medical Biomaterials

    OpenAIRE

    Gulaboski, Rubin; Markovski, Velo

    2015-01-01

    The use of biomaterials in the medicine, dentistry and pharmacy represents probably a major breakthrough in tackling many diseases or disabilities in the last 50 years. We refer to varios techniques that are used for the characterization of the structure and the composition of the biomaterials. Voltammetry is an electrochemical technique that helps mainly in understanding the redox properties of various biomaterials containing some suitable redox centers in their structure. We give in this le...

  11. Determination of water-soluble and insoluble (dilute-HCl-extractable) fractions of Cd, Pb and Cu in Antarctic aerosol by square wave anodic stripping voltammetry: distribution and summer seasonal evolution at Terra Nova Bay (Victoria Land)

    Energy Technology Data Exchange (ETDEWEB)

    Annibaldi, A.; Truzzi, C.; Illuminati, S.; Bassotti, E.; Scarponi, G. [Polytechnic University of Marche - Ancona, Department of Marine Science, Ancona (Italy)

    2007-02-15

    Eight PM10 aerosol samples were collected in the vicinity of the ''Mario Zucchelli'' Italian Antarctic Station (formerly Terra Nova Bay Station) during the 2000-2001 austral summer using a high-volume sampler and precleaned cellulose filters. The aerosol mass was determined by differential weighing of filters carried out in a clean chemistry laboratory under controlled temperature and humidity. A two-step sequential extraction procedure was used to separate the water-soluble and the insoluble (dilute-HCl-extractable) fractions. Cd, Pb and Cu were determined in the two fractions using an ultrasensitive square wave anodic stripping voltammetric (SWASV) procedure set up for and applied to aerosol samples for the first time. Total extractable metals showed maxima at midsummer for Cd and Pb and a less clear trend for Cu. In particular, particulate metal concentrations ranged as follows: Cd 0.84-9.2 {mu}g g{sup -1} (average 4.7 {mu}g g{sup -1}), Pb 13.2-81 {mu}g g{sup -1} (average 33 {mu}g g{sup -1}), Cu 126-628 {mu}g g{sup -1} (average 378 {mu}g g{sup -1}). In terms of atmospheric concentration, the values were: Cd 0.55-6.3 pg m{sup -3} (average 3.4 pg m{sup -3}), Pb 8.7-48 pg m{sup -3} (average 24 pg m{sup -3}), Cu 75-365 pg m{sup -3} (average 266 pg m{sup -3}). At the beginning of the season the three metals appear widely distributed in the insoluble (HCl-extractable) fraction (higher proportions for Cd and Pb, 90-100%, and lower for Cu, 70-90%) with maxima in the second half of December. The soluble fraction then increases, and at the end of the season Cd and Pb are approximately equidistributed between the two fractions, while for Cu the soluble fraction reaches its maximum level of 36%. Practically negligible contributions are estimated for crustal and sea-spray sources. Low but significant volcanic contributions are estimated for Cd and Pb ({proportional_to}10% and {proportional_to}5%, respectively), while there is an evident although not

  12. 复合锑膜修饰铜电极溶出伏安法测定水中痕量镉、铅%Determination of trace lead and cadmium in water by stripping voltammetry with a copper-based composite antimony film electrode

    Institute of Scientific and Technical Information of China (English)

    尹丽君; 凌玉; 刘刚; 李萍; 吴守国

    2011-01-01

    制备了一个铜锑合金层过渡的锑膜修饰铜电极,用于水中镉和铅的检测.该电极以铜电极为基底,先利用循环伏安法得到铜锑合金层,然后在合金层表面沉积一层锑膜.研究了电沉积和操作参数对溶出峰电流的影响.在浓度范围1~100μg/L的Cd(Ⅱ)和Pb(Ⅱ)溶液中,该电极显示出良好的线性关系,线性相关系数分别为0.996 0和0.995 2.铜基复合锑膜电极对Cd(Ⅱ)和Pb(Ⅱ)的检出限分别为0.25μg/L和0.08 μg/L(信噪比为3).该电极具有成本低、易制作、稳定、低毒、重现性好等优点,有望应用于环境水质的现场监测.%A copper-based Cu-Sb/Sb composite film electrode consisting of a copper-antimony alloy transitional layer and an outer electrodeposited antimony film was fabricated on a copper substrate. The novel structured composite antimony film electrode was utilized for determination of Cd( Ⅱ ) and Pb( Ⅱ) with square wave anodic stripping voltammetry. The electrode was first prepared by cyclic voltammetry to obtain a copper-antimony alloy layer on the surface of a copper substrate. Then, an antimony film was plated on the alloy layer by electrolytic deposition potentiostatically. The composite antimony film electrode displayed excellent linear behavior in the detection of Cd( Ⅱ) and Pb( Ⅱ ) with the concentration ranging from 1 to 100 μg/L (R2 =0. 996 0 and 0. 995 2 for Cd( Ⅱ ) and Pb( Ⅱ ) respectively). The detection limit of the electrode was estimated to be 0. 25 μg/L and 0. 08 μg/L for Cd( II ) and Pb( II ) > respectively (S/N=3). The prepared composite antimony film electrode possesses low cost, long term stability, low toxicity, high sensitivity and good reproducibility, which makes it a hopeful candidate for on-site water monitoring for heavy metals.

  13. A Single-Use, In Vitro Biosensor for the Detection of T-Tau Protein, A Biomarker of Neuro-Degenerative Disorders, in PBS and Human Serum Using Differential Pulse Voltammetry (DPV).

    Science.gov (United States)

    Dai, Yifan; Molazemhosseini, Alireza; Liu, Chung Chiun

    2017-02-19

    A single-use, in vitro biosensor for the detection of T-Tau protein in phosphate-buffer saline (PBS) and undiluted human serum was designed, manufactured, and tested. Differential pulse voltammetry (DPV) served as the transduction mechanism. This biosensor consisted of three electrodes: working, counter, and reference electrodes fabricated on a PET sheet. Both working and counter electrodes were thin gold film, 10 nm in thickness. Laser ablation technique was used to define the size and structure of the biosensor. The biosensor was produced using cost-effective roll-to-roll process. Self-assembled monolayers (SAM) of 3-mercaptopropionic acid (MPA) were employed to covalently immobilize the anti-T-Tau (T-Tau antibody) on the gold working electrode. A carbodiimide conjugation approach using N-(3-dimethylaminopropyl)-N'-ethylcarbodiimide hydrochloride (EDC) and N-hydroxysuccinimide (NHS) cross-linked anti-T-Tau to the carboxylic groups on one end of the MPA. A T-Tau protein ladder with six isoforms was used in this study. The anti-T-Tau concentration used was 500,000 pg/mL. The T-Tau protein concentration ranged from 1000 pg/mL to 100,000 pg/mL. DPV measurements showed excellent responses, with a good calibration curve. Thus, a practical tool for simple detection of T-Tau protein, a biomarker of neuro-degenerative disorders, has been successfully developed. This tool could also be extended to detect other biomarkers for neuro-degenerative disorders, such as P-Tau protein and β-amyloid 42.

  14. Study on Application of Cinchonine _ modified Carbon Paste Electrode:Anodic Stripping Voltammetry Determination of Bismuth%辛可宁修饰碳糊电极的应用研究——铋的阳极溶出伏安法测定

    Institute of Scientific and Technical Information of China (English)

    张海丽; 叶永康; 徐斌

    2000-01-01

    A method for the determination of bismuth is reported with self _ made carbon paste electrode modified by cinchonine. After bismuth ions are accumulated under the applied potential of -1.00 V for 120 s on the chemical modified electrode in 1 mol/L H2SO4 solution, there is a sensitive oxidation peak of Bi at -0.022 V(vs SCE) in the determination by anodic stripping voltammetry(ASV). Dependence of current on concentration is linear from 1.0×10-8 to 1.0×10-4 mol/L of Bi3+. The detection limit is 5.0×10-9 mol/L. Other metal ions do not interfere in the determination.%报道了利用辛可宁修饰碳糊电极测定铋的方法,在1 mol/L H2SO4溶液中,通过在-1.00 V电位下富集Bi3+后,在-0.20 ~+0.15 V电位范围内作阳极溶出伏安法测定。在-0.022 V处有一灵敏的氧化峰,峰电流与Bi3+浓度在1.0×10-8 ~1.0×10-4 mol/L范围内成良好的线性关系,检出限为5.0×10-9 mol/L。其他金属离子不干扰测定。

  15. Differential pulse anodic stripping voltammetric determination of lead(II) with a 1,4-bis(prop-2'-enyloxy)-9,10-anthraquinone modified carbon paste electrode.

    Science.gov (United States)

    Mousavi, M F; Rahmani, A; Golabi, S M; Shamsipur, M; Sharghi, H

    2001-08-30

    A sensitive and selective method for the determination of lead(II) with a 1,4-bis(prop-2'-enyloxy)-9,10-anthraquinone (AQ) modified carbon paste electrode has been developed. The method is based on non-electrolytic preconcentration via complex formation with modifier, followed by an accumulation period with a negative potential (-1.5 V), and then by a proper anodic stripping. The analytical performance was evaluated with respect to the quantity of modifier in the paste, concentration of electrolyte solution, preconcentration time, lead(II) concentration, and other variables. A linear calibration graph was obtained in the concentration range 2.00x10(-9)-1.06x10(-5) M Pb(II) (n=21, r=0.9999) with 30 s preconcentration time. The detection limit was found to be 1x10(-9) M. For eight preconcentration/determination cycles, the differential pulse voltammetric response was reproduced with 5.0 and 3.7% relative standard deviations at 2.00x10(-8) and 2.00x10(-6) M Pb(II), respectively. Rapid and convenient renewal of electrode surface allows the use of a single modified electrode surface in multiple analytical determinations over several weeks. Many coexisting metal ions had little or no effect on the determination of lead(II). The developed method was applied to lead determination in waste waters.

  16. Pulse

    Science.gov (United States)

    ... resting for at least 10 minutes. Take the exercise heart rate while you are exercising. ... pulse rate can help determine if the person's heart is pumping. Pulse ... rate gives information about your fitness level and health.

  17. Sensitive and reproducible quantification of Cu2+ by stripping with a carbon paste electrode modified with humic acid.

    Science.gov (United States)

    Thobie-Gautier, Christine; da Silva, Wilson T Lopes; Rezende, Maria O O; El Murr, Nabil

    2003-09-01

    The preparation of a humic acid modified carbon paste electrode (HA-MCPE) as well as the behavior of its surface as complexing agent toward Cu2+ cations are described. Electrochemical studies of the reduction of the complexed cations and of the anodic stripping oxidation of the resulting copper are outlined. The anodic stripping current was correlated to the Cu2+ concentrations. A well-defined method for the preparation of reproducible electrodes is described. The effects on the current response obtained by cyclic voltammetry of the humic acid ratio, the pH, the accumulation time, and the speed scan rate were studied. Calibration graphs were linear over the range 3 x 10(-8)-10(-5) mol L(-1) Cu2+ and the relative standard deviation (R.S.D.) was 1.2% (n=5) for [Cu2+] = 1.6 x 10(-5) mol L(-1). 5 min accumulation time for [Cu2+] > 10(-7) mol L(-1) and 10 min for [Cu2+] < 10(-7) mol L(-1) were sufficient to permit sensitive and reproducible measurements. The electrode was successfully used to measure Cu2+ in real samples and the results were compared to those obtained by the standard method with differential pulse anodic stripping voltammetry.

  18. Propagation of short laser pulses in partially stripped plasma%有限长激光脉冲在部分离化等离子体中的传播

    Institute of Scientific and Technical Information of China (English)

    柳剑鹏; 刘明萍; 陶向阳; 刘三秋

    2015-01-01

    In order to study the propagation characteristics of short laser pulses in partially stripped plasma , parameters evolution equation of short laser pulses in partially ionized plasma was derived using variational method .The effect parameters of wakefield , relativistic self-focusing and intensity of partially stripped plasma were analyzed .The coupled evolution equations of the laser spot size and the pulse length were derived and the propagation of a short laser pulse in partially stripped plasma was analyzed under the effects of transverse wakefield ( TWF ) and longitudinal wakefield (LWF).The results show that laser pulse can be allowed to propagate in patitally stripped plasma only when a certain condition is satisfied .The evolution of the pulse length should be considered in partially stripped plasma .When laser pulse and plasma density is constant , with the increasing of ionization degree , wakefield will enhance the self-focusing of the laser pulse further .Longitudinal wakefield has more obvious effect on self-focusing of laser pulse than transverse wakefield .The results may be significant theoretically to the mechanism of ionization-induced injection and acceleration by an intense laser pulse.%为了研究有限长激光脉冲在部分离化等离子体中的传播特性,采用变分法推导出有限长激光脉冲在部分离化等离子体中的参量演化方程,分析了尾波场、相对论自聚焦和部分离化非线性极化强度的影响因素;通过分析焦斑半径和脉冲宽度满足的耦合方程,讨论了横向和纵向尾波场影响下的激光脉冲传播特性。结果表明,由于焦斑半径和脉冲宽度的耦合,激光脉冲在部分离化等离子体中传播必须满足一定条件;在部分离化等离子体中,考虑激光传播时脉冲宽度的变化是有必要的;对给定强度的激光脉冲,等离子体密度不变时,随着电离程度增大,尾波场会进一步增强激光脉冲的自

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

    Directory of Open Access Journals (Sweden)

    Chalder Nogueira Nunes

    2016-01-01

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

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

    Science.gov (United States)

    2016-01-01

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

  1. Determination of dextromethorphan hydrobromide by differential pulse anodic stripping voltammetry%微分脉冲阳极溶出伏安法测定氢溴酸右美沙芬

    Institute of Scientific and Technical Information of China (English)

    林晓华; 王桂芬; 王爽; 许桂花; 王清珊

    2010-01-01

    应用循环伏安法和微分脉冲阳极溶出伏安法在玻碳电极上对氢溴酸右美沙芬的伏安行为进行了研究.实验结果表明,在pH 6.5的B-R(Britton-Robinson)缓冲底液中,氢溴酸右美沙芬在+1.01 V(vs.Ag/AgCl)处有一明显的氧化峰,在4.0×10~(-6)~8.0×10~(-5) mol/L范围内与峰电流呈良好的线性关系(r=0.995 1),检出限为5.6×10~(-7) mol/L.用该方法对氢溴酸右美沙芬片进行了测定,回收率为98.6%~102.9%,结果令人满意,还对其电极反应机理进行了初步探讨.

  2. 中草药对DNA氧化损伤水平的微分脉冲伏安法测定%Determination of the Levels of DNA Damage Induced by Chinese Herbal Medicine Using Differential Pulse Voltammetry

    Institute of Scientific and Technical Information of China (English)

    利健文; 陈任宏; 崔丽京; 汪小根

    2012-01-01

    Effects of DNA damage induced by Chinese herbal medicine were studied by differential pulse voltammetric ( DPV) method. The voltammeitric behaviour of 8-hydorxy-2'-deoxyano-sine ( 8-OHdG) in the phosphate buffer (pH 5. 0) was investigated at a glassy carbon electrode by cyclic voltammetry (CV) and DPV. A well-defined oxidation peak of 8-OHdG at +0. 5 V was found, and its current intensity was proportional to concentration of 8-OHdG in the range of 1. 0×10 -6 - 7. 1 ×10-4 mol/L. The regression equation was Ip((μA) =0.004 3e(mol/L) +4 ×10-8 ( r =0. 999 8) and the detection limit (S/N = 3 ) was 3. 5× 10-7 mol/L. The method was applied in analysis of the levels of 8-OHdG in the calf thymus DNA(ctDNA) exposed to concentration of 40 g/L of glycynhiza, cherokee rose, eucommia ulmoides, pinellia, nux vomica extract for 2 h, respectively, and the blood of Kunming mice exposed to low and high concentration of nux vomica extract by mouth injection for 30 consecutive days. The results showed that glycyrrhiza, cherokee rose, eucommia ulmoides, pinellia ex-tract could not cause ctDNA oxidative damage, and nux vomica extract can cause DNA oxidative dam-age to the formation of 8-OHdG in the average level of (3. 2 0. 2)μmol/L. The average levels of 8-OHdG were (2. 0 0. 1) (μmol/L and (5. 3 0. 3) μmol/L in the blood after a long-term administration of low concentration and high concentration of nux vomica extracts of Kunming mice, respectively. The study indicated that nux vomica contained the potential genotoxicity.%采用微分脉冲伏安法(DPV)研究了中草药对脱氧核糖核酸分子(DNA)的损伤效应.在pH 5.0的磷酸盐缓冲液中,采用DPV法研究了8-羟基脱氧鸟苷(8-OHdG)在玻碳电极上的伏安行为,发现8-OHdG在+0.5 V电位处产生一灵敏的微分脉冲阳极氧化峰.该氧化峰的峰电流与8-OHdG的浓度在1.0×10-6~7.1 ×10-4 mol/L范围内呈良好的线性关系,r=0.9998,检出限(S/N=3)为3.5×10-7 mol/L.将该方法应

  3. A brief review: Ultrafast electron diffractive voltammetry: General formalism and applications

    CERN Document Server

    Chang, Kiseok; Tao, Zhensheng; Han, Tzong-Ru T; Ruan, Chong-Yu

    2013-01-01

    We present a general formalism of ultrafast diffractive voltammetry approach as a contact-free tool to investigate the ultrafast surface charge dynamics in nanostructured interfaces. As case studies, the photoinduced surface charging processes in oxidized silicon surface and the hot electron dynamics in nanoparticle-decorated interface are examined based on the diffractive voltammetry framework. We identify that the charge redistribution processes appear on the surface, sub-surface, and vacuum levels when driven by intense femtosecond laser pulses. To elucidate the voltammetry contribution from different sources, we perform controlled experiments using shadow imaging techniques and N-particle simulations to aid the investigation of the photovoltage dynamics in the presence of pho- toemission. We show that voltammetry contribution associated with photoemission has a long decay tail and plays a more visible role in the nanosecond timescale, whereas the ultrafast voltammetry are dominated by local charge transfe...

  4. Cathodic stripping voltammetric determination of arsenic in sugarcane brandy at a modified carbon nanotube paste electrode.

    Science.gov (United States)

    Teixeira, Meryene C; Tavares, Elisângela de F L; Saczk, Adelir A; Okumura, Leonardo L; Cardoso, Maria das Graças; Magriotis, Zuy M; de Oliveira, Marcelo F

    2014-07-01

    We have developed an eletroanalytical method that employs Cu(2+) solutions to determine arsenic in sugarcane brandy using an electrode consisting of carbon paste modified with carbon nanotubes (CNTPE) and polymeric resins. We used linear sweep (LSV) and differential-pulse (DPV) voltammetry with cathodic stripping for CNTPE containing mineral oil or silicone as binder. The analytical curves were linear from 30 to 110μgL(-1) and from 10 to 110μgL(-1) for LSV and DPV, respectively. The limits of detection (L.O.D.) and quantification (L.O.Q.) of CNTPE were 10.3 and 34.5μgL(-1) for mineral oil and 3.4 and 11.2μgL(-1) for silicone. We applied this method to determine arsenic in five commercial sugarcane brandy samples. The results agreed well with those obtained by hydride generation combined with atomic absorption spectrometry (HG AAS).

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

    Science.gov (United States)

    Hoang, Vu Dang; Huyen, Dao Thi; Phuc, Phan Hong

    2013-01-01

    The electroreduction behaviour and determination of cefoperazone using a hanging mercury drop electrode were investigated. Cyclic voltammograms of cefoperazone recorded in universal Britton-Robinson buffers pH 3–6 exhibited a single irreversible cathodic peak. The process was adsorption-controlled. Britton-Robinson buffer 0.04 M pH 4.0 was selected as a supporting electrolyte for quantitative purposes by differential pulse and square wave adsorptive cathodic stripping voltammetry. The experimental voltammetric conditions were optimized using Central Composite Face design. A reduction wave was seen in the range from −0.7 to −0.8 V. These voltammetric techniques were successfully validated as per ICH guidelines and applied for the determination of cefoperazone in its single and sulbactam containing powders for injection and statistically comparable to USP-HPLC. They were further extended to determine cefoperazone in spiked human urine with no matrix effect. PMID:24109542

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

    Directory of Open Access Journals (Sweden)

    Vu Dang Hoang

    2013-01-01

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

  7. Adsorptive cathodic stripping voltammetric determination of cefoperazone in bulk powder, pharmaceutical dosage forms, and human urine.

    Science.gov (United States)

    Hoang, Vu Dang; Huyen, Dao Thi; Phuc, Phan Hong

    2013-01-01

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

  8. Stripping chronopotentiometry at scanned deposition potential (SSCP). Part 5. Features of multi-metal systems

    NARCIS (Netherlands)

    Town, R.M.; Leeuwen, van H.P.

    2004-01-01

    This paper considers the mutual effects of metals on each other in scanned deposition potential stripping chronopotentiometry measurements (SSCP) on multi-metal systems. As compared to stripping voltammetry, depletive SSCP displays a certain resistance to the impact of intermetallic compounds, while

  9. Preparation of NiO-graphene oxide nanosensor for adsorptive stripping voltammetric determination of dinoterbon in food samples

    Directory of Open Access Journals (Sweden)

    Kasaram Roja

    2016-09-01

    Full Text Available Graphene oxide (GO modified NiO electrochemical nanosensor was developed for the determination of the dinoterbon in food samples using adsorptive stripping voltammetry. The modified nanosensor characterized by TEM, XRD, cyclic and adsorptive stripping voltammetry. Dinoterbon pesticide exhibited a single well-defined cathodic peak at pH 4.0 at Britton–Robinson buffer (-810.0 mV. The voltammetric characterization of the pesti­cide residues is evaluated and the parameter such as the effect of pH, scan rate, pulse amplitude, deposition potential and deposition time were optimized. The current–concen­tration plot obtained using this peak was straight-lined over the range from 0.05 to 50.00 µg mL-1 with limit of detection (LOD 0.028 µg mL-1. The proposed method was efficiently applied to the determination of dinoterbon in food samples. The mean recoveries of the pesticide 97.40 to 99.88 % with a relative standard deviation of 0.114 % in food samples respectively.

  10. Stripping voltammetric determination of palladium, platinum and rhodium in freshwater and sediment samples from South African water resources

    CSIR Research Space (South Africa)

    Van der Horst, C

    2012-08-01

    Full Text Available of platinum (Pt2+), palladium (Pd2+) or rhodium (Rh2+) by means of adsorptive cathodic stripping voltammetry. Optimised experimental conditions included composition of the supporting electrolyte, complexing agent concentration, deposition potential, deposition...

  11. Cyclic voltammetry of supported BLMs

    Science.gov (United States)

    Murgasova, Renata; Sabo, Jan; Ottova, Angelica L.; Tien, H. T.

    1996-06-01

    The transfer of an electron across a bilayer lipid membrane (BLM) is one of the BLMs most exciting processes. A number of well known electron mediators have been investigated using the method of cyclic voltammetry on a Teflon coated platinum wire, the tip of which has been modified by a self-assembled bilayer lipid membrane (s-BLM). The electrical capacitance of the s-BLM system was measured as a function of frequency. The results are discussed in terms of electron transfer and redox reactions.

  12. Stripping voltammetric detection of nephrotoxic drug cefitizoxime in wastewater

    Directory of Open Access Journals (Sweden)

    Jahangir Ahmad Rather

    2015-06-01

    Full Text Available The objective of the present work is to develop the stripping voltammetric method for determination of nephrotoxic drug cefitizoxime in pharmaceutical formulation and its application to wastewater analysis. Solubilized system of different surfactants viz. cationic, anionic and non-ionic influences the electrochemical response of cefitizoxime. Solubilized system of CTAB containing cefitizoxime enhanced the peak current while anionic and non-ionic showed an opposite effect. The current signal due to the reduction process is a function of concentration of the cefitizoxime, pH of medium, type of surfactant and accumulation time at electrode surface. The proposed SWCAdSV (Squarewave Cathodic Adsorptive Voltammtery and DPCAdSV (Differential Pulse Cathodic Adsorptive Voltammetry are linear over concentration range 1.732–6.901 μg/mL and 4.792–30.672 μg/mL with detection limit of 0.76 ng/mL and 2.63 ng/mL, respectively. The method is successfully applied for determination of cefitizoxime in pharmaceutical formulation and wastewater with mean percentage recovery of 99.73% and 98.51%, respectively.

  13. The Strip Module

    DEFF Research Database (Denmark)

    Pedersen, Tommy

    1996-01-01

    -ship code available at the department. It will be structured as a general preprocessor mainly to determine the hydrodynamic mass and damping. A strip processor including three different theories: A linear frequency domain strip theory, a quadratic strip theory and a nonlinear time domain strip theory...

  14. Approximate strip exchanging.

    Science.gov (United States)

    Roy, Swapnoneel; Thakur, Ashok Kumar

    2008-01-01

    Genome rearrangements have been modelled by a variety of primitives such as reversals, transpositions, block moves and block interchanges. We consider such a genome rearrangement primitive Strip Exchanges. Given a permutation, the challenge is to sort it by using minimum number of strip exchanges. A strip exchanging move interchanges the positions of two chosen strips so that they merge with other strips. The strip exchange problem is to sort a permutation using minimum number of strip exchanges. We present here the first non-trivial 2-approximation algorithm to this problem. We also observe that sorting by strip-exchanges is fixed-parameter-tractable. Lastly we discuss the application of strip exchanges in a different area Optical Character Recognition (OCR) with an example.

  15. Solar UV Photooxidation as Pretreatment for Stripping Voltammetric Trace Metal Analysis in River Water

    Directory of Open Access Journals (Sweden)

    Gelaneh Woldemichael

    2011-01-01

    Full Text Available The application of solar ultraviolet radiation as sample pretreatment or preparation step in stripping voltammetric analysis of trace metals in presence of low levels of dissolved organic carbon (DOC natural water samples (river water was studied. River water samples were collected from downstream of Warnow river (Germany and acidified to pH of 2±0.2 (by addition of 1 mL of ultrapure 65% HNO3 per liter sample. Furthermore, 100 μL/L of hydrogen peroxide solution (ultrapure, 30% H2O2 was added to the samples as photochemical reaction initiator. The samples were transferred to polyethylene terephthalate (PET bottles and irradiated with solar radiation of UV-A intensity of 3.6 mW/m2 for six hours, and the concentrations of Zn, Cd, Pb, and Cu were determined by differential pulse anodic stripping voltammetry (DPASV. The comparison of the values with the results obtained for the original untreated sample and artificial UV-treated one proved that solar UV radiation can be applied to the digestion of dissolved organic carbon in trace metal analysis in natural waters like river water, lake waters, well waters, and so forth.

  16. The Strip Module

    DEFF Research Database (Denmark)

    Pedersen, Tommy

    1996-01-01

    When the behaviour of a ship in waves is to be predicted it is convenient to have a tool which includes different approaches to the problem.The aim of this project is to develop such a tool named the strip theory module. The strip theory module will consist of submodules dependent on the I......-ship code available at the department. It will be structured as a general preprocessor mainly to determine the hydrodynamic mass and damping. A strip processor including three different theories: A linear frequency domain strip theory, a quadratic strip theory and a nonlinear time domain strip theory...

  17. Varicose vein stripping

    Science.gov (United States)

    ... vein stripping; Venous reflux - vein stripping; Venous ulcer - veins Images Circulatory system References American Family Physician. Management of varicose veins. www.aafp.org/afp/2008/1201/p1289.html . ...

  18. A solid paraffin-based carbon paste electrode modified with 2-aminothiazole organofunctionalized silica for differential pulse adsorptive stripping analysis of nickel in ethanol fuel

    Energy Technology Data Exchange (ETDEWEB)

    Takeuchi, Regina M. [Departamento de Quimica Analitica, Instituto de Quimica, UNESP, CP 355, 14801-970 Araraquara, SP (Brazil)]. E-mail: takeuchi@iq.unesp.br; Santos, Andre L. [Departamento de Quimica Analitica, Instituto de Quimica, UNESP, CP 355, 14801-970 Araraquara, SP (Brazil); Padilha, Pedro M. [Departamento de Quimica e Bioquimica-IB/UNESP, CP 510, 18618-000 Botucatu, SP (Brazil); Stradiotto, Nelson R. [Departamento de Quimica Analitica, Instituto de Quimica, UNESP, CP 355, 14801-970 Araraquara, SP (Brazil)

    2007-02-19

    A solid paraffin-based carbon paste electrode modified with 2-aminothiazole organofunctionalized silica (SiAt-SPCPE) was applied to Ni{sup 2+} determination in commercial ethanol fuel samples. The proposed method comprised four steps: (1) Ni{sup 2+} preconcentration at open circuit potential directly in the ethanol fuel sample, (2) transference of the electrode to an electrochemical cell containing DMG, (3) differential pulse voltammogram registering and (4) surface regeneration by polishing the electrode. The proposed method combines the high Ni{sup 2+} adsorption capacity presented by 2-aminothiazole organofunctionalized silica with the electrochemical properties of the Ni(DMG){sub 2} complex, whose electrochemical reduction provides the analytical signal. All experimental parameters involved in the proposed method were optimized. Using a preconcentration time of 20 min, it was obtained a linear range from 7.5 x 10{sup -9} to 1.0 x 10{sup -6} mol L{sup -1} with detection limit of 2.0 x 10{sup -9} mol L{sup -1}. Recovery values between 96.5 and 102.4% were obtained for commercial samples spiked with 1.0 {mu}mol L{sup -1} Ni{sup 2+} and the developed electrode was totally stable in ethanolic solutions. The contents of Ni{sup 2+} found in the commercial samples using the proposed method were compared to those obtained by graphite furnace atomic absorption spectroscopy by using the F- and t-test. Neither the F- nor t-values exceeded the critical values at 95% confidence level, confirming that there are not statistical differences between the results obtained by both methods. These results indicate that the developed electrode can be successfully employed to reliable Ni{sup 2+} determination in commercial ethanol fuel samples without any sample pretreatment or dilution step.

  19. 基于表面活性剂存在下电化学结合化学计量学同时测定3种着色剂%Simultaneous differential pulse stripping voltammetric determination of three food colorants in presence of CTAB with aid of chemometrics

    Institute of Scientific and Technical Information of China (English)

    钟永生; 桂怿; 倪永年

    2012-01-01

    利用微分脉冲伏安法研究了日落黄、苋菜红和柠檬黄等3种着色剂在裸玻碳电极上的电化学行为及定量分析测定的可行性.实验发现,在表面活性剂溴化十六烷基三甲铵(CTAB,浓度为40.0×10-6 mol·L-1)存在下,3种着色剂日落黄、苋菜红和柠檬黄均具有较高的电化学测定灵敏度,它们的线性范围分别为4.0~40.0,5.0~60.0和2.5~35.0 nmol·L-1,对应的最低检测线分别为1.54,2.38和1.10 nmol·L-1.但这3种被测物质中日落黄和苋菜红的伏安波谱相互重叠,因此在不进行化学分离预处理的情况下很难对这3种着色剂同时进行测定.采用偏最小二乘法、主成分分析以及它们的一阶导数等化学计量学方法对它们的重叠伏安谱图进行解析和定量分析,结果表明,导数偏最小二乘法的计算结果最好,总相对预测误差(RPET)为6.18%.利用提出的方法对冰激凌、汽水和糖果等实际样中的3种着色剂进行直接测定,获得了较好的定量分析结果.%The differential pulse stripping voltammetric (DPSV) method was developed, to determine hree colorants,sunset yellow,amaranth and tartrazine. The method proposed was based on the adsorptive accumulation of the colorants on the carbon electrode,and the oxidation of the absorptive species by the voltam-metry. The 40. 0×10-6 mol · L-1 of cetyltrimethyl ammonium bromide (CTAB) was used as the optimal for the experiment. The linear concentration ranges were found to be 4. 0-40. 0.5. 0-60. 0 and 2. 5-35. 0 nmol · L-1 ,for sunset yellow, amaranth and tartrazine, respectively. Their corresponding detection limits were 1. 54,2. 38 and 1. 10 nmol · L-1. Since the voltammograms of these colorants were seriously overlapped, it was difficult to determine them individually from the voltammetric signals of the mixtures. Thus, some chemometrics methods,such as partial least squares (PLS),principle component regression (PCR) and their first-order derivative

  20. 微波消解-铋膜/Nation修饰电极溶出伏安法测定鳗鱼中的镉含量%Determination of Cadmium in Eel by Microwave Digestion Followed by Stripping Voltammetry on Bismuth/Nation Modified Electrode

    Institute of Scientific and Technical Information of China (English)

    李静; 李红波; 范大和; 王伟

    2011-01-01

    A stripping voltammetric method based on microwave digestion was developed for determining cadmium in eel on a bismuth/nafion modified electrode. Oxidation yield a well-defined square wave peak for Cd^2+ at about - 0.85 V. Nation concentration, bismuth film thickness, buffer solution pH, deposition potential accumulation time and other potential interference factors were investigated. A linear relationship was found between peak area and cadmium concentration over the range of 4.0 to 14.0 μg/L with a correlation coefficient of 0.9964. The limit of detection of the method was 0.2 μg/L. The sensor was highly sensitive and effective to detect cadmium even in the presence of several excess potential interference ions.%运用铋膜/Nation修饰电极耦合微波消解技术测定鳗鱼中的Cd^2+。Cd^2+在-0.85V处出现清晰的方波氧化峰。Nafion、铋膜的厚度、缓冲液的pH值、富集电位、富集时间及可能干扰物质的影响因素进行考察。Cd^2+在4.0~14.0μg/L质量浓度范围内线性关系,线性相关性系数为0.9964,检出限为0.2ug/L。结果表明,该传感器在过量的干扰离子存在条件下,表现出超灵敏性和有效性。

  1. Voltage biasing, cyclic voltammetry, & electrical impedance spectroscopy for neural interfaces.

    Science.gov (United States)

    Wilks, Seth J; Richner, Tom J; Brodnick, Sarah K; Kipke, Daryl R; Williams, Justin C; Otto, Kevin J

    2012-02-24

    Electrical impedance spectroscopy (EIS) and cyclic voltammetry (CV) measure properties of the electrode-tissue interface without additional invasive procedures, and can be used to monitor electrode performance over the long term. EIS measures electrical impedance at multiple frequencies, and increases in impedance indicate increased glial scar formation around the device, while cyclic voltammetry measures the charge carrying capacity of the electrode, and indicates how charge is transferred at different voltage levels. As implanted electrodes age, EIS and CV data change, and electrode sites that previously recorded spiking neurons often exhibit significantly lower efficacy for neural recording. The application of a brief voltage pulse to implanted electrode arrays, known as rejuvenation, can bring back spiking activity on otherwise silent electrode sites for a period of time. Rejuvenation alters EIS and CV, and can be monitored by these complementary methods. Typically, EIS is measured daily as an indication of the tissue response at the electrode site. If spikes are absent in a channel that previously had spikes, then CV is used to determine the charge carrying capacity of the electrode site, and rejuvenation can be applied to improve the interface efficacy. CV and EIS are then repeated to check the changes at the electrode-tissue interface, and neural recordings are collected. The overall goal of rejuvenation is to extend the functional lifetime of implanted arrays.

  2. Ultrafast cyclic voltammetry with asymmetrical potential scan

    Institute of Scientific and Technical Information of China (English)

    Zhi Yong Guo; Xiang Qin Lin

    2008-01-01

    Based on the perfect ohmic drop compensation by online electronic positive feedback, ultrafast cyclic voltammetry withasymmetrical potential scan is achieved for the first time, with the reduction of anthracene acting as the test system. Compared withthe traditional cyclic voltammetry utilizing symmetrical triangular waveform as the excitation one, the new method allows a simplerapproach to mechanistic analysis of ultrafast chemical reactions coupled with a charge transfer. And perhaps more important, it alsoprovides a way to eliminate the interference of the adsorbed product in dynamic monitoring.

  3. Simultaneous DPV determination of morphine and codeine using dsDNA modified screen printed electrode strips coupled with electromembrane extraction

    Directory of Open Access Journals (Sweden)

    Rouhollah Feizbakhsh

    2016-01-01

    Full Text Available In this work a sensitive electrochemical sensor for simultaneous determination of morphine and codeine constructed by application of disposable screen printed carbon electrode strips (SPCE modified by double strand (ds calf thymus DNA. According to the results of the modified SPCE strips and experimented parameters, we observed a considerable shift between potentials of morphine and codeine current peaks. Related to these observed shifts, we studied on the effect of the concentration of modifier and pH value on the anodic oxidation pattern of morphine and codeine in the case of optimize the method to get better signals with maximum potential distance. Also to boosting the LODs of this electroanalytical method coupled with an electro-membrane preconcentration (EME step. The calibration curve which was plotted by the variation of differential pulse voltammetry (DPV currents as a function of different morphine and codeine concentration were linear within the range of 0.7– 40 µM and 2.3- 40 µM for morphine and codeine respectively. Also the limits of detection were 0.07 µM and 0.23 µM, respectively. Finally, the proposed method was able to determine morphine and codeine simultaneously and effectively in urinary real samples

  4. Polyol synthesis of nanosized Pt/C electrocatalysts assisted by pulse microwave activation

    Energy Technology Data Exchange (ETDEWEB)

    Lebegue, E.; Baranton, S.; Coutanceau, C. [Laboratoire de Catalyse en Chimie Organique (LACCO), UMR 6503 CNRS, Universite de Poitiers, 40 av recteur Pineau, F-86000 Poitiers (France)

    2011-02-01

    A polyol process assisted by pulse microwave activation was used to prepare efficient Pt/C electrocatalysts for PEMFC applications with reducing cost. Catalysts from pulsed microwave method were compared with a catalyst issued from a classical method, in terms of active surface area, platinum loading and activity towards the oxygen reduction reaction. A design of experiments (DOE derived from the Taguchi method) has been implemented to optimize experimental parameters only related to pulse microwave activation, the intrinsic synthesis parameters (concentration of platinum salt, platinum/carbon weight ratio and pH) being kept constant. Controlled parameters were duration of microwave pulse, maximum temperature and total duration of the synthesis. Considered responses were catalyst active surface area and the Pt/C loading. An optimized configuration of synthesis parameter was proposed. The confirmation experiment revealed a trend in agreement with that expected. Three catalysts (two from pulsed microwave synthesis method and one prepared by the classical method) were characterized by transmission electron microscopy, cyclic voltammetry and CO stripping. Catalysts from pulsed microwave method display higher characteristics than the one prepared by the classical method. The Pt/C catalyst from the confirmation experiment displays the highest catalytic activity toward oxygen reduction reaction. (author)

  5. Linear Sweep Voltammetry of Adsorbed Neutral Red.

    Science.gov (United States)

    1982-05-01

    E. Creager, G. T. Marks, D. A. Aikens and H. H. Richtol Prepared for Publication in Journal of Electroanalytical Chemistry Rensselaer Polytechnic... Electroanalytical Chemistry It. KEY WORDS (Continue oun reverse side It necessary mid Ideneliy by block ntaibor) Neutral Red, cyclic voltammetry, adsorbed dye 20

  6. Steady state oxygen reduction and cyclic voltammetry

    DEFF Research Database (Denmark)

    Rossmeisl, Jan; Karlberg, Gustav; Jaramillo, Thomas;

    2008-01-01

    The catalytic activity of Pt and Pt3Ni for the oxygen reduction reaction is investigated by applying a Sabatier model based on density functional calculations. We investigate the role of adsorbed OH on the activity, by comparing cyclic voltammetry obtained from theory with previously published...

  7. Voltammetry at porous electrodes: A theoretical study

    CERN Document Server

    Barnes, Edward O; Li, Peilin; Compton, Richard G

    2014-01-01

    Theory is presented to simulate both chronoamperometry and cyclic voltammetry at porous electrodes fabricated by means of electro-deposition around spherical templates. A theoretical method to extract heterogeneous rate constants for quasireversible and irreversible systems is proposed by the approximation of decoupling of the diffusion within the porous electrode and of bulk diffusion to the electrode surface.

  8. 预镀铋膜修饰碳糊电极差分脉冲伏安法测定废水中铅和镉%Ex-situ Plating Bismuth Film Modified Carbon Paste Electrode for the Determination of Trace Lead and Cadmium by Differential Pulse Voltammetry

    Institute of Scientific and Technical Information of China (English)

    雷存喜; 刘蓉; 沈毓儒; 赵运林; 董萌; 曾戴弟

    2014-01-01

    采用预镀铋膜法制得铋膜修饰碳糊电极,当沉积时间为540 s得到最优铋膜.采用差分脉冲伏安法(DPV)实现了对痕量Pb2+、Cd2+的同时测定.优化了DPV测定条件,当富集时间为150 s、富集电位为-1.25 V、HAc-NaAc缓冲底液的pH为4.5时,Pb2+、Cd2+的峰电流最大.在最优的实验条件下,Pb2+和Cd2+的峰电流与其浓度呈良好的线性关系,线性相关系数R分别为0.9912和0.9937,线性范围分别为1~10μmol/L和5~50 μmol/L,Pb2+和Cd2+的检出限分别为0.32 μmol/L和2.01 μmol/L.对实际废水样品进行了加标回收实验,其中Pb2+和Cd2+的回收率分别为98.4%~102.6%和95.4%~104.6%.%Ex-situ plating bismuth film modified carbon paste electrode was prepared for the measurement of Pb2+ and Cd2+ by differential pulse voltammetry(DPV).Pb and Cd were deposited on the surface of bismuth and displayed well defined peaks when the preconcentration time of bismuth was 540 s.The conditions of several key operational parameters were optimized.Under the optimum conditions,the oxidation peak currents changed linearly with the concentration of Pb2+ and Cd2+ at the range of 1-10 μmol/L and 5-50 μmol/L,with the detection limits of 0.32 μmol/L for Pb2+ and 2.01 μmol/L for Cd2+,and the recoveries of Pb2+ and Cd2+ in electroplating waste water were 98.4%-102.6% and 95.4%-104.6%,respectively.

  9. Anatomy Comic Strips

    Science.gov (United States)

    Park, Jin Seo; Kim, Dae Hyun; Chung, Min Suk

    2011-01-01

    Comics are powerful visual messages that convey immediate visceral meaning in ways that conventional texts often cannot. This article's authors created comic strips to teach anatomy more interestingly and effectively. Four-frame comic strips were conceptualized from a set of anatomy-related humorous stories gathered from the authors' collective…

  10. Science Comic Strips

    Science.gov (United States)

    Kim, Dae Hyun; Jang, Hae Gwon; Shin, Dong Sun; Kim, Sun-Ja; Yoo, Chang Young; Chung, Min Suk

    2012-01-01

    Science comic strips entitled Dr. Scifun were planned to promote science jobs and studies among professionals (scientists, graduate and undergraduate students) and children. To this end, the authors collected intriguing science stories as the basis of scenarios, and drew four-cut comic strips, first on paper and subsequently as computer files.…

  11. Anatomy Comic Strips

    Science.gov (United States)

    Park, Jin Seo; Kim, Dae Hyun; Chung, Min Suk

    2011-01-01

    Comics are powerful visual messages that convey immediate visceral meaning in ways that conventional texts often cannot. This article's authors created comic strips to teach anatomy more interestingly and effectively. Four-frame comic strips were conceptualized from a set of anatomy-related humorous stories gathered from the authors' collective…

  12. ALICE silicon strip module

    CERN Multimedia

    Maximilien Brice

    2006-01-01

    This small silicon detector strip will be inserted into the inner tracking system (ITS) on the ALICE detector at CERN. This detector relies on state-of-the-art particle tracking techniques. These double-sided silicon strip modules have been designed to be as lightweight and delicate as possible as the ITS will eventually contain five square metres of these devices.

  13. Cyclic Voltammetry And Linear Sweep Voltammetry Study Of Cyclic Tertiary Amines

    Institute of Scientific and Technical Information of China (English)

    ZHAO Ping; TIAN JinPing; YIN YingWu

    2001-01-01

    @@ Cyclic six membered a-aminonitrile have proved to be very versatile synthetic intermediates and have been widely used in the construction of a large number of indole alkaloids. In order to obtain some information about the mechanisn of electrochemical synthesis of aaminonitrile. Electrochemistry behaviors that include cyclic voltammetry and linear sweep voltammetry of cyclic tertiary amines which including N-benzylpiperidine (NBP), 1-(l-Methoxycarbonyl ethyl) piperidine (MCEP), N-methylcarbonylppiperidine (NMCP), Nethylpiperidine(NEP) was studied.

  14. Cyclic Voltammetry And Linear Sweep Voltammetry Study Of Cyclic Tertiary Amines

    Institute of Scientific and Technical Information of China (English)

    ZHAO; Ping

    2001-01-01

    Cyclic six membered a-aminonitrile have proved to be very versatile synthetic intermediates and have been widely used in the construction of a large number of indole alkaloids. In order to obtain some information about the mechanisn of electrochemical synthesis of aaminonitrile. Electrochemistry behaviors that include cyclic voltammetry and linear sweep voltammetry of cyclic tertiary amines which including N-benzylpiperidine (NBP), 1-(l-Methoxycarbonyl ethyl) piperidine (MCEP), N-methylcarbonylppiperidine (NMCP), Nethylpiperidine(NEP) was studied.……

  15. Voltammetry as a Model for Teaching Chemical Instrumentation.

    Science.gov (United States)

    Gunasingham, H.; Ang, K. P.

    1985-01-01

    Voltammetry is used as a model for teaching chemical instrumentation to chemistry undergraduates at the National University of Singapore. Lists six criteria used to select a successful teaching model and shows how voltammetry satisfies each criterion. (JN)

  16. Development of floating strip micromegas detectors

    Energy Technology Data Exchange (ETDEWEB)

    Bortfeldt, Jonathan

    2014-04-28

    Micromegas are high-rate capable, high-resolution micro-pattern gaseous detectors. Square meter sized resistive strip Micromegas are foreseen as replacement of the currently used precision tracking detectors in the Small Wheel, which is part of the forward region of the ATLAS muon spectrometer. The replacement is necessary to ensure tracking and triggering performance of the muon spectrometer after the luminosity increase of the Large Hadron Collider beyond its design value of 10{sup 34} cm{sup -2}s{sup -1} around 2020. In this thesis a novel discharge tolerant floating strip Micromegas detector is presented and described. By individually powering copper anode strips, the effects of a discharge are confined to a small region of the detector. This reduces the impact of discharges on the efficiency by three orders of magnitude, compared to a standard Micromegas. The physics of the detector is studied and discussed in detail. Several detectors are developed: A 6.4 x 6.4 cm{sup 2} floating strip Micromegas with exchangeable SMD capacitors and resistors allows for an optimization of the floating strip principle. The discharge behavior is investigated on this device in depth. The microscopic structure of discharges is quantitatively explained by a detailed detector simulation. A 48 x 50 cm{sup 2} floating strip Micromegas is studied in high energy pion beams. Its homogeneity with respect to pulse height, efficiency and spatial resolution is investigated. The good performance in high-rate background environments is demonstrated in cosmic muon tracking measurements with a 6.4 x 6.4 cm{sup 2} floating strip Micromegas under lateral irradiation with 550 kHz 20 MeV proton beams. A floating strip Micromegas doublet with low material budget is developed for ion tracking without limitations from multiple scattering in imaging applications during medical ion therapy. Highly efficient tracking of 20 MeV protons at particle rates of 550 kHz is possible. The reconstruction of the

  17. Optimization and validation of an automated voltammetric stripping technique for ultratrace metal analysis

    Energy Technology Data Exchange (ETDEWEB)

    Monticelli, D. [Dipartimento di Scienze Chimiche e Ambientali, Universita degli Studi dell' Insubria, Via Valleggio 11, 22100 Como (Italy)]. E-mail: damiano.monticelli@uninsubria.it; Ciceri, E. [Dipartimento di Scienze Chimiche e Ambientali, Universita degli Studi dell' Insubria, Via Valleggio 11, 22100 Como (Italy); Dossi, C. [Dipartimento di Scienze Chimiche e Ambientali, Universita degli Studi dell' Insubria, Via Valleggio 11, 22100 Como (Italy)

    2007-07-02

    A new automated batch method for the determination of ultratrace metals (nanogram per liter level) was developed and validated. Instrumental and chemical parameters affecting the performance of the method were carefully assessed and optimized. A wide range of voltammetric methods under different chemical conditions were tested. Cadmium, lead and copper were determined by anodic stripping voltammetry (ASV), while nickel, cobalt, rhodium and uranium by adsorptive cathodic stripping voltammetry (AdCSV). The figures of merit of all of these methods were determined: very good precision and accuracy were achieved, e.g. relative percentage standard deviation in the 4-13% for ASV and 2-5% for AdCSV. The stripping methods were applied to the determination of cadmium, lead, copper, nickel, cobalt, rhodium and uranium in lake water samples and the results were found to be comparable with ICP-MS data.

  18. Pulse electrodeposition to prepare core-shell structured AuPt@Pd/C catalyst for formic acid fuel cell application

    Science.gov (United States)

    Lu, Xueyi; Luo, Fan; Song, Huiyu; Liao, Shijun; Li, Hualing

    2014-01-01

    A novel core-shell structured AuPt@Pd/C catalyst for the electrooxidation of formic acid is synthesized by a pulse electrodeposition process, and the AuPt core nanoparticles are obtained by a NaBH4 reduction method. The catalyst is characterized with X-ray powder diffraction and transmission electron microscopy, thermogravimetric analysis, cyclic voltammetry, CO stripping and X-ray photoelectron spectroscopy. The core-shell structure of the catalyst is revealed by the increase in particle size resulting from a Pd layer covering the AuPt core, and by a negative shift in the CO stripping peaks. The addition of a small amount of Pt improves the dispersion of Au and results in smaller core particles. The catalyst's activity is evaluated by cyclic voltammetry in formic acid solution. The catalyst shows excellent activity towards the anodic oxidation of formic acid, the mass activity reaches 4.4 A mg-1Pd and 0.83 A mg-1metal, which are 8.5 and 1.6 times that of commercial Pd/C. This enhanced electrocatalytic activity could be ascribed to the good dispersion of Au core particles resulting from the addition of Pt, as well as to the interaction between the Pd shell layer and the Au and Pt in the core nanoparticles.

  19. Evaluation of homogeneous electrocatalysts by cyclic voltammetry.

    Science.gov (United States)

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

    2014-10-06

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

  20. Stripping with dry ice

    Science.gov (United States)

    Malavallon, Olivier

    1995-04-01

    Mechanical-type stripping using dry ice (solid CO2) consists in blasting particles of dry ice onto the painted surface. This surface can be used alone or in duplex according to type of substrate to be treated. According to operating conditions, three physical mechanisms may be involved when blasting dry ice particles onto a paint system: thermal shock, differential thermal contraction, and mechanical shock. The blast nozzle, nozzle travel speed, blast angle, stripping distance, and compressed air pressure and media flow rate influence the stripping quality and the uniformity and efficiency obtained.

  1. Study of Copper and Purine-Copper Complexes on Modified Carbon Electrodes by Cyclic and Elimination Voltammetry

    Science.gov (United States)

    Trnkova, Libuse; Zerzankova, Lenka; Dycka, Filip; Mikelova, Radka; Jelen, Frantisek

    2008-01-01

    Using a paraffin impregnated graphite electrode (PIGE) and mercury-modified pyrolytic graphite electrode with basal orientation (Hg-PGEb) copper(II) and Cu(II)-DNA purine base solutions have been studied by cyclic (CV) and linear sweep voltammetry (LSV) in connection with elimination voltammetry with linear scan (EVLS). In chloride and bromide solutions (pH 6), the redox process of Cu(II) proceeded on PIGE with two cathodic and two anodic potentially separated signals. According to the elimination function E4, the first cathodic peak corresponds to the reduction Cu(II) + e- → Cu(I) with the possibility of fast disproportionation 2Cu(I) → Cu(II)+ Cu(0). The E4 of the second cathodic peak signalized an electrode process controlled by a surface reaction. The electrode system of Cu(II) on Hg-PGEb in borate buffer (pH 9.2) was characterized by one cathodic and one anodic peak. Anodic stripping voltammetry (ASV) on PIGE and cathodic stripping voltammetry (CSV) on Hg-PGEb were carried out at potentials where the reduction of copper ions took place and Cu(I)-purine complexes were formed. By using ASV and CSV in combination with EVLS, the sensitivity of Cu(I)-purine complex detection was enhanced relative to either ASV or CSV alone, resulting in higher peak currents of more than one order of magnitude. The statistical treatment of CE data was used to determine the reproducibility of measurements. Our results show that EVLS in connection with the stripping procedure is useful for both qualitative and quantitative microanalysis of purine derivatives and can also reveal details of studied electrode processes. PMID:27879715

  2. Applications of convolution voltammetry in electroanalytical chemistry.

    Science.gov (United States)

    Bentley, Cameron L; Bond, Alan M; Hollenkamp, Anthony F; Mahon, Peter J; Zhang, Jie

    2014-02-18

    The robustness of convolution voltammetry for determining accurate values of the diffusivity (D), bulk concentration (C(b)), and stoichiometric number of electrons (n) has been demonstrated by applying the technique to a series of electrode reactions in molecular solvents and room temperature ionic liquids (RTILs). In acetonitrile, the relatively minor contribution of nonfaradaic current facilitates analysis with macrodisk electrodes, thus moderate scan rates can be used without the need to perform background subtraction to quantify the diffusivity of iodide [D = 1.75 (±0.02) × 10(-5) cm(2) s(-1)] in this solvent. In the RTIL 1-ethyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide, background subtraction is necessary at a macrodisk electrode but can be avoided at a microdisk electrode, thereby simplifying the analytical procedure and allowing the diffusivity of iodide [D = 2.70 (±0.03) × 10(-7) cm(2) s(-1)] to be quantified. Use of a convolutive procedure which simultaneously allows D and nC(b) values to be determined is also demonstrated. Three conditions under which a technique of this kind may be applied are explored and are related to electroactive species which display slow dissolution kinetics, undergo a single multielectron transfer step, or contain multiple noninteracting redox centers using ferrocene in an RTIL, 1,4-dinitro-2,3,5,6-tetramethylbenzene, and an alkynylruthenium trimer, respectively, as examples. The results highlight the advantages of convolution voltammetry over steady-state techniques such as rotating disk electrode voltammetry and microdisk electrode voltammetry, as it is not restricted by the mode of diffusion (planar or radial), hence removing limitations on solvent viscosity, electrode geometry, and voltammetric scan rate.

  3. Voltammetry: mathematical modelling and Inverse Problem

    CERN Document Server

    Koshev, N A; Kuzina, V V

    2016-01-01

    We propose the fast semi-analytical method of modelling the polarization curves in the voltammetric experiment. The method is based on usage of the special func- tions and shows a big calculation speed and a high accuracy and stability. Low computational needs of the proposed algorithm allow us to state the set of Inverse Problems of voltammetry for the reconstruction of metal ions concentrations or the other parameters of the electrolyte under investigation.

  4. Adsorptive stripping voltammetric determination of imipramine, trimipramine and desipramine employing titanium dioxide nanoparticles and an Amberlite XAD-2 modified glassy carbon paste electrode.

    Science.gov (United States)

    Sanghavi, Bankim J; Srivastava, Ashwini K

    2013-03-07

    An Amberlite XAD-2 (XAD2) and titanium dioxide nanoparticles (TNPs) modified glassy carbon paste electrode (XAD2-TNP-GCPE) was developed for the determination of imipramine (IMI), trimipramine (TRI) and desipramine (DES). The electrochemical behavior of these molecules was investigated employing cyclic voltammetry (CV), chronocoulometry (CC), electrochemical impedance spectroscopy (EIS) and adsorptive stripping differential pulse voltammetry (AdSDPV). After optimization of analytical conditions using a XAD2-TNP-GCPE electrode at pH 6.0 phosphate buffer (0.1 M), the peak currents were found to vary linearly with its concentration in the range of 1.30 × 10(-9) to 6.23 × 10(-6) M for IMI, 1.16 × 10(-9) to 6.87 × 10(-6) M for TRI and 1.43 × 10(-9) to 5.68 × 10(-6) M for DES. The detection limits (S/N = 3) of 3.93 × 10(-10), 3.51 × 10(-10) and 4.35 × 10(-10) M were obtained for IMI, TRI and DES respectively using AdSDPV. The prepared modified electrode showed several advantages such as a simple preparation method, high sensitivity, very low detection limits and excellent reproducibility. The proposed method was employed for the determination of IMI, TRI and DES in pharmaceutical formulations, blood serum and urine samples.

  5. A Validated Adsorptive Stripping Voltammetric Determination of Antidiabetic Agent Pioglitazone HCl in Tablets and Biological Fluids

    Science.gov (United States)

    Al-Arfaj, Nawal Ahmad; Al-Abdulkareem, Eman Abdullah; Aly, Fatma Ahmad

    2008-01-01

    Square-wave adsorptive cathodic stripping voltammetry was used to determine pioglitazone HCl in Britton Robinson buffer of pH5. The adsorptive cathodic peak was observed at -1.5 V vs. Ag/AgCl. The peak response was characterized with respect to pH, supporting electrolyte, frequency, scan increment, pulse-amplitude, accumulation potential and pre-concentration time. Under optimal conditions, the peak current is proportional to the concentration of pioglitazone HCl, and a linear calibration graphs were obtained within the concentration levels of 10-8 and 10-4 M following different accumulation time periods (0-300 s). The obtained results were analyzed and the statistical parameters were calculated. The detection limit is 8.08 × 10-9 M (3.17 ng ml-1) using 300 s pre-concentration time, whereas the quantitative limit is 2.45 × 10-8 M (9.63 ng ml-1). The proposed method was applied to assay the drug in pharmaceutical formulations and biological fluids. The pharmacokinetic parameters of drug in human plasma were estimated as: Cmax=785.8 ng ml-1, tmax=1.5 h, Ke=0.125 h-1 and t1/2=8 h which are favorably compared with those reported in literature. PMID:23675103

  6. Cathodic Stripping Voltammetry of Thioamides on a Rotating Silver Disk Electrode.

    Science.gov (United States)

    1984-01-01

    MAR 2 1 ൒34 18 SUPPLEMENTARY NOTES Prepared for publication in the Journal of Electroanalytical Chemistry and Interfacial Electrochemistry 19 KEY...Publication in Journal Electroanalytical Chemistry And Interfacial Electrochemistry Department of Chemistry State University of New York at Buffalo

  7. The Generalized Standard Addition Method: Intermetallic Interferences in Anodic Stripping Voltammetry.

    Science.gov (United States)

    1981-02-01

    determinging the scan. -9- Reagents: HC, HNO 3, and KC were Ultrex grade, (J.T. Baker Co.); KNO3 , CH3COONa, and CH3COOH were Baker Analyzed Reagent grade...the analysis of Zn can be compensated for but not without paying a price . The theory of multicomponent *nalysis in the pre- sence of interferences (32

  8. Determination of triazines in hemodialysis saline solutions by adsorptive stripping voltammetry after extraction in acetonitrile

    Directory of Open Access Journals (Sweden)

    Nascimento Paulo Cícero do

    2003-01-01

    Full Text Available A method for the voltammetric determination of 2-methylthio-4,6-dialkylamino-1,3,5-triazine (triazines herbicides in hemodialysis (HD saline solutions was developed. The herbicides were detected in the saline solutions at the hanging mercury drop electrode (HMDE with high sensitivities only after extraction of the analytes in acetonitrile (ACN. The salting out effect originated by the saline environment existing in the solutions enabled the extractions. The volume ratio between the saline and ACN phases was investigated in order to find the best sensitivity to detect the triazines. The speciation amongst them (ametryn, desmetryn, prometryn and terbutryn was not possible. Recoveries between 88 and 107% were calculated in spiked samples, and detection limits of 0.03 mumol L-1 were calculated for the triazines in the saline samples using this methodology.

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

    Science.gov (United States)

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

    2012-01-01

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

  10. The mathematical model of the stripping voltammetry hydrogen evolution/dissolution process on Pd layer

    Energy Technology Data Exchange (ETDEWEB)

    Skital, Piotr M. [Faculty of Chemistry, Rzeszow University of Technology, Wincentego Pola Str. 2, 35-959 Rzeszow (Poland); Sanecki, Przemyslaw T., E-mail: psanecki@prz.rzeszow.p [Faculty of Chemistry, Rzeszow University of Technology, Wincentego Pola Str. 2, 35-959 Rzeszow (Poland); Kaczmarski, Krzysztof [Faculty of Chemistry, Rzeszow University of Technology, Wincentego Pola Str. 2, 35-959 Rzeszow (Poland)

    2010-08-01

    The advanced two-plate mathematical model of electrochemical hydrogen evolution/dissolution process has been presented and discussed. The model, with Langmuir adsorption equation, has been experimentally verified by the use of the glassy carbon/Pd layer electrode system at different scan rates. The two cathodic-anodic stages of hydrogen evolution/dissolution process in 0.1 M and 0.001 M HCl solutions have been interpreted and discussed. The thickness of the layer and the way of deposition were also investigated. The fundamental kinetic problem of a change of electrode properties during electrode process as an effect of the elementary hydrogen presence in the solid electrode is presented and interpreted. The isopotential point phenomenon, an electrochemical analog of isosbestic point in absorption spectroscopy, was unexpectedly discovered as experimental effect of hydrogen adsorption and {alpha} variability.

  11. Paramagnetic nanoparticle-based detection of hepatitis B virus using cathodic stripping voltammetry.

    Science.gov (United States)

    Fatemi, Kamal; Ghourchian, Hedayatollah; Ziaee, Abed-Ali; Samiei, Shahram; Hanaee, Hana

    2009-03-01

    A nanoparticle-based electrochemical method for detection of hepatitis B virus DNA sequences has been developed. This method relies on the adsorption of amplified hepatitis B virus DNA strands on to probe-coated paramagnetic particles and electrochemical detection of hybridized strands using a hanging mercury drop electrode. For hepatitis B virus detection, a combination of dynamic DNA hybridization on transportable reactive surfaces and label-free detection of DNA based on the electrochemical determination of adenines was used. Separation of the hybridization area from the detection electrode eliminates non-specific adsorption of long DNAs, and combining this method with dynamic synthesis of probe may result in new flexible approaches for detection of other infectious agents by lab-on-a-chip technology.

  12. Determination of losartan and triamterene in pharmaceutical compounds and urine using cathodic adsorptive stripping voltammetry.

    Science.gov (United States)

    Ensafi, Ali Asghar; Hajian, Reza

    2008-01-01

    A square-wave voltammetric procedure for the electroanalytical determination of losartan and triamterene in Britton-Robinson buffer (pH 3.0, 0.1 mol L(-1)) as a supporting electrolyte containing 30 ng mL(-1) of copper ions was developed. Opposite to the case of triamterene, losartan can not be reduced at a mercury electrode alone, but a new peak appears at -0.25 V in the presence of copper due to the formation of a complex between copper(II) and losartan. An accumulation potential of -0.30 V during 80 s for the prior adsorption of losartan-copper(II) and triamterene on the electrode surface was used. The response of the system was found to be linear in the range of 30.0 - 270.0 nmol L(-1) for losartan and two linear dynamic ranges containing 0.5-200.0 and 200.0-400.0 nmol L(-1) of triamterene. The limits of detections were 9.7 and 0.3 nmol L(-1) for losartan and triamterene, respectively. The relative standard deviations for five replicate analyses of 100.0 and 10.0 nmol L(-1) losartan and triamterene were 5.5%. Applicability to assay the drugs in urine and pharmaceutical formulations was illustrated with satisfactory results. The direct-current polarography of triamterene indicates that the reduction of a related drug is strongly dependent on the pH of the solution. A linear segment was found with slope value of -63.6 mV pH(-1) in the pH range of 2.0 - 6.0. The stoichiometry and complex formation constant (beta) for losartan-Cu(II), number of transfer electrons (n), transfer coefficients (alpha) and number of proton transfers were also estimated.

  13. Direct Determination of Nimesulide in Natural Waters and Wastewater by Cathodic Stripping Voltammetry.

    Science.gov (United States)

    Miranda, Luciane; Pereira, Vanessa C; Machado, Christiane S; Torres, Yohandra R; Dos Anjos, Vanessa E; Quináia, Sueli P

    2017-06-29

    Pharmaceuticals are included in a group of compounds considered as contaminants of emerging concern (CECs) in environmental matrices. The quantification of CECs is typically accomplished using chromatographic methods that require several sample pretreatment steps. The current study proposes a voltammetric method to quantify directly nimesulide (NIM) in aqueous samples. The voltammetric parameters were optimized and chosen based on the profile of the voltammograms and peak current intensity. The adequacy of the analytical method was evaluated using validation criteria, such as accuracy, selectivity, linearity, detection, and quantification limits. Linearity was assessed by a standard addition curve at a concentration range of 0.5-130 µg L(-1) of NIM. The limit of quantification was 0.50 µg L(-1), with 60 s of preconcentration time. Accuracy was expressed as recovery percentages of NIM and ranged from 111.4 to 119.8%. The voltammetric method herein proposed has several advantages over others already used to determine NIM, such as fewer sample pretreatment steps, faster, and cheaper analyses. NIM was detected in wastewater samples at concentration levels ranging from 101.7 to 385.0 µg L(-1). This result is the first evidence about NIM occurrences in environmental matrices in the area surrounding the Itaipu Lake reservoir in Brazil.

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

    Science.gov (United States)

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

    2012-01-01

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

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

    Science.gov (United States)

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

    2007-01-01

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

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

    Science.gov (United States)

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

    2008-01-01

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

  17. FIELD MEASUREMENT TECHNOLOGY FOR MERCURY IN SOIL AND SEDIMENT MTI INC'S PDV 6000 STRIPPING VOLTAMMETRY

    Science.gov (United States)

    Monitoring Technologies International Pty. Ltd. (MTI) has developed a Portable Digital Voltammeter (PDV) designed to identify and measure the concentration of heavy metal ions. MTI's PDV 6000 was demonstrated under the U.S. Environmental Protection Agency Superfund Innovative Tec...

  18. Detection of food additives by voltammetry at the liquid-liquid interface.

    Science.gov (United States)

    Herzog, Grégoire; Kam, Victor; Berduque, Alfonso; Arrigan, Damien W M

    2008-06-25

    Electrochemistry at the liquid-liquid interface enables the detection of nonredoxactive species with electroanalytical techniques. In this work, the electrochemical behavior of two food additives, aspartame and acesulfame K, was investigated. Both ions were found to undergo ion-transfer voltammetry at the liquid-liquid interface. Differential pulse voltammetry was used for the preparation of calibration curves over the concentration range of 30-350 microM with a detection limit of 30 microM. The standard addition method was applied to the determination of their concentrations in food and beverage samples such as sweeteners and sugar-free beverages. Selective electrochemically modulated liquid-liquid extraction of these species in both laboratory solutions and in beverage samples was also demonstrated. These results indicate the suitability of liquid-liquid electrochemistry as an analytical approach in food analysis.

  19. micro strip gas chamber

    CERN Multimedia

    1998-01-01

    About 16 000 Micro Strip Gas Chambers like this one will be used in the CMS tracking detector. They will measure the tracks of charged particles to a hundredth of a millimetre precision in the region near the collision point where the density of particles is very high. Each chamber is filled with a gas mixture of argon and dimethyl ether. Charged particles passing through ionise the gas, knocking out electrons which are collected on the aluminium strips visible under the microscope. Such detectors are being used in radiography. They give higher resolution imaging and reduce the required dose of radiation.

  20. [Post-stripping telangiectasis].

    Science.gov (United States)

    Hutinel, B; Maraval, M

    1985-01-01

    These telangiectasia appear between one and six months after the operation, especially in cases of capillary fragility. The most common localizations are the antero-internal and external sides of the thighs and knees. Unnecessary strippings, of continent saphenous veins, are the most frequent cause of these. Their prevention consists of the least possible traumatising stripping, using a fine stripper, a very rigorous post-operative support, and the wearing of light varicose stockings or tights for between one and three months. The treatment using microsclerosis, often delicate, should not be undertaken before six months.

  1. Determination of genotoxic effects of methidathion alkaline hydrolysis in human lymphocytes using the micronucleus assay and square-wave voltammetry.

    Science.gov (United States)

    Stivaktakis, Polychronis D; Giannakopoulos, Evangelos; Vlastos, Dimitris; Matthopoulos, Demetrios P

    2017-02-01

    The interaction of pesticides with environmental factors, such as pH, may result in alterations of their physicochemical properties and should be taken into consideration in regard to their classification. This study investigates the genotoxicity of methidathion and its alkaline hydrolysis by-products in cultured human lymphocytes, using the square-wave voltammetry (square wave-adsorptive cathodic stripping voltammetry (SW-AdCSV) technique) and the cytokinesis block micronucleus assay (CBMN assay). According to the SW-AdCSV data the alkaline hydrolysis of methidathion results in two new molecules, one non-electro-active and a second electro-active which is more genotoxic than methidathion itself in cultured human lymphocytes, inducing higher micronuclei frequencies. The present study confirms the SW-AdCSV technique as a voltammetric method which can successfully simulates the electrodynamics of the cellular membrane.

  2. Study of Copper and Purine-Copper Complexes on Modified Carbon Electrodes by Cyclic and Elimination Voltammetry

    Directory of Open Access Journals (Sweden)

    Frantisek Jelen

    2008-01-01

    Full Text Available Using a paraffin impregnated graphite electrode (PIGE and mercury-modifiedpyrolytic graphite electrode with basal orientation (Hg-PGEb copper(II and Cu(II-DNApurine base solutions have been studied by cyclic (CV and linear sweep voltammetry(LSV in connection with elimination voltammetry with linear scan (EVLS. In chlorideand bromide solutions (pH 6, the redox process of Cu(II proceeded on PIGE with twocathodic and two anodic potentially separated signals. According to the eliminationfunction E4, the first cathodic peak corresponds to the reduction Cu(II e- → Cu(I withthe possibility of fast disproportionation 2Cu(I → Cu(II Cu(0. The E4 of the secondcathodic peak signalized an electrode process controlled by a surface reaction. Theelectrode system of Cu(II on Hg-PGEb in borate buffer (pH 9.2 was characterized by onecathodic and one anodic peak. Anodic stripping voltammetry (ASV on PIGE and cathodicstripping voltammetry (CSV on Hg-PGEb were carried out at potentials where thereduction of copper ions took place and Cu(I-purine complexes were formed. By usingASV and CSV in combination with EVLS, the sensitivity of Cu(I-purine complexdetection was enhanced relative to either ASV or CSV alone, resulting in higher peakcurrents of more than one order of magnitude. The statistical treatment of CE data wasused to determine the reproducibility of measurements. Our results show that EVLS inconnection with the stripping procedure is useful for both qualitative and quantitativemicroanalysis of purine derivatives and can also reveal details of studied electrodeprocesses.

  3. Study of Copper and Purine-Copper Complexes on Modified Carbon Electrodes by Cyclic and Elimination Voltammetry.

    Science.gov (United States)

    Trnkova, Libuse; Zerzankova, Lenka; Dycka, Filip; Mikelova, Radka; Jelen, Frantisek

    2008-01-24

    Using a paraffin impregnated graphite electrode (PIGE) and mercury-modifiedpyrolytic graphite electrode with basal orientation (Hg-PGEb) copper(II) and Cu(II)-DNApurine base solutions have been studied by cyclic (CV) and linear sweep voltammetry(LSV) in connection with elimination voltammetry with linear scan (EVLS). In chlorideand bromide solutions (pH 6), the redox process of Cu(II) proceeded on PIGE with twocathodic and two anodic potentially separated signals. According to the eliminationfunction E4, the first cathodic peak corresponds to the reduction Cu(II) e⁻ → Cu(I) withthe possibility of fast disproportionation 2Cu(I) → Cu(II) Cu(0). The E4 of the secondcathodic peak signalized an electrode process controlled by a surface reaction. Theelectrode system of Cu(II) on Hg-PGEb in borate buffer (pH 9.2) was characterized by onecathodic and one anodic peak. Anodic stripping voltammetry (ASV) on PIGE and cathodicstripping voltammetry (CSV) on Hg-PGEb were carried out at potentials where thereduction of copper ions took place and Cu(I)-purine complexes were formed. By usingASV and CSV in combination with EVLS, the sensitivity of Cu(I)-purine complexdetection was enhanced relative to either ASV or CSV alone, resulting in higher peakcurrents of more than one order of magnitude. The statistical treatment of CE data wasused to determine the reproducibility of measurements. Our results show that EVLS inconnection with the stripping procedure is useful for both qualitative and quantitativemicroanalysis of purine derivatives and can also reveal details of studied electrodeprocesses.

  4. Voltammetry of redox analytes at trace concentrations with nanoelectrode ensembles.

    Science.gov (United States)

    Moretto, Ligia Maria; Pepe, Niki; Ugo, Paolo

    2004-04-19

    Gold nanoelectrodes ensembles (NEEs) have been prepared by electroless plating of Au nanoelectrode elements within the pores of a microporous polycarbonate template membrane. Cyclic voltammograms recorded in (ferrocenylmethyl) trimethylammonium hexafluorophosphate (FA(+) PF(6)(-)) solutions showed that these NEEs operate in the "total-overlap" response regime, giving well resolved peak shaped voltammograms. Experimental results show that the faradaic/background currents ratios at the NEE are independent on the total geometric area of the ensemble, so that NEE can be enlarged or miniaturized at pleasure without influencing the very favorable signal/noise ratio. Differential pulse voltammetry (DPV) at the NEE is optimized for direct determinations at trace levels. DPV at NEE allowed the determination (with no preconcentration) of trace amounts of FA(+), with a detection limit of 0.02muM. The use of NEE and DPV in cytochrome c (cyt c) solutions showed the possibility to observe the direct electrochemistry of submicromolar concentration of the protein, even without the need of adding any promoter or mediator.

  5. ALICE Silicon Strip Detector

    CERN Multimedia

    Nooren, G

    2013-01-01

    The Silicon Strip Detector (SSD) constitutes the two outermost layers of the Inner Tracking System (ITS) of the ALICE Experiment. The SSD plays a crucial role in the tracking of the particles produced in the collisions connecting the tracks from the external detectors (Time Projection Chamber) to the ITS. The SSD also contributes to the particle identification through the measurement of their energy loss.

  6. Asymmetric Marcus-Hush theory for voltammetry.

    Science.gov (United States)

    Laborda, Eduardo; Henstridge, Martin C; Batchelor-McAuley, Christopher; Compton, Richard G

    2013-06-21

    The current state-of-the-art in modeling the rate of electron transfer between an electroactive species and an electrode is reviewed. Experimental studies show that neither the ubiquitous Butler-Volmer model nor the more modern symmetric Marcus-Hush model are able to satisfactorily reproduce the experimental voltammetry for both solution-phase and surface-bound redox couples. These experimental deviations indicate the need for revision of the simplifying approximations used in the above models. Within this context, models encompassing asymmetry are considered which include different vibrational and solvation force constants for the electroactive species. The assumption of non-adiabatic electron transfer is also examined. These refinements have provided more satisfactory models of the electron transfer process and they enable us to gain more information about the microscopic characteristics of the system by means of simple electrochemical measurements.

  7. Corrosive electrochemistry of jamesonite by cyclic voltammetry

    Institute of Scientific and Technical Information of China (English)

    余润兰; 胡岳华; 邱冠周; 覃文庆

    2004-01-01

    The corrosive electrochemistry of jamesonite was studied by cyclic voltammetry. Every peak in voltammograms was identified through thermodynamic calculation. The results show an irreversible electrode process by the strong adsorption of oxidation elemental sulfur on jamesonite. A deficient-metal and sulfur-rich compound is formed under the potential of 80 mV at pH 6.86. The passive action by elemental sulfur occurs from 80 to 470 mV and S2O23- , SO24- are produced at potential over 470 mV. The anodic peak producing SO24- is inhibited due to the deposition of PbSO4 at higher potential in Na2SO4 solution. The corrosive action of jamesonite becomes strong and the redox characterization similar to PbS, FeS and Sb2 S3 appears at pH 9.18.

  8. Anodic stripping voltammetric determination of Zn, Pb and Cu traces in whisky samples

    Energy Technology Data Exchange (ETDEWEB)

    Barbeira, P.J.S. [Departamento de Quimica - ICEx - UFMG, Belo Horizonte, MG (Brazil); Stradiotto, N.R. [Departamento de Quimica - FFCLRP - USP, Ribeirao Preto, SP (Brazil)

    1998-07-01

    The simultaneous ``in natura`` determination of trace Zn, Pb and Cu in whisky samples by anodic stripping voltammetry (ASV), using a hanging mercury drop electrode, without previous treatment or addition of supporting electrolyte is described. The choice of an appropriate stripping voltammetric method and deposition potential minimizes the influence of the organic content and ensures a good reproducibility of the measurements. The reliability of the method was tested comparing the results with those of atomic absorption spectroscopy (AAS), with differences of about 10%. The method allows the determination of heavy metal ions in the {mu}g L{sup -1} range. (orig.) With 3 figs., 1 tab., 18 refs.

  9. Model predictions of copper speciation in coastal water compared to measurements by analytical voltammetry.

    Science.gov (United States)

    Ndungu, Kuria

    2012-07-17

    Trace metal toxicity to aquatic biota is highly dependent on the metaĺs chemical speciation. Accordingly, metal speciation is being incorporated in to water quality criteria and toxicity regulations using the Biotic Ligand Model (BLM) but there are currently no BLM for biota in marine and estuarine waters. In this study, I compare copper speciation measurements in a typical coastal water made using Competitive ligand exchange-adsorptive cathodic stripping voltammetry (CLE-ACSV) to model calculations using Visual MINTEQ. Both Visual MINTEQ and BLM use similar programs to model copper interactions with dissolved organic matter-DOM (i.e., the Stockholm Humic Model and WHAM-Windermere Humic Aqueous Model, respectively). The total dissolved (14). The modeled [Cu2+] could be fitted to the experimental values better after the conditional stability constant for copper binding to fulvic acid (FA) complexes in DOM in the SHM was adjusted to account for higher concentration of strong Cu-binding sites in FA.

  10. Parabolic Strip Telescope

    CERN Document Server

    Chadzitaskos, Goce

    2013-01-01

    We present a proposal of a new type of telescopes using a rotating parabolic strip as the primary mirror. It is the most principal modification of the design of telescopes from the times of Galileo and Newton. In order to demonstrate the basic idea, the image of an artificial constellation observed by this kind of telescope was reconstructed using the techniques described in this article. As a working model of this new telescope, we have used an assembly of the primary mirror---a strip of acrylic glass parabolic mirror 40 cm long and 10 cm wid shaped as a parabolic cylinder of focal length 1 m---and an artificial constellation, a set of 5 apertures in a distance of 5 m illuminated from behind. In order to reconstruct the image, we made a series of snaps, each after a rotation of the constellation by 15 degrees. Using Matlab we reconstructed the image of the artificial constellation.

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

    Science.gov (United States)

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

    2011-08-28

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

  12. Toward an in situ phosphate sensor in seawater using Square Wave Voltammetry.

    Science.gov (United States)

    Barus, C; Romanytsia, I; Striebig, N; Garçon, V

    2016-11-01

    A Square Wave Voltammetry electrochemical method is proposed to measure phosphate in seawater as pulse techniques offer a higher sensitivity as compared to classical cyclic voltammetry. Chronoamperometry cannot be either adapted for an in situ sensor since this method requires to have controlled convection which will be impossible in a miniaturised sensor. Tests and validation of Square Wave Voltammetry parameters have been performed using an open cell and for the first time with a small volume (<400µL) laboratory prototypes. Two designs of prototypes have been compared. Using high frequency (f=250Hz) allows to obtain a linear behaviour between 0.1 and 1µmolL(-1) with a very low limit of detection of 0.05 µmolL(-1) after 60min of complexation waiting time. In order to obtain a linear regression for a larger concentration range i.e. 0.25-4µmolL(-1), a lower frequency of 2.5Hz is needed. A limit of detection of 0.1µmolL(-1) is obtained in this case after 30min of complexation waiting time for the peak measured at E=0.12V. Changing the position of the molybdenum electrode for the complexation step and moving the detection into another electrochemical cell allow to decrease the reaction time down to 5min. Copyright © 2016 Elsevier B.V. All rights reserved.

  13. Dendrimer-encapsulated copper as a novel oligonucleotides label for sensitive electrochemical stripping detection of DNA hybridization.

    Science.gov (United States)

    Gao, Huan; Jiang, Xue; Dong, Yang-Jun; Tang, Wan-Xin; Hou, Cong; Zhu, Ning-Ning

    2013-10-15

    This paper describes the synthesis and characterization of a novel electrochemical label for sensitive electrochemical stripping detection of DNA hybridization based on dendrimer-encapsulated copper. The generation 4.5 (G 4.5) carboxyl-terminated poly(amidoamine) dendrimer with a trimesyl core was used as a template for synthesis of Cu²⁺/dendrimer nanocomposites (Cu-DNCs). Ratios of Cu²⁺/dendrimer were optimized in order to obtain stable nanocomposites with maximal copper loading in the interior of a polymeric shell. Cu-DNCs labeled DNA probe was employed for determining a target ssDNA immobilized on multi-walled carbon nanotubes-modified glassy carbon electrode (GCE) based on a specific hybridization reaction. The hybridization events were monitored by electrochemical detection of Cu anchored on the hybrids after the release in a diluted nitric acid by anodic stripping differential pulse voltammetry (ASDPV). The results showed that only a complementary sequence could form a dsDNA with the Cu-DNCs DNA probe and give an obvious electrochemical signal. The non-complementary sequence exhibited negligible signal change compared with the blank measurement (means: the electrode containing no target DNA incubating in hybridization buffer solution containing Cu-DNCs DNA probe for a certain time). The use of Cu encapsulated-dendrimer as tags and ASDPV for the detection of the released Cu ions could enhance the hybridization signal, and result in the increase of the sensitivity for the target DNA. Under the conditions employed here, the detection limit for measuring the full complementary sequence is down to pM level. Copyright © 2013 Elsevier B.V. All rights reserved.

  14. The renewable bismuth bulk annular band working electrode: fabrication and application in the adsorptive stripping voltammetric determination of nickel(II) and cobalt(II).

    Science.gov (United States)

    Baś, Bogusław; Węgiel, Krystian; Jedlińska, Katarzyna

    2015-06-30

    The paper presents the first report on fabrication and application of a user friendly and mercury free electrochemical sensor, with the renewable bismuth bulk annular band working electrode (RBiABE), in stripping voltammetry (SV). The sensor body is partly filled with the internal electrolyte solution, in which the RBiABE is cleaned and activated before each measurement. Time of the RBiABE contact with the sample solution is precisely controlled. The usefulness of this sensor was tested by Ni(II) and Co(II) traces determination by means of differential pulse adsorptive stripping voltammetry (DP AdSV), after complexation with dimethylglyoxime (DMG) in ammonia buffer (pH 8.2). The experimental variables (composition of the supporting electrolyte, pre-concentration potential and time, potential of the RBiABE activation, and DP parameters), as well as possible interferences, were investigated. The linear calibration graphs for Ni(II) and Co(II), determined individually and together, in the range from 1×10(-8) to 70×10(-8)molL(-1) and from 1×10(-9) to 70×10(-9)molL(-1) respectively, were obtained. The calculated limit of detection (LOD), for 30s of the accumulation time, was 3×10(-9)molL(-1) for Ni(II) in case of a single element's analysis, whereas the LOD was 5×10(-9)molL(-1) for Ni(II) and 3×10(-10)molL(-1) for Co(II), when both metal ions were measured together. The repeatability of the Ni(II) and Co(II) adsorptive stripping voltammetric signals obtained at the RBiABE were equal to 5.4% and 2.5%, respectively (n=5). Finally, the proposed method was validated by determining Ni(II) and Co(II) in the certified reference waters (SPS-SW1 and SPS-SW2) with satisfactory results.

  15. Cyclic voltammetry of fast conducting electrocatalytic films.

    Science.gov (United States)

    Costentin, Cyrille; Savéant, Jean-Michel

    2015-07-15

    In the framework of contemporary energy challenges, cyclic voltammetry is a particularly useful tool for deciphering the kinetics of catalytic films. The case of fast conducting films is analyzed, whether conduction is of the ohmic type or proceeds through rapid electron hopping. The rate-limiting factors are then the diffusion of the substrate in solution and through the film as well as the catalytic reaction itself. The dimensionless combination of the characteristics of these factors allows reducing the number of actual parameters to a maximum of two. The kinetics of the system may then be fully analyzed with the help of a kinetic zone diagram. Observing the variations of the current-potential responses with operational parameters such as film thickness, the potential scan rate and substrate concentration allows a precise assessment of the interplay between these factors and of the values of the rate controlling factors. A series of thought experiments is described in order to render the kinetic analysis more palpable.

  16. High-Rate Capable Floating Strip Micromegas

    CERN Document Server

    Bortfeldt, Jonathan; Biebel, Otmar; Danger, Helge; Flierl, Bernhard; Hertenberger, Ralf; Lösel, Philipp; Moll, Samuel; Parodi, Katia; Rinaldi, Ilaria; Ruschke, Alexander; Zibell, André

    2015-01-01

    We report on the optimization of discharge insensitive floating strip Micromegas (MICRO-MEsh GASeous) detectors, fit for use in high-energy muon spectrometers. The suitability of these detectors for particle tracking is shown in high-background environments and at very high particle fluxes up to 60MHz/cm$^2$. Measurement and simulation of the microscopic discharge behavior have demonstrated the excellent discharge tolerance. A floating strip Micromegas with an active area of 48cm$\\times$50cm with 1920 copper anode strips exhibits in 120GeV pion beams a spatial resolution of 50$\\mu$m at detection efficiencies above 95%. Pulse height, spatial resolution and detection efficiency are homogeneous over the detector. Reconstruction of particle track inclination in a single detector plane is discussed, optimum angular resolutions below $5^\\circ$ are observed. Systematic deviations of this $\\mu$TPC-method are fully understood. The reconstruction capabilities for minimum ionizing muons are investigated in a 6.4cm$\\time...

  17. 同时测定癌症病人血液中锌镉铅铜的微分脉冲阳极溶出伏安法%Simultaneous Determination of Zinc, Cadmium, Lead and Copper in Blood from Cancerous Patients by Differential Pulse Anodic Stripping Voltammetry

    Institute of Scientific and Technical Information of China (English)

    刘保启; 王玉春; 胡孝忠; 张玉华

    2003-01-01

    用微分脉冲阳极溶出伏安法同时测定癌症病人血液中的锌、镉、铅和铜,以为癌症与这 4种微量元素在血液中含量的相关性研究提供实验数据; 癌症病人血液用硝酸-高氯酸消化,消化后的白色固体加水溶解,以 0.100 mol/L硫酸铵为底液,在三电极体系中进行测定,以峰电位定性,峰电流定量; 用该法测定了 3 种癌症病人血液中的锌、镉、铅和铜,相对标准偏差为 2.9%~ 3.3% (n=6),加标回收率为 98%~ 110%; 该法不用除氧、干扰少、分辨率好、准确度高,适用于临床血液中锌、镉、铅和铜的测定和研究.

  18. Underpotential Deposition Study and Determination of Bismuth on Gold Electrode by Using Voltammetry

    Institute of Scientific and Technical Information of China (English)

    DU,Yong-Ling(杜永令); WANG,Chun-Ming(王春明)

    2002-01-01

    The cyclic voltammetry (CV) and the semidifferential anodic stripping voltanmetry (SdASV) were used for investigation of bismuth(Ⅲ) underpotential deposition (UPD) on gold electrode. Based on the excellent electrochemical properties of Au/Bi UPD system, a new method for determining bismuth (Ⅲ)was established. A solution of 0.1 mol/L HNO3 was selected as the supporting electrolyte. Factors affecting the Bi(Ⅲ) UPD and stripping steps were investigated and an opthmized analytical procedure was developed. The calibration plots for Bi(Ⅲ) concentration in the range 1.25 × 10-8-1.0 × 10-7 mol/L were obtained. The detection limit, calculated as three times the standard deviation of the analytical signal of 8.3×10-8 mol/L for a 90 s electrodeposition at 0.00 V (while the solution magnetically stirred at a speed of 300 rpm), was 7.5× 10-9 mol/ L. For8 successive determinations of 1.25 × 10-7 mol/L Bi(Ⅲ), the obtained RSD (relative standard deviation) was 0.4%. The developed method was applied to bismuth determining in medicine and urine samples. The analytical results were compared with that of atomic emission spectrometry (AES) method.

  19. Spray Rolling Aluminum Strip

    Energy Technology Data Exchange (ETDEWEB)

    Lavernia, E.J.; Delplanque, J-P; McHugh, K.M.

    2006-05-10

    Spray forming is a competitive low-cost alternative to ingot metallurgy for manufacturing ferrous and non-ferrous alloy shapes. It produces materials with a reduced number of processing steps, while maintaining materials properties, with the possibility of near-net-shape manufacturing. However, there are several hurdles to large-scale commercial adoption of spray forming: 1) ensuring strip is consistently flat, 2) eliminating porosity, particularly at the deposit/substrate interface, and 3) improving material yield. Through this program, a new strip/sheet casting process, termed spray rolling, has been developed, which is an innovative manufacturing technique to produce aluminum net-shape products. Spray rolling combines the benefits of twin-roll casting and conventional spray forming, showing a promising potential to overcome the above hurdles associated with spray forming. Spray rolling requires less energy and generates less scrap than conventional processes and, consequently, enables the development of materials with lower environmental impacts in both processing and final products. Spray Rolling was developed as a collaborative project between the University of California-Davis, the Colorado School of Mines, the Idaho National Engineering and Environmental Laboratory, and an industry team. The following objectives of this project were achieved: (1) Demonstration of the feasibility of the spray rolling process at the bench-scale level and evaluation of the materials properties of spray rolled aluminum strip alloys; and (2) Demonstration of 2X scalability of the process and documentation of technical hurdles to further scale up and initiate technology transfer to industry for eventual commercialization of the process.

  20. Cell-based chip for the detection of anticancer effect on HeLa cells using cyclic voltammetry.

    Science.gov (United States)

    El-Said, Waleed Ahmed; Yea, Cheol-Heon; Kim, Hyunhee; Oh, Byung-Keun; Choi, Jeong-Woo

    2009-01-01

    HeLa cells directly immobilized on gold-patterned silicon substrate were used to assess the biological toxicity of anticancer drugs (hydroxyurea and cyclophosphamide). Immobilization of HeLa cells was confirmed by optical microscopy, and cell growth, viability and drug-related toxicity were examined by cyclic voltammetry and potentiometric stripping analysis. The voltammetric behaviors of HeLa cells displayed a quasi-reversible pattern with the peak current exhibiting a linear relationship with cell number. The attached living cells were exposed to different concentrations of hydroxyurea and cyclophosphamide as anticancer drugs, which induced the change of cyclic voltammetry current peak. As the exposed concentration of anticancer drugs was increased, the change of current peak was increased, which indicates the decrease of cell viability. Trypan Blue dyeing was performed to confirm the results of the effect of anticancer drugs on the cell viability which was obtained from cyclic voltammetry assay. The proposed direct cell immobilization method technique can be applied to the fabrication of cell chip for diagnosis, drug detection, and on-site monitoring.

  1. Solid-state pulse forming module with adjustable pulse duration

    Science.gov (United States)

    Wang, Langning; Liu, Jinliang; Qiu, Yongfeng; Chu, Xu; Zhang, Qingmeng

    2017-03-01

    A new solid-state pulse forming module is described in this paper. The pulse forming module is fabricated on a glass ceramic substrate, with the dimension of 250 mm × 95 mm × 4 mm. By changing the copper strips used in the pulse forming modules, the pulse duration of the obtained pulsed can range from 80 ns to 140 ns. Both the simulation and tests show that the pulse forming module has a good pulse forming ability. Under a high voltage in microsecond's time, the new pulse forming modules can hold off a voltage up to 25 kV higher than that of the previous study. In addition, future optimization for the field enhancement near the thin electrode edge has been proposed and simulated.

  2. Stoichiometry and Formation Constant Determination by Linear Sweep Voltammetry.

    Science.gov (United States)

    Schultz, Franklin A.

    1979-01-01

    In this paper an experiment is described in which the equilibrium constants necessary for determining the composition and distribution of lead (II)-oxalate species may be measured by linear sweep voltammetry. (Author/BB)

  3. Anodic Stripping Determination of Pt (IV) Based on the Anodic Oxidation of Cu from the Intermetallic Phase of Cu[3]Pt

    OpenAIRE

    Ustinova, Elvira Maratovna; Kolpakova, Nina Alexandrovna

    2014-01-01

    It is shown that platinum can be determined by anodic stripping voltammetry at the peak of selective electrooxidation of copper from intermetallic phase with platinum of Cu[3]Pt composition. The composition of intermetallic copper-platinum phase formed on the electrode during pre-electrolysis was calculated on the amount of potential displacement (delta Е) of copper electrooxidation.

  4. Strip shape control capability of hot wide strip rolling mills

    Institute of Scientific and Technical Information of China (English)

    Renzhong Wang; Quan Yang; Anrui He; Jian Shao; Haitao Bian

    2008-01-01

    The elasticity deformation of rolls was analyzed by means of two-dimensional f'mite element method (FEM) with vari-able thickness. Three typical mills were used as objects for analysis. A thorough study was done on the control capabilities of these mills on the strip shape. Then the strip shape control capabilities of the three mills was compared synthetically.

  5. DNA-binding Studies of Daunorubicin in the Presence of Methylene Blue by Spectroscopy and Voltammetry Techniques

    Institute of Scientific and Technical Information of China (English)

    HAJIAN Reza; SHAMS Nafiseh; PARVIN Afsaneh

    2009-01-01

    The interaction of daunorubicin with calf thymus DNA has been investigated with the use of methylene blue dye as a spectral probe by the application of UV-Vis spectrophotometry, spectrofluorometry and voltammetry. The voltammetric behavior of daunorubicin has been investigated at a glassy carbon electrode using cyclic and differen-tial pulse voitammetry. Both UV-vis spectrophotometry and cyclic voltammetry studies confirmed the intercalation reaction. The results showed that both daunorubicin and methylene blue molecules could intercalate into the double helix of DNA. The apparent binding constant of daunorubicin with DNA has been found to be 7.8 × 104 L˙mol-1.The fluorescence signal of daunorubicin and methylene blue was quenched with DNA addition. The Stern-Volmer equation was plotted based on the quenching fluorescence signal of daunorubicin.

  6. Poly(glutamic acid) nanofibre modified glassy carbon electrode: Characterization by atomic force microscopy, voltammetry and electrochemical impedance

    Energy Technology Data Exchange (ETDEWEB)

    Santos, Daniela Pereira; Zanoni, Maria Valnice Boldrin; Bergamini, Marcio Fernando [Departamento de Quimica Analitica, Instituto de Quimica, Universidade Estadual Paulista, Caixa Postal 355, 14800-900 Araraquara, S.P. (Brazil); Chiorcea-Paquim, Ana-Maria; Diculescu, Victor Constantin [Departamento de Quimica, Faculdade de Ciencias e Tecnologia, Universidade de Coimbra, 3004-535 Coimbra (Portugal); Oliveira Brett, Ana-Maria [Departamento de Quimica, Faculdade de Ciencias e Tecnologia, Universidade de Coimbra, 3004-535 Coimbra (Portugal)], E-mail: brett@ci.uc.pt

    2008-04-20

    Glassy carbon electrodes (GCE) were modified with poly(glutamic acid) acid films prepared using three different procedures: glutamic acid monomer electropolymerization (MONO), evaporation of poly(glutamic acid) (PAG) and evaporation of a mixture of poly(glutamic acid)/glutaraldehyde (PAG/GLU). All three films showed good adherence to the electrode surface. The performance of the modified GCE was investigated by cyclic voltammetry and differential pulse voltammetry, and the films were characterized by atomic force microscopy (AFM) and electrochemical impedance spectroscopy (EIS). The three poly(glutamic acid) modified GCEs were tested using the electrochemical oxidation of ascorbic acid and a decrease of the overpotential and the improvement of the oxidation peak current was observed. The PAG modified electrode surfaces gave the best results. AFM morphological images showed a polymeric network film formed by well-defined nanofibres that may undergo extensive swelling in solution, allowing an easier electron transfer and higher oxidation peaks.

  7. Pulse on Pulse

    DEFF Research Database (Denmark)

    Schmidt, Ulrik; Carlson, Merete

    2012-01-01

    Pulse on Pulse” investigates the relation between signifying processes and non-signifying material dynamism in the installation Pulse Room (2006-) by Mexican Canadian artist Rafael Lozano-Hemmer. In Pulse Room the sense of pulse is ambiguous. Biorhythms are transmitted from the pulsing energy...... and pulsating ‘room’. Hence, the visitors in Pulse Room are invited into a complex scenario that continuously oscillates between various aspects of signification (the light bulbs representing individual lives; the pulse itself as the symbolic ‘rhythm of life’) and instants of pure material processuality...... a multilayered sense of time and space that is central to the sensory experience of Pulse Room as a whole. Pulse Room is, at the very same time, an anthropomorfized archive of a past intimacy and an all-encompassing immersive environment modulating continuously in real space-time....

  8. Analysis/design of strip reinforced random composites (strip hybrids)

    Science.gov (United States)

    Chamis, C. C.; Sinclair, J. H.

    1978-01-01

    Advanced analysis methods and composite mechanics were applied to a strip-reinforced random composite square panel with fixed ends to illustrate the use of these methods for the a priori assessment of the composite panel when subjected to complex loading conditions. The panel was assumed to be of E-glass random composite. The strips were assumed to be of three advanced unidirectional composites to cover a range of low, intermediate, and high modulus stiffness. The panels were assumed to be subjected to complex loadings to assess their adequacy as load-carrying members in auto body, aircraft engine nacelle and windmill blade applications. The results show that strip hybrid panels can be several times more structurally efficient than the random composite base materials. Some of the results are presented in graphical form and procedures are described for use of these graphs as guides for preliminary design of strip hybrids.

  9. Analysis/design of strip reinforced random composites /strip hybrids/

    Science.gov (United States)

    Chamis, C. C.; Sinclair, J. H.

    1978-01-01

    Results are described which were obtained by applying advanced analysis methods and composite mechanics to a strip-reinforced random composite square panel with fixed ends. This was done in order to illustrate the use of these methods for the apriori assessment of the composite panel when subjected to complex loading conditions. The panel was assumed to be of E-Glass/Random Composite. The strips were assumed to be of three advanced unidirectional composites to cover a range of low, intermediate, and high modulus stiffness. The panels were assumed to be subjected to complex loadings to assess their adequacy as load-carrying members in auto body, aircraft engine nacelle, and windmill blade applications. The results show that strip hybrid panels can be several times more structurally efficient than the random composite base materials. Some of the results are presented in graphical form and procedures are described for use of these graphs as guides for preliminary design of strip hybrids.

  10. Sampled-current voltammetry at microdisk electrodes: kinetic information from pseudo steady state voltammograms.

    Science.gov (United States)

    Perry, Samuel C; Al Shandoudi, Laila M; Denuault, Guy

    2014-10-07

    In sampled-current voltammetry (SCV), current transients acquired after stepping the potential along the redox wave of interest are sampled at a fixed time to produce a sigmoidal current-potential curve akin to a pseudo steady state voltammogram. Repeating the sampling for different times yields a family of sampled-current voltammograms, one for each time scale. The concept has been used to describe the current-time-potential relationship at planar electrodes but rarely employed as an electroanalytical method except in normal pulse voltammetry where the chronoamperograms are sampled once to produce a single voltammogram. Here we combine the unique properties of microdisk electrodes with SCV and report a simple protocol to analyze and compare the microdisk sampled-current voltammograms irrespective of sampling time. This is particularly useful for microelectrodes where cyclic voltammograms change shape as the mass transport regime evolves from planar diffusion at short times to hemispherical diffusion at long times. We also combine microdisk sampled-current voltammetry (MSCV) with a conditioning waveform to produce voltammograms where each data point is recorded with the same electrode history and demonstrate that the waveform is crucial to obtaining reliable sampled-current voltammograms below 100 ms. To facilitate qualitative analysis of the voltammograms, we convert the current-potential data recorded at different time scales into a unique sigmoidal curve, which clearly highlights kinetic complications. To quantitatively model the MSCVs, we derive an analytical expression which accounts for the diffusion regime and kinetic parameters. The procedure is validated with the reduction of Ru(NH3)6(3+), a model one electron outer sphere process, and applied to the derivation of the kinetic parameters for the reduction of Fe(3+) on Pt microdisks. The methodology reported here is easily implemented on computer controlled electrochemical workstations as a new

  11. Microtube strip heat exchanger

    Science.gov (United States)

    Doty, F. D.

    1991-04-01

    During the last quarter, Doty Scientific, Inc. (DSI) continued to make progress on the microtube strip (MTS) heat exchangers. The team has begun a heat exchanger stress analysis; however, they have been concentrating the bulk of their analytical energies on a computational fluid dynmaics (CFD) model to determine the location and magnitude of shell-side flow maldistribution which decreases heat exchanger effectiveness. DSI received 120 fineblanked tubestrips from Southern Fineblanking (SFB) for manufacturing process development. Both SFB and NIST provided inspection reports of the tubestrips. DSI completed the tooling required to encapsulate a tube array and press tubestrips on the array. Pressing the tubestrips on tube arrays showed design deficiencies both in the tubestrip design and the tooling design. DSI has a number of revisions in process to correct these deficiencies. The research effort has identified a more economical fusible alloy for encapsulating the tube array, and determined the parameters required to successfully encapsulate the tube array with the new alloy. A more compact MTS heat exchanger bank was designed.

  12. Magnetic stripping studies for SPL

    CERN Document Server

    Posocco, P; CERN. Geneva. BE Department

    2010-01-01

    Magnetic stripping of H- can seriously enhance the beam losses along the SPL machine. These losses depend on the beam energy, on the beam transverse distribution and on the intensity of the magnetic field. For radioprotection issues the losses must be limited to 1 W/m. In this paper we will concentrate on the stripping phenomena inside the quadrupole magnets with the aim of defining the quadrupole range for the design phase of SPL.

  13. Improved lower bound for online strip packing

    NARCIS (Netherlands)

    Harren, Rolf; Kern, Walter

    2012-01-01

    In the two-dimensional strip packing problem a number of rectangles have to be packed without rotation or overlap into a strip such that the height of the strip used is minimal. The width of the rectangles is bounded by 1 and the strip has width 1 and infinite height. We study the online version of

  14. The Dark Side of the Moebius Strip.

    Science.gov (United States)

    Schwarz, Gideon E.

    1990-01-01

    Discussed are various models proposed for the Moebius strip. Included are a discussion of a smooth flat model and two smooth flat algebraic models, some results concerning the shortest Moebius strip, the Moebius strip of least elastic energy, and some observations on real-world Moebius strips. (KR)

  15. Energy resolution in X-ray detecting micro-strip gas counters

    CERN Document Server

    Bateman, J E; Derbyshire, G E; Duxbury, D M; Mir, J A; Spill, E J; Stephenson, R

    2002-01-01

    Systematic measurements of the energy resolution available from a Micro-Strip Gas Counter (MSGC) are presented. The effect of factors such as bias potential, gas filling and strip geometry on the energy resolution are examined in detail and related to a simple model. The geometry of the MSGC is adapted to permit 'wall-less' detection of X-rays and this results in useful improvements in the pulse height spectra.

  16. Hitchhiker's Guide to Voltammetry: Acute and Chronic Electrodes for in Vivo Fast-Scan Cyclic Voltammetry.

    Science.gov (United States)

    Rodeberg, Nathan T; Sandberg, Stefan G; Johnson, Justin A; Phillips, Paul E M; Wightman, R Mark

    2017-02-15

    Fast-scan cyclic voltammetry (FSCV) has been used for over 20 years to study rapid neurotransmission in awake and behaving animals. These experiments were first carried out with carbon-fiber microelectrodes (CFMs) encased in borosilicate glass, which can be inserted into the brain through micromanipulators and guide cannulas. More recently, chronically implantable CFMs constructed with small diameter fused-silica have been introduced. These electrodes can be affixed in the brain with minimal tissue response, which permits longitudinal measurements of neurotransmission in single recording locations during behavior. Both electrode designs have been used to make novel discoveries in the fields of neurobiology, behavioral neuroscience, and psychopharmacology. The purpose of this Review is to address important considerations for the use of FSCV to study neurotransmitters in awake and behaving animals, with a focus on measurements of striatal dopamine. Common issues concerning experimental design, data collection, and calibration are addressed. When necessary, differences between the two methodologies (acute vs chronic recordings) are discussed. The topics raised in this Review are particularly important as the field moves beyond dopamine toward new neurochemicals and brain regions.

  17. Laser and optical system for laser assisted hydrogen ion beam stripping at SNS

    Science.gov (United States)

    Liu, Y.; Rakhman, A.; Menshov, A.; Webster, A.; Gorlov, T.; Aleksandrov, A.; Cousineau, S.

    2017-03-01

    Recently, a high-efficiency laser assisted hydrogen ion (H-) beam stripping was successfully carried out in the Spallation Neutron Source (SNS) accelerator. The experiment was not only an important step toward foil-less H- stripping for charge exchange injection, it also set up a first example of using megawatt ultraviolet (UV) laser source in an operational high power proton accelerator facility. This paper reports in detail the design, installation, and commissioning result of a macro-pulsed multi-megawatt UV laser system and laser beam transport line for the laser stripping experiment.

  18. Direct electrodeposition of gold nanotube arrays of rough and porous wall by cyclic voltammetry and its applications of simultaneous determination of ascorbic acid and uric acid.

    Science.gov (United States)

    Yang, Guangming; Li, Ling; Jiang, Jinhe; Yang, Yunhui

    2012-08-01

    Gold nanotube arrays of rough and porous wall has been synthesized by direct electrodeposition with cyclic voltammetry utilizing anodic aluminum oxide template (AAO) and polycarbonate membrane (PC) during short time (only 3 min and 2 min, respectively). The mechanism of the direct electrodeposition of gold nanotube arrays by cyclic voltammetry (CV) has been discussed. The morphological characterizations of the gold nanotube arrays have been investigated by scanning electron microscopy (SEM). A simultaneous determination of ascorbic acid (AA) and uric acid (UA) by differential pulse voltammetry (DPV) was constructed by attaching gold nanotube arrays (using AAO) onto the surface of a glassy carbon electrode (GCE). The electrochemical behavior of AA and UA at this modified electrode has been studied by CV and differential pulse voltammetry (DPV). The sensor offers an excellent response for AA and UA and the linear response range for AA and UA were 1.02×10(-7)-5.23×10(-4) mol L(-1) and 1.43×10(-7)-4.64×10(-4) mol L(-1), the detection limits were 1.12×10(-8) mol L(-1) and 2.24×10(-8) mol L(-1), respectively. This sensor shows good regeneration, stability and selectivity and has been used for the determination of AA and UA in real human urine and serum samples with satisfied results. Copyright © 2012 Elsevier B.V. All rights reserved.

  19. Electrooxidation of morin hydrate at a Pt electrode studied by cyclic voltammetry.

    Science.gov (United States)

    Masek, Anna; Chrzescijanska, Ewa; Zaborski, Marian

    2014-04-01

    The process and the kinetics of the electrochemical oxidation of morin in an anhydrous electrolyte have been investigated using cyclic and differential pulse voltammetry. The oxidation mechanism proceeds in sequential steps related to the hydroxyl groups in the three aromatic rings. The oxidation of the 2',4'dihydroxy moiety at the B ring of morin occurs first, at very low positive potentials, and is a one-electron, one-proton irreversible reaction. The rate constant, electron transfer coefficient and diffusion coefficients involved in the electrochemical oxidation of morin were determined. The influence of the deprotonation of the ring B hydroxyl moiety is related to the electron/proton donating capacity of morin and to its radical scavenging antioxidant activity.

  20. Pulse on Pulse

    DEFF Research Database (Denmark)

    Schmidt, Ulrik; Carlson, Merete

    2012-01-01

    and pulsating ‘room’. Hence, the visitors in Pulse Room are invited into a complex scenario that continuously oscillates between various aspects of signification (the light bulbs representing individual lives; the pulse itself as the symbolic ‘rhythm of life’) and instants of pure material processuality......“Pulse on Pulse” investigates the relation between signifying processes and non-signifying material dynamism in the installation Pulse Room (2006-) by Mexican Canadian artist Rafael Lozano-Hemmer. In Pulse Room the sense of pulse is ambiguous. Biorhythms are transmitted from the pulsing energy...... of the visitor’s beating heart to the blink of a fragile light bulb, thereby transforming each light bulb into a register of individual life. But at the same time the blinking light bulbs together produce a chaotically flickering light environment composed by various layers of repetitive rhythms, a vibrant...

  1. Fast Selective Detection of Pyocyanin Using Cyclic Voltammetry

    DEFF Research Database (Denmark)

    Alatraktchi, Fatima AlZahra'a; Andersen, Sandra Breum; Johansen, Helle Krogh;

    2016-01-01

    method to detect pyocyanin in a complex electroactive environment using commercially available electrodes. It is shown that cyclic voltammetry measurements between -1.0 V to 1.0 V reveal a potential detection window of pyocyanin of 0.58-0.82 V that is unaffected by other redox-active interferents...

  2. Fast Selective Detection of Pyocyanin Using Cyclic Voltammetry

    DEFF Research Database (Denmark)

    Al Atraktchi, Fatima Al-Zahraa; Breum Andersen, Sandra; Johansen, Helle Krogh;

    2016-01-01

    method to detect pyocyanin in a complex electroactive environment using commercially available electrodes. It is shown that cyclic voltammetry measurements between –1.0 V to 1.0 V reveal a potential detection window of pyocyanin of 0.58–0.82 V that is unaffected by other redox-active interferents...

  3. Differential cyclic voltammetry for selective and amplified detection

    NARCIS (Netherlands)

    Megen, M.J.J; Odijk, M.; Wiedemair, J.; Olthuis, W.; Berg, van den A.

    2012-01-01

    We propose to combine two existing electrochemical techniques, cyclic voltammetry (CV) and redox cycling (RC), in order to obtain amplified and selective detection of redox active species. This combination is achieved by applying CV waveforms to two electrodes spaced 1.20 mu m apart, with one of the

  4. Fast Selective Detection of Pyocyanin Using Cyclic Voltammetry

    DEFF Research Database (Denmark)

    Alatraktchi, Fatima AlZahra'a; Andersen, Sandra Breum; Johansen, Helle Krogh

    2016-01-01

    method to detect pyocyanin in a complex electroactive environment using commercially available electrodes. It is shown that cyclic voltammetry measurements between -1.0 V to 1.0 V reveal a potential detection window of pyocyanin of 0.58-0.82 V that is unaffected by other redox-active interferents...

  5. Differential cyclic voltammetry for selective and amplified detection

    NARCIS (Netherlands)

    van Megen, M.J.J.; Odijk, Mathieu; Wiedemair, Justyna; Olthuis, Wouter; van den Berg, Albert

    2012-01-01

    We propose to combine two existing electrochemical techniques, cyclic voltammetry (CV) and redox cycling (RC), in order to obtain amplified and selective detection of redox active species. This combination is achieved by applying CV waveforms to two electrodes spaced 1.20 mu m apart, with one of the

  6. A Cyclic Voltammetry Experiment for the Instrumental Analysis Laboratory.

    Science.gov (United States)

    Baldwin, Richard P.; And Others

    1984-01-01

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

  7. A Cyclic Voltammetry Experiment for the Instrumental Analysis Laboratory.

    Science.gov (United States)

    Baldwin, Richard P.; And Others

    1984-01-01

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

  8. Square wave voltammetry at the dropping mercury electrode: Theory

    Science.gov (United States)

    Christie, J.H.; Turner, J.A.; Osteryoung, R.A.

    1977-01-01

    The theoretical aspects of square wave voltammetry at the dropping mercury electrode are presented. The technique involves scanning the entire potential range of interest on a single drop of a DME. Asymmetries in the waveform as well as variations in current measurement parameters are discussed. Indications are that previous uses of the waveform may not have utilized all its capabilities.

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

    Science.gov (United States)

    Jeong, Yong-Hoon; Choe, Han-Cheol

    2015-08-01

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

  10. Elimination Voltammetry with Linear Scan as a New Detection Method for DNA Sensors

    Directory of Open Access Journals (Sweden)

    Rene Kizek

    2005-11-01

    Full Text Available The paper describes successful coupling of adsorptive transfer stripping (AdTS andelimination voltammetry with linear scan (EVLS for the resolution of reduction signals of cytosine (Cand adenine (A residues in hetero-oligodeoxynucleotides (ODNs. Short ODNs (9-mers and 20-merswere adsorbed from a small volume on a hanging mercury drop electrode (HMDE. After washing ofthe ODN-modified electrode by water and its transferring to an electrochemical cell, voltammetric curves were measured. The AdTS EVLS was able to determine of C/A ratio of ODNs through theelimination function conserving the diffusion current component and eliminating kinetic and chargingcurrent components. This function, which provides the elimination signal in a peak-counterpeak form,increased the current sensitivity for A and C resolution, and for the recognition of bases sequences inODN chains. Optimal conditions of elimination experiments such as pH, time of adsorption, and scanrate were found. The combination of EVLS with AdTS procedure can be considered as a newdetection method in a DNA sensor.

  11. Stripping voltammetric determination of mercury(II) at antimony-coated carbon paste electrode.

    Science.gov (United States)

    Ashrafi, Amir M; Vytřas, Karel

    2011-10-15

    A new procedure was elaborated to determine mercury(II) using an anodic stripping square-wave voltammetry at the antimony film carbon paste electrode (SbF-CPE). In highly acidic medium of 1M hydrochloric acid, voltammetric measurements can be realized in a wide potential window. Presence of cadmium(II) allows to separate peaks of Hg(II) and Sb(III) and apparently catalyses reoxidation of electrolytically accumulated mercury, thus allowing its determination at ppb levels. Calibration dependence was linear up to 100 ppb Hg with a detection limit of 1.3 ppb. Applicability of the method was tested on the real river water sample.

  12. Restitution of enamel after interdental stripping.

    Science.gov (United States)

    Lundgren, T; Milleding, P; Mohlin, B; Nannmark, U

    1993-01-01

    This paper studies the effect of interdental stripping on the enamel surface and evaluates methods to restitute the treated surface. Extracted teeth mounted in a semielastic material were subjected to stripping by different kinds of steel strips. The treated enamel surfaces were then polished in several different ways. The effects were studied by SEM and profilometry. It was concluded that the coarsest strips produced irregularities of such a magnitude that polishing had very limited effect. Polishing starting with coarse polishing strips followed by gradually finer gave the best result. An increase in number of strokes and use of all grades of polishing strips slightly improved the result.

  13. Thin-film voltammetry and its analytical applications: a review.

    Science.gov (United States)

    Tian, Huihui; Li, Yunchao; Shao, Huibo; Yu, Hua-Zhong

    2015-01-15

    Electrochemical reactions at the interfaces of immiscible electrolyte solutions (ITIES) are of fundamental importance in the fields of chemical, biological and pharmaceutical sciences. Four-electrode cell setup, scanning electrochemical microscopy (SECM) and thin-film voltammetry are the three most frequently used methods for studying the electrochemical processes at these interfaces. The principle, experimental design, advantages and challenges of the three methods are described and compared. The thin-film voltammetry is highlighted for its simplicity in experimental operation and kinetic data analysis. Its versatile analytical applications are discussed in detail, including the study of redox properties of hydrophobic compounds, evaluation of interfacial electron transfer kinetics, synthesis of nanoparticles/nanostructures, and illustration of cross-membrane ion transport phenomena.

  14. Monolayer Assemblies of a De Novo Designed 4-alpha-Helix Bundle Carboprotein and Its Sulfur Anchor Fragment on Au(111) Surfaces Addressed by Voltammetry and In Situ Scanning Tunneling Microscopy

    DEFF Research Database (Denmark)

    Brask, Jesper; Wackerbarth, Hainer; Jensen, Knud J.

    2003-01-01

    carboprotein without thiol anchor have been prepared and investigated for comparison. Cyclic and differential pulse voltammetry (DPV) of the proteins show desorption peaks around -750 mV (SCE), whereas the thiol anchor desorption peak is at -685 mV. The peaks are by far the highest for thiol monomeric 4-R...

  15. A compact high-voltage pulse generator based on pulse transformer with closed magnetic core.

    Science.gov (United States)

    Zhang, Yu; Liu, Jinliang; Cheng, Xinbing; Bai, Guoqiang; Zhang, Hongbo; Feng, Jiahuai; Liang, Bo

    2010-03-01

    A compact high-voltage nanosecond pulse generator, based on a pulse transformer with a closed magnetic core, is presented in this paper. The pulse generator consists of a miniaturized pulse transformer, a curled parallel strip pulse forming line (PFL), a spark gap, and a matched load. The innovative design is characterized by the compact structure of the transformer and the curled strip PFL. A new structure of transformer windings was designed to keep good insulation and decrease distributed capacitance between turns of windings. A three-copper-strip structure was adopted to avoid asymmetric coupling of the curled strip PFL. When the 31 microF primary capacitor is charged to 2 kV, the pulse transformer can charge the PFL to 165 kV, and the 3.5 ohm matched load can deliver a high-voltage pulse with a duration of 9 ns, amplitude of 84 kV, and rise time of 5.1 ns. When the load is changed to 50 ohms, the output peak voltage of the generator can be 165 kV, the full width at half maximum is 68 ns, and the rise time is 6.5 ns.

  16. New Cyclic Voltammetry Method for Examining Phase Transitions: Simulated Results

    OpenAIRE

    2006-01-01

    We propose a new experimental technique for cyclic voltammetry, based on the first-order reversal curve (FORC) method for analysis of systems undergoing hysteresis. The advantages of this electrochemical FORC (EC-FORC) technique are demonstrated by applying it to dynamical models of electrochemical adsorption. The method can not only differentiate between discontinuous and continuous phase transitions, but can also quite accurately recover equilibrium behavior from dynamic analysis of systems...

  17. Surface Catalytic Mechanism in Square-Wave Voltammetry

    OpenAIRE

    Mirceski, Valentin; Gulaboski, Rubin

    2001-01-01

    A pseudo-first-order catalytic mechanism in which both reactant and product of the redox reaction are strongly immobilized on the electrode surface is theoretically analyzed under conditions of square-wave voltammetry (SWV). A mathematical procedure is developed for diffusionless conditions. The relationships between the properties of the voltammetric response and both the kinetic parameters of the redox reaction and the parameters of the excitement signal are studied. The phenomenon...

  18. Determination of ziram in vegetable samples by square wave voltammetry

    Institute of Scientific and Technical Information of China (English)

    Ping Qiu; Yong Nian Ni

    2008-01-01

    The electrochemical behaviour and electrode reaction mechanism of ziram (zinc-dimethyl dithiocarbamate) on a hanging mercury drop electrode were investigated in Britton-Robinson (B-R) buffer by using cyclic and square wave voltammetry (SWV).Based on these studies a voltammetric method for determination of ziram was developed and applied to determine the ziram in synthetic and spiked vegetable samples,satisfactory results were obtained in both eases.

  19. Hardy spaces for the strip

    Science.gov (United States)

    Bakan, Andrew; Kaijser, Sten

    2007-09-01

    In this paper we shall study Hardy spaces of analytic functions in a strip . Our main result is on one hand an intrinsic characterization of the spaces and on the second that polynomials are dense. We also present an orthogonal (in ) basis of polynomials.

  20. Heavy metal distribution in organic and siliceous marine sponge tissues measured by square wave anodic stripping voltammetry.

    Science.gov (United States)

    Illuminati, S; Annibaldi, A; Truzzi, C; Scarponi, G

    2016-10-15

    May sponge spicules represent a "tank" to accumulate heavy metals? In this study we test this hypothesis determining the distribution of Cd, Pb and Cu concentrations between organic and siliceous tissues in Antarctic Demospongia (Sphaerotylus antarcticus, Kirkpatrikia coulmani and Haliclona sp.) and in the Mediterranean species Petrosia ficiformis. Results show that although, in these sponges, spicules represent about 80% of the mass content, the accumulation of pollutant is lower in the spicules than in the corresponding organic fraction. The contribution of tissues to the total sponge content of Cd, Pb and Cu is respectively 99%, 82% and 97% for Antarctic sponges and 96%, 95% and 96% for P. ficiformis, similar in polar and temperate organisms. These results pave the way to a better understanding of the role of marine sponges in uptaking heavy metals and to their possible use as monitor of marine ecosystems, recommend by the Water Framework Directive. Copyright © 2016 Elsevier Ltd. All rights reserved.

  1. Elimination of the copper-zinc interference in anodic stripping voltammetry by addition of a complexing agent.

    Science.gov (United States)

    Brandes Marques, A L; Chierice, G O

    1991-07-01

    The addition of cyanide and Triton X-100 suppress the formation of the CuZn intermetallic compound in ASV making it possible to determine traces of zinc(II) in the presence of an excess of copper ions. The precision of the method (5%) and the accuracy (error of 1.4%) in sea water are satisfactory.

  2. Solution voltammetry of 4 nm magnetite iron oxide nanoparticles.

    Science.gov (United States)

    Roberts, Joseph J P; Westgard, John A; Cooper, Laura M; Murray, Royce W

    2014-07-30

    The voltammetry of solution-dispersed magnetite iron oxide Fe3O4 nanoparticles is described. Their currents are controlled by nanoparticle transport rates, as shown with potential step chronoamperometry and rotated disk voltammetry. In pH 2 citrate buffer with added NaClO4 electrolyte, solution cyclic voltammetry of these nanoparticles (average diameter 4.4 ± 0.9 nm, each containing ca. 30 Fe sites) displays an electrochemically irreversible oxidation with E(PEAK) at ca. +0.52 V and an irreversible reduction with E(PEAK) at ca. +0.2 V vs Ag/AgCl reference electrode. These processes are presumed to correspond to the formal potentials for one-electron oxidation of Fe(II) and reduction of Fe(III) at their different sites in the magnetite nanoparticle structure. The heterogeneous electrode reaction rates of the nanoparticles are very slow, in the 10(-5) cm/s range. The nanoparticles are additionally characterized by a variety of tools, e.g., TEM, UV/vis, and XPS spectroscopies.

  3. H- Beam Stripping Loss at Background Partial Pressure of Ar

    Institute of Scientific and Technical Information of China (English)

    Hu Chundong; Wang Shaohu; Hu Liqun

    2005-01-01

    It has been observed that H- current could be improved by adding Ar to H2 plasma.But due to a slower pumping speed for Ar with the existing pumping scheme, the tank pressure will increase quickly during the length of a beam pulse. Since H- stripping loss depends on the tank pressure and gas species, part of the H- beam can be converted to H0 and then H0 can be converted into H+ with background H2 and Ar gas thickness. Therefore, the H- beam current,measured by a Faraday cup, situated at a distance L from GG (ground grid), will decrease because it will be converted into a H+ current. This gives a ratio of the Faraday cup net current to the H- beam current before stripping at background partial pressure of Ar.

  4. Intraply Hybrid Composites Would Contain Control Strips

    Science.gov (United States)

    Chamis, Christos C.; Shiao, Chi-Yu

    1996-01-01

    "Smart" structural components with sensors and/or actuators distributed throughout their volumes made of intraply hybrid composite materials, according to proposal. Strips of hybrid control material interspersed with strips of ordinary (passive) composite material in some layers, providing distributed control capability. For example, near and far edges of plate bent upward by commanding bottom control strips to expand and simultaneously commanding upper control strips to contract.

  5. Industrial 2-kW TEA CO2 laser for paint stripping of aircraft

    Science.gov (United States)

    Schweizer, Gerhard; Werner, L.

    1995-03-01

    Paint stripping of aircraft with pulsed laser radiation has several advantages compared to traditional methods of depainting: selective removal of individual layers possible, suitable for sensitive surfaces, workpiece ready for immediate repainting, and considerable reduction of contaminated waste. For paint stripping of large aircraft pulsed lasers with average power of at least 2 kW are required. Amongst the various types of pulsed lasers technical and economical considerations clearly favor TEA CO2 lasers for this application. The first commercially available TEA CO2 laser with an average power in excess of 2 kW, especially designed for depainting, has been developed by Urenco. The key data of this laser are: pulse energy up to 9 J, repetition rate up to 330 Hz, and beam quality: `flat top'.

  6. Adsorption and desorption of bis-(3-sulfopropyl) disulfide during Cu electrodeposition and stripping at Au electrodes.

    Science.gov (United States)

    Chiu, Yong-Da; Dow, Wei-Ping; Krug, Klaus; Liu, Yung-Fang; Lee, Yuh-Lang; Yau, Shueh-Lin

    2012-10-09

    The adsorption and desorption of bis-(3-sulfopropyl) disulfide (SPS) on Cu and Au electrodes and its electrochemical effect on Cu deposition and dissolution were examined using cyclic voltammetry stripping (CVS), field-emission scanning electron microscopy (FESEM), and X-ray photoelectron spectroscopy (XPS). SPS dissociates into 3-mercapto-1-propanesulfonate when it is contacted with Au and Cu electrodes, producing Cu(I)- and Au(I)-thiolate species. These thiolates couple with chloride ions and promote not only the reduction of Cu(2+) in Cu deposition but also the oxidation of Cu(0) to Cu(+) in Cu stripping. During Cu electrodeposition on the SPS-modified Au electrode, thiolates transfer from Au onto the Cu underpotential deposition (UPD) layer. The Cu UPD layer stabilizes a large part of the transferred thiolates which subsequently is buried by the Cu overpotential deposition (OPD) layer. The buried thiolates reappear on the Au electrode after the copper deposit is electrochemically stripped off. A much smaller part of thiolates transfers to the top of the Cu OPD layer. In contrast, when SPS preadsorbs on a Cu-coated Au electrode, almost all of the adsorbed SPS leaves the Cu surface during Cu electrochemical stripping and does not return to the uncovered Au surface. A reaction mechanism is proposed to explain these results.

  7. Using Comic Strips in Language Classes

    Science.gov (United States)

    Csabay, Noémi

    2006-01-01

    The author believes that using comic strips in language-learning classes has three main benefits. First, comic strips motivate younger learners. Second, they provide a context and logically connected sentences to help language learning. Third, their visual information is helpful for comprehension. The author argues that comic strips can be used in…

  8. Fast variation method for elastic strip calculation.

    Science.gov (United States)

    Biryukov, Sergey V

    2002-05-01

    A new, fast, variation method (FVM) for determining an elastic strip response to stresses arbitrarily distributed on the flat side of the strip is proposed. The remaining surface of the strip may have an arbitrary form, and it is free of stresses. The FVM, as well as the well-known finite element method (FEM), starts with the variational principle. However, it does not use the meshing of the strip. A comparison of FVM results with the exact analytical solution in the special case of shear stresses and a rectangular strip demonstrates an excellent agreement.

  9. Antenna structure with distributed strip

    Science.gov (United States)

    Rodenbeck, Christopher T.

    2008-03-18

    An antenna comprises electrical conductors arranged to form a radiating element including a folded line configuration and a distributed strip configuration, where the radiating element is in proximity to a ground conductor. The folded line and the distributed strip can be electrically interconnected and substantially coplanar. The ground conductor can be spaced from, and coplanar to, the radiating element, or can alternatively lie in a plane set at an angle to the radiating element. Embodiments of the antenna include conductor patterns formed on a printed wiring board, having a ground plane, spacedly adjacent to and coplanar with the radiating element. Other embodiments of the antenna comprise a ground plane and radiating element on opposed sides of a printed wiring board. Other embodiments of the antenna comprise conductors that can be arranged as free standing "foils". Other embodiments include antennas that are encapsulated into a package containing the antenna.

  10. In situ generation and detection of methyl radical by voltammetry

    Institute of Scientific and Technical Information of China (English)

    2003-01-01

    In persulfate-acetate, dimethyl sulfoxide or tert-butyl alcohol systems, in situ generation and detection of methyl free radical are realized with voltammetry. It includes the following successive processes. The persulfate S2O82- is polarographically reduced via one-electron addition to sulfate radical SO4-., the SO4-. Initiates chain reaction with acetate, dimethyl sulfoxide, or tert-butyl alcohol on the electrode surface to produce a methyl radical, and one-electron reduction of the methyl radical yields its polarographic reduction wave. In comparison with the known techniques such as ultraviolet radiolysis coupling with electron spin resonance, etc., the proposed method is simple, sensitive and selective.

  11. Analysis of captopril in surface waters by differential pulse voltammetry method

    Energy Technology Data Exchange (ETDEWEB)

    Baranowska, I.; Markowski, P.; Wilk, K.

    2009-07-01

    One of the important problems concerning waters ecosystems is the presence of pharmaceuticals remains in different kinds of surface waters. These compounds cause huge changes in waters environment. They cause genetic changes in water organisms, are not also neutral for people in case of penetrating into drinking water. (Author)

  12. Strategies for low detection limit measurements with cyclic voltammetry.

    Science.gov (United States)

    Wiedemann, D J; Kawagoe, K T; Kennedy, R T; Ciolkowski, E L; Wightman, R M

    1991-12-15

    Cyclic voltammetry of Nafion-coated, carbon-fiber electrodes is used to detect trace concentrations of dopamine, both in a flow injection apparatus and in the brain of an anaesthetized rat. To improve signal-to-noise ratios, the sources of noise during cyclic voltammetry have been determined and strategies have been developed to decrease the noise. With the potentiostat employed, the measured noise is comparable to that expected for Johnson noise from the feedback resistor of the current transducer. Additional noise arises from the waveform generator employed and, in some cases, line noise. Line noise is discriminated against by starting each cyclic voltammogram either in phase or 180 degrees out of phase with the line frequency. When used in vivo, additional noise also arises from the physiological activity of the animal. Detection limits are found to closely correspond to those predicted on the basis of simulation of the voltammetric shape and the measured noise. Detection limits are improved by the use of appropriate analog and digital filtering, ensemble averaging, and appropriate timing of repetitive cyclic voltammograms. The combined use of these techniques enables the in vivo detection of approximately 100 nM of dopamine with a signal-to-noise ratio of 25.

  13. Thin film voltammetry of metabolic enzymes in rat liver microsomes

    Science.gov (United States)

    Krishnan, Sadagopan; Rusling, James F.

    2007-01-01

    We report herein thin film voltammetry and kinetics of electron transfer for redox proteins in rat liver microsomes for the first time. Films were made layer-by-layer from liver microsomes and polycations on pyrolytic graphite electrodes. Cyclic voltammograms were chemically reversible with a midpoint potential of −0.48 V vs SCE at 0.1 V s−1 in pH 7.0 phosphate buffer. Reduction peak potentials shifted negative at higher scan rates, and oxidation-reduction peak current ratios were ∼1 consistent with non-ideal quasireversible thin film voltammetry. Analysis of oxidation-reduction peak separations gave an average apparent surface electron transfer rate constant of 30 s−1. Absence of significant electrocatalytic reduction of O2 or H2O2 and lack of shift in midpoint potential when CO is added that indicates lack of an iron heme cofactor suggest that peaks can be attributed to oxidoreductases present in the microsomes rather than cytochrome P450 enzymes. PMID:18037986

  14. Buffer strips in composites at elevated temperature

    Science.gov (United States)

    Bigelow, C. A.

    1983-01-01

    The composite material 'buffer strip' concept is presently investigated at elevated temperatures for the case of graphite/polyimide buffer strip panels using a (45/0/45/90)2S layup, where the buffer strip material was 0-deg S-glass/polyimide. Each panel was loaded in tension until it failed, and radiographs and crack opening displacements were recorded during the tests to determine fracture onset, fracture arrest, and the extent of damage in the buffer strip after crack arrest. At 177 + or - 3 C, the buffer strips increased the panel strength by at least 40 percent in comparison with panels without buffer strips. Compared to similar panels tested at room temperature, those tested at elevated temperature had lower residual strengths, but higher failure strains.

  15. Stripping, Sex, and Popular Culture

    OpenAIRE

    Roach, Catherine M.

    2007-01-01

    At the heart of Stripping, Sex, and Popular Culture lies a very personal story, of author Catherine Roach's response to the decision of her life-long best friend to become an exotic dancer. Catherine and Marie grew up together in Canada and moved to the USA to enroll in PhD programs at prestigious universities. For various reasons, Marie left her program and instead chose to work as a stripper. The author, at first troubled and yet fascinated by her friend's decision, follows Marie's journey ...

  16. 3D silicon strip detectors

    Energy Technology Data Exchange (ETDEWEB)

    Parzefall, Ulrich [Physikalisches Institut, Universitaet Freiburg, Hermann-Herder-Str. 3, D-79104 Freiburg (Germany)], E-mail: ulrich.parzefall@physik.uni-freiburg.de; Bates, Richard [University of Glasgow, Department of Physics and Astronomy, Glasgow G12 8QQ (United Kingdom); Boscardin, Maurizio [FBK-irst, Center for Materials and Microsystems, via Sommarive 18, 38050 Povo di Trento (Italy); Dalla Betta, Gian-Franco [INFN and Universita' di Trento, via Sommarive 14, 38050 Povo di Trento (Italy); Eckert, Simon [Physikalisches Institut, Universitaet Freiburg, Hermann-Herder-Str. 3, D-79104 Freiburg (Germany); Eklund, Lars; Fleta, Celeste [University of Glasgow, Department of Physics and Astronomy, Glasgow G12 8QQ (United Kingdom); Jakobs, Karl; Kuehn, Susanne [Physikalisches Institut, Universitaet Freiburg, Hermann-Herder-Str. 3, D-79104 Freiburg (Germany); Lozano, Manuel [Instituto de Microelectronica de Barcelona, IMB-CNM, CSIC, Barcelona (Spain); Pahn, Gregor [Physikalisches Institut, Universitaet Freiburg, Hermann-Herder-Str. 3, D-79104 Freiburg (Germany); Parkes, Chris [University of Glasgow, Department of Physics and Astronomy, Glasgow G12 8QQ (United Kingdom); Pellegrini, Giulio [Instituto de Microelectronica de Barcelona, IMB-CNM, CSIC, Barcelona (Spain); Pennicard, David [University of Glasgow, Department of Physics and Astronomy, Glasgow G12 8QQ (United Kingdom); Piemonte, Claudio; Ronchin, Sabina [FBK-irst, Center for Materials and Microsystems, via Sommarive 18, 38050 Povo di Trento (Italy); Szumlak, Tomasz [University of Glasgow, Department of Physics and Astronomy, Glasgow G12 8QQ (United Kingdom); Zoboli, Andrea [INFN and Universita' di Trento, via Sommarive 14, 38050 Povo di Trento (Italy); Zorzi, Nicola [FBK-irst, Center for Materials and Microsystems, via Sommarive 18, 38050 Povo di Trento (Italy)

    2009-06-01

    While the Large Hadron Collider (LHC) at CERN has started operation in autumn 2008, plans for a luminosity upgrade to the Super-LHC (sLHC) have already been developed for several years. This projected luminosity increase by an order of magnitude gives rise to a challenging radiation environment for tracking detectors at the LHC experiments. Significant improvements in radiation hardness are required with respect to the LHC. Using a strawman layout for the new tracker of the ATLAS experiment as an example, silicon strip detectors (SSDs) with short strips of 2-3 cm length are foreseen to cover the region from 28 to 60 cm distance to the beam. These SSD will be exposed to radiation levels up to 10{sup 15}N{sub eq}/cm{sup 2}, which makes radiation resistance a major concern for the upgraded ATLAS tracker. Several approaches to increasing the radiation hardness of silicon detectors exist. In this article, it is proposed to combine the radiation hard 3D-design originally conceived for pixel-style applications with the benefits of the established planar technology for strip detectors by using SSDs that have regularly spaced doped columns extending into the silicon bulk under the detector strips. The first 3D SSDs to become available for testing were made in the Single Type Column (STC) design, a technological simplification of the original 3D design. With such 3D SSDs, a small number of prototype sLHC detector modules with LHC-speed front-end electronics as used in the semiconductor tracking systems of present LHC experiments were built. Modules were tested before and after irradiation to fluences of 10{sup 15}N{sub eq}/cm{sup 2}. The tests were performed with three systems: a highly focused IR-laser with 5{mu}m spot size to make position-resolved scans of the charge collection efficiency, an Sr{sup 90}{beta}-source set-up to measure the signal levels for a minimum ionizing particle (MIP), and a beam test with 180 GeV pions at CERN. This article gives a brief overview of

  17. Adsorptive stripping voltammetric determination of chromium in gallium.

    Science.gov (United States)

    Palrecha, M M; Mathur, P K

    1997-12-19

    The electroanalytical chemistry of trace metals has progressed strongly with the development of cathodic stripping voltammetry (CSV) preceded by adsorption collection of organic metal complexes. A sensitive method for the determination of trace amount of chromium in gallium is described. Gallium is dissolved in sodium hydroxide containing hydrogen peroxide. The method is based on the catalytic activity of nitrate ions on the reduction of Cr(III)TTHA (triethylene tetramine-N,N,N',N'',N''',N'''-hexaacetic acid) complex. The sensitivity of this method is further improved by adsorption preconcentration of Cr(III)TTHA complex at a hanging mercury drop electrode (HMDE). The Cr(III) formed at the electrode surface by the reduction of Cr(VI), which is present in the bulk solution, is immediately complexed by TTHA. The adsorbed complex is then reduced at a peak potential of - 1.26 V, and the peak height of Cr(III) reduction is measured. The determination limit was restricted by the amount of chromium present in the reagent blank solution. The method is suitable for the determination of chromium at level as low as 0.2 mug g(-1) (with about 50 mg of sample) and a relative standard deviation of 15%.

  18. Adsorptive stripping voltammetric determination of the antidepressant drug sulpiride.

    Science.gov (United States)

    Farghaly, O A

    2000-10-01

    The electrochemical behaviour of the antidepressant drug sulpiride (SP) at a hanging mercury drop electrode (HMDE) is investigated. Linear sweep cathodic stripping voltammetry (LSCSV) was used to determine sulpiride in the presence of 0.01 M sodium acetate medium pH 10.5 and 25 +/- 1 degrees C. Different parameters such as, supporting electrolyte, pH, accumulation potential, scan rate, accumulation time and ionic strength, were tested to optimize the conditions for the determination of SP. The adsorbed form is reduced irreversibly. The linear concentration range is from 2 x 10(-9) to 5 x 10(-8) M SP. Experimentally, 2 x 10(-9) M (0.68 ppb) with accumulation time 60 s can be determined successfully. Furthermore, a theoretical detection limit of 2 x 10(-10) M (0.068 ppb) Sp was calculated. The interferences of some metal ions, ascorbic acid and some amino acids were studied. The method was applied to the analysis of tablets and spiked urine, with recoveries of 104 +/- 3 and 101 + 3, and the relative standard deviation of 3.3 and 3.4%, respectively.

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

    Energy Technology Data Exchange (ETDEWEB)

    Ammar, Hafedh Belhadj, E-mail: hbelhadjammar@yahoo.fr; Brahim, Mabrouk Ben; Abdelhédi, Ridha; Samet, Youssef

    2016-02-01

    The performance of boron-doped diamond (BDD) electrode for the detection of metronidazole (MTZ) as the most important drug of the group of 5-nitroimidazole was proven using cyclic voltammetry (CV) and square wave voltammetry (SWV) techniques. A comparison study between BDD, glassy carbon and silver electrodes on the electrochemical response was carried out. The process is pH-dependent. In neutral and alkaline media, one irreversible reduction peak related to the hydroxylamine derivative formation was registered, involving a total of four electrons. In acidic medium, a prepeak appears probably related to the adsorption affinity of hydroxylamine at the electrode surface. The BDD electrode showed higher sensitivity and reproducibility analytical response, compared with the other electrodes. The higher reduction peak current was registered at pH 11. Under optimal conditions, a linear analytical curve was obtained for the MTZ concentration in the range of 0.2–4.2 μmol L{sup −1}, with a detection limit of 0.065 μmol L{sup −1}. - Highlights: • SWV for the determination of MTZ • Boron-doped diamond as a new electrochemical sensor • Simple and rapid detection of MTZ • Efficiency of BDD for sensitive determination of MTZ.

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

    Science.gov (United States)

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

    2016-02-01

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

  1. Optimizing the Stripping Procedure for LHCb

    CERN Document Server

    Richardson, Rachel

    2017-01-01

    The LHCb experiment faces a major challenge from the large amounts of data received while the LHC is running. The ability to sort this information in a useful manner is important for working groups to perform physics analyses. Both hardware and software triggers are used to decrease the data rate and then the stripping process is used to sort the data into streams and further into stripping lines. This project studies the hundreds of stripping lines to look for overlaps between them in order to make the stripping process more efficient.

  2. Noise considerations of the Beetle amplifier used with long silicon strip detectors

    CERN Document Server

    Köstner, S

    2005-01-01

    An attempt is made to predict the thermal noise and the shot noise for silicon strip detectors connected to the Beetle preamplifier from basic electronic noise principles. The calibration pulse shapes are used to determine the frequency dependant gain function of the Beetle. The calculated noise values are compared with measurements on the prototype ladders. In addition the signal propagation in the very long ladders is studied using a spice simulation. From this the effect of the thermal noise originating from the ohmic resistors of the detector readout strips is estimated.

  3. Robotic voltammetry with carbon nanotube-based sensors: a superb blend for convenient high-quality antimicrobial trace analysis

    Science.gov (United States)

    Theanponkrang, Somjai; Suginta, Wipa; Weingart, Helge; Winterhalter, Mathias; Schulte, Albert

    2015-01-01

    A new automated pharmacoanalytical technique for convenient quantification of redox-active antibiotics has been established by combining the benefits of a carbon nanotube (CNT) sensor modification with electrocatalytic activity for analyte detection with the merits of a robotic electrochemical device that is capable of sequential nonmanual sample measurements in 24-well microtiter plates. Norfloxacin (NFX) and ciprofloxacin (CFX), two standard fluoroquinolone antibiotics, were used in automated calibration measurements by differential pulse voltammetry (DPV) and accomplished were linear ranges of 1–10 μM and 2–100 μM for NFX and CFX, respectively. The lowest detectable levels were estimated to be 0.3±0.1 μM (n=7) for NFX and 1.6±0.1 μM (n=7) for CFX. In standard solutions or tablet samples of known content, both analytes could be quantified with the robotic DPV microtiter plate assay, with recoveries within ±4% of 100%. And recoveries were as good when NFX was evaluated in human serum samples with added NFX. The use of simple instrumentation, convenience in execution, and high effectiveness in analyte quantitation suggest the merger between automated microtiter plate voltammetry and CNT-supported electrochemical drug detection as a novel methodology for antibiotic testing in pharmaceutical and clinical research and quality control laboratories. PMID:25670899

  4. Affecting of aquatic vascular plant Lemna minor by cisplatin revealed by voltammetry.

    Science.gov (United States)

    Supalkova, Veronika; Beklova, Miroslava; Baloun, Jiri; Singer, Christoph; Sures, Bernd; Adam, Vojtech; Huska, Dalibor; Pikula, Jiri; Rauscherova, Libuse; Havel, Ladislav; Zehnalek, Josef; Kizek, Rene

    2008-02-01

    Within the context of application of platinum derivates based effective cytostatics, we can suppose that these risk metals can get into aquatic ecosystems where they can show biologic availability for food chain. In the present work we report on investigation of affecting of duckweed (Lemna minor) by various doses of cisplatin (0, 5, 10, 20, 40, 80 and 160 microM) for 4 days. The toxic influence of cisplatin was evaluated on the basis of growth inhibition expressed as number of leaves, growth rate, and total amount of biomass. The result value of 96hEC50, calculated from growth inhibition with comparison of growth rates, was 6.93 microM. Moreover we aimed on determination of cisplatin content using differential pulse voltammetry. The highest content of cisplatin (320 ng g(-1) of fresh weight) was determined in plants treated by 80 microM at the second day of treatment. Plants protect themselves against heavy metals by means of synthesis of cysteine-rich peptides such as glutathione and phytochelatins. Thus thiol determination in the treated plants by means of Brdicka reaction followed. The marked increase in thiol concentration detected is associated with defence reaction of the plant against stress caused by cisplatin.

  5. Removal of Differential Capacitive Interferences in Fast-Scan Cyclic Voltammetry.

    Science.gov (United States)

    Johnson, Justin A; Hobbs, Caddy N; Wightman, R Mark

    2017-06-06

    Due to its high spatiotemporal resolution, fast-scan cyclic voltammetry (FSCV) at carbon-fiber microelectrodes enables the localized in vivo monitoring of subsecond fluctuations in electroactive neurotransmitter concentrations. In practice, resolution of the analytical signal relies on digital background subtraction for removal of the large current due to charging of the electrical double layer as well as surface faradaic reactions. However, fluctuations in this background current often occur with changes in the electrode state or ionic environment, leading to nonspecific contributions to the FSCV data that confound data analysis. Here, we both explore the origin of such shifts seen with local changes in cations and develop a model to account for their shape. Further, we describe a convolution-based method for removal of the differential capacitive contributions to the FSCV current. The method relies on the use of a small-amplitude pulse made prior to the FSCV sweep that probes the impedance of the system. To predict the nonfaradaic current response to the voltammetric sweep, the step current response is differentiated to provide an estimate of the system's impulse response function and is used to convolute the applied waveform. The generated prediction is then subtracted from the observed current to the voltammetric sweep, removing artifacts associated with electrode impedance changes. The technique is demonstrated to remove select contributions from capacitive characteristics changes of the electrode both in vitro (i.e., in flow-injection analysis) and in vivo (i.e., during a spreading depression event in an anesthetized rat).

  6. Solidification Structure of Low Carbon Steel Strips with Different Phosphorus Contents Produced by Strip Casting

    Institute of Scientific and Technical Information of China (English)

    Na LI; Zhenyu LIU; Yiqing QIU; Zhaosen LIN; Xianghua LIU; Guodong WANG

    2006-01-01

    In the present paper, low carbon steel strips with different phosphorus contents were produced using a twin roll strip casting process. The solidification structure was studied and its features were analyzed in detail. It was found that the strips possessed a fine microstructure compared with the mould cast steels. With increasing phosphorus content more ferrite has been formed with finer grains.

  7. Fast-Scan Cyclic Voltammetry (FSCV) Detection of Endogenous Octopamine in Drosophila melanogaster Ventral Nerve Cord.

    Science.gov (United States)

    Pyakurel, Poojan; Privman Champaloux, Eve; Venton, B Jill

    2016-08-17

    Octopamine is an endogenous biogenic amine neurotransmitter, neurohormone, and neuromodulator in invertebrates and has functional analogy with norepinephrine in vertebrates. Fast-scan cyclic voltammetry (FSCV) can detect rapid changes in neurotransmitters, but FSCV has not been optimized for octopamine detection in situ. The goal of this study was to characterize octopamine release in the ventral nerve cord of Drosophila larvae for the first time. A FSCV waveform was optimized so that the potential for octopamine oxidation would not be near the switching potential where interferences can occur. Endogenous octopamine release was stimulated by genetically inserting either the ATP sensitive channel, P2X2, or the red-light sensitive channelrhodopsin, CsChrimson, into cells expressing tyrosine decarboxylase (TDC), an octopamine synthesis enzyme. To ensure that release is due to octopamine and not the precursor tyramine, the octopamine synthesis inhibitor disulfiram was applied, and the signal decreased by 80%. Stimulated release was vesicular, and a 2 s continuous light stimulation of CsChrimson evoked 0.22 ± 0.03 μM of octopamine release in the larval ventral nerve cord. Repeated stimulations were stable with 2 or 5 min interstimulation times. With pulsed stimulations, the release was dependent on the frequency of applied light pulse. An octopamine transporter has not been identified, and blockers of the dopamine transporter and serotonin transporter had no significant effect on the clearance time of octopamine, suggesting that they do not take up octopamine. This study shows that octopamine can be monitored in Drosophila, facilitating future studies of how octopamine release functions in the insect brain.

  8. 十六烷基三甲基溴化铵存在下锑膜修饰玻碳电极差分脉冲溶出伏安法测定尿中痕量铅、镉%Antimony film-plated glassy carbon electrode for simultaneous determination of trace lead and cadmium in urine by differential pulse stripping voltammetry in the presence of cetyltrimethylammonium bromide

    Institute of Scientific and Technical Information of China (English)

    公维磊; 王长芹; 杨金玲; 张凯

    2014-01-01

    目的 考察并优化同位镀锑膜修饰玻碳电极同时测定pb2+、Cd2+的方法.方法 采用十六烷基三甲基溴化铵(CTAB)作为增敏剂,以锑膜修饰玻碳电极作为工作电极差分脉冲溶出伏安法测定尿中痕量pb2+、Cd2+.结果 pb2+、Cd2+在锑膜电极上可得到灵敏的溶出峰,溶出电位分别为-0.48 V和-0.73 V.当富集时间为180 s时,pb2+、Cd2+的线性范围为0 ~ 100 μg/L(r≥0.991),检出限分别为0.47 μg/L和0.78 μg/L,pb2+、Cd2+的加标回收率分别为92.0% ~ 104.3%和94.0% ~102.6%,相对标准偏差(RSD)分别为4.1% ~5.0%和2.8% ~6.1%.利用该方法测定了尿样中Pb的含量,结果令人满意.结论 该方法灵敏度高,精密度、准确性好,锑膜修饰玻碳电极可作为一种新的环保膜电极代替汞膜电极用于尿样中Pb含量的检测.

  9. Computer-controlled instrumentation for fast voltammetry at ultramicroelectrodes

    Science.gov (United States)

    Pospíšil, L.; Fiedler, J.; Fanelli, N.

    2000-04-01

    In this article we describe an electrochemical experimental setup for cyclic voltammetry operating from low (1 V/s) to very high (200 kV/s) scan rates. The system is designed to achieve an acceptable cost and to be user friendly for nonexperts. The instrumentation is based on a commercial arbitrary wave form generator, a digital oscilloscope, a general purpose interface bus interface to a PC, and a laboratory-built potentiostat. There are no complicated manual operations, instead the software creates dialog with an operator to control commands for the instruments. Requirements for the wave form synthesis and the data acquisition are given. Various data-smoothing methods for treating 8-bit fast scan data are evaluated. The performance was tested on the oxidation of ferrocene in acetonitrile. The estimated value of the standard heterogeneous rate constant, k0=0.8±0.1 cms-1, is in reasonable agreement with the most recent reports from other laboratories.

  10. Study of quinones reactions with wine nucleophiles by cyclic voltammetry.

    Science.gov (United States)

    Oliveira, Carla M; Barros, António S; Ferreira, António C S; Silva, Artur M S

    2016-11-15

    Quinones are electrophilic species which can react with various nucleophiles, like wine antioxidants, such as sulfur dioxide or ascorbic acid, thiols, amino acids, and numerous polyphenols. These reactions are very important in wine aging because they mediate oxygen reactions during both production and bottle aging phases. In this work, the major challenge was to determine the interaction between ortho-quinones and wine nucleophiles (amino acids, thiols, and the antioxidants SO2 and ascorbic acid), by cyclic voltammetry. Wine-model solutions with gallic acid, caffeic acid, or (+)-catechin and nucleophilic compounds were used. To understand the effect of nucleophilic addition in wine, a white wine with the same added nucleophiles was also analysed. Cyclic voltammograms were taken with glassy carbon electrode or screen-printed carbon electrodes, respectively, for wine-model and white wines solutions, in the absence and in the presence of nucleophiles. A nucleophilic order profile related to the cathodic current intensity decrease was observed.

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

    Science.gov (United States)

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

    2015-11-14

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

  12. Cyclic Voltammetry Probe Approach Curves with Alkali Amalgams at Mercury Sphere-Cap Scanning Electrochemical Microscopy Probes.

    Science.gov (United States)

    Barton, Zachary J; Rodríguez-López, Joaquín

    2017-03-07

    We report a method of precisely positioning a Hg-based ultramicroelectrode (UME) for scanning electrochemical microscopy (SECM) investigations of any substrate. Hg-based probes are capable of performing amalgamation reactions with metal cations, which avoid unwanted side reactions and positive feedback mechanisms that can prove problematic for traditional probe positioning methods. However, prolonged collection of ions eventually leads to saturation of the amalgam accompanied by irreversible loss of Hg. In order to obtain negative feedback positioning control without risking damage to the SECM probe, we implement cyclic voltammetry probe approach surfaces (CV-PASs), consisting of CVs performed between incremental motor movements. The amalgamation current, peak stripping current, and integrated stripping charge extracted from a shared CV-PAS give three distinct probe approach curves (CV-PACs), which can be used to determine the tip-substrate gap to within 1% of the probe radius. Using finite element simulations, we establish a new protocol for fitting any CV-PAC and demonstrate its validity with experimental results for sodium and potassium ions in propylene carbonate by obtaining over 3 orders of magnitude greater accuracy and more than 20-fold greater precision than existing methods. Considering the timescales of diffusion and amalgam saturation, we also present limiting conditions for obtaining and fitting CV-PAC data. The ion-specific signals isolated in CV-PACs allow precise and accurate positioning of Hg-based SECM probes over any sample and enable the deployment of CV-PAS SECM as an analytical tool for traditionally challenging conditions.

  13. Hardy inequalities in strips on ruled surfaces

    Directory of Open Access Journals (Sweden)

    2006-01-01

    Full Text Available We consider the Dirichlet Laplacian in infinite two-dimensional strips defined as uniform tubular neighbourhoods of curves on ruled surfaces. We show that the negative Gauss curvature of the ambient surface gives rise to a Hardy inequality and we use this to prove certain stability of spectrum in the case of asymptotically straight strips about mildly perturbed geodesics.

  14. Tactual Strip Maps as Navigational Aids.

    Science.gov (United States)

    Golledge, R. G.

    1991-01-01

    This article reviews the history and use of tactual maps by blind and visually impaired travelers. It discusses textual patterns, symbols, and graphics; differences between conventional geographic-cartographic maps and strip maps used as navigational aids; and current advances, including disposable, quick-to-produce, and easy-to-update strip maps.…

  15. 33 CFR 157.128 - Stripping system.

    Science.gov (United States)

    2010-07-01

    ... of the following devices for stripping oil from each cargo tank: (1) A positive displacement pump. (2) A self-priming centrifugal pump. (3) An eductor (4) Any other device accepted by the Commandant. (d... positive displacement pump or a self-priming centrifugal pump, the stripping system must have the...

  16. Water problems in Gaza Strip,Palestine

    Institute of Scientific and Technical Information of China (English)

    Ismail ALGHALBAN

    2001-01-01

    The only source for water in Gaza strip, southern Palestine, is the groundwater aquifer. The Pliocene - Pleistocene aquifer has two serious problems: quantity and quality. This study is an attempt to identify the problems and to suggest solutions for water problems in Gaza strip. In addition, some rules for rehabilitation of the aquifers were suggested.

  17. 7 CFR 29.6041 - Strips.

    Science.gov (United States)

    2010-01-01

    ... 7 Agriculture 2 2010-01-01 2010-01-01 false Strips. 29.6041 Section 29.6041 Agriculture Regulations of the Department of Agriculture AGRICULTURAL MARKETING SERVICE (Standards, Inspections, Marketing... INSPECTION Standards Definitions § 29.6041 Strips. The sides of a tobacco leaf from which the stem has...

  18. Voltammetry and Electrocatalysis of Achrornobacter Xylosoxidans Copper Nitrite Reductase on Functionalized Au(111)-Electrode Surfaces

    DEFF Research Database (Denmark)

    Welinder, Anna C.; Zhang, Jingdong; Hansen, Allan G.;

    2007-01-01

    A long-standing issue in protein film voltammetry (PFV), particularly electrocatalytic voltammetry of redox enzyme monolayers, is the variability of protein adsorption modes, reflected in distributions of catalytic activity of the adsorbed protein/enzyme molecules. Use of well-defined, atomically...

  19. Double peak electric field distortion in heavily irradiated silicon strip detectors

    CERN Document Server

    Eremin, Vladimir; Roe, Shaun; Ruggiero, G; Verbitskaya, E

    2004-01-01

    Non-uniform distribution of the electric field outlined as double peak distortion (DPD) is considered for heavily irradiated silicon strip detectors, which were developed for the CERN-ATLAS semiconductor tracker. DPD originates from the non-uniform accumulation of electrons and holes from the bulk generated current that are captured by radiation induced defects: deep acceptors and donors with mid-gap energy levels. This corresponds to the formation of the low electric field region in the detector central part that consequently will delay charge collection. The electric field distributions at different reverse biases, fluences and detector operational temperatures are calculated using a one-dimensional Poisson equation as it was done earlier for pad detectors. It has been shown that due to the electric field focusing at the strips the DPD effect is more pronounced for strip detectors as compared to that in pad detectors. The double peak electric field distribution is evinced experimentally in current pulse res...

  20. Disposable Carbon Dots Modified Screen Printed Carbon Electrode Electrochemical Sensor Strip for Selective Detection of Ferric Ions

    Directory of Open Access Journals (Sweden)

    Shao Chien Tan

    2017-01-01

    Full Text Available A disposable electrochemical sensor strip based on carbon nanodots (C-Dots modified screen printed carbon electrode (SPCE was fabricated for selective detection of ferric ions (Fe3+ in aqueous solution. C-Dots of mean diameters within the range of 1–7 nm were synthesized electrochemically from spent battery carbon rods. The analytical performance of this electrochemical sensor strip was characterized using cyclic voltammetry (CV and electrochemical impedance spectroscopy (EIS. The deposition of C-Dots had enhanced the electron-transfer kinetics and current intensity of the SPCE remarkably by 734% as compared to that of unmodified SPCE. Under optimized conditions, the electrochemical sensor strip exhibited a linear detection range of 0.5 to 25.0 ppm Fe3+ with a limit of detection (LOD of 0.44±0.04 ppm (at S/N ratio = 3. Validation of results by the electrochemical sensor strip was done by comparing analysis results obtained using an Atomic Absorption Spectrometer (AAS.

  1. Circuit realization microwave antennas-oscillator on strip antennas

    OpenAIRE

    Golynskyy, V. D.; Prudyus, I. N.

    2009-01-01

    Showing special feature of development circuitries microwave transistors antennasoscillator on strip dielectric-resonator-antennas. Showing circuitries and technical characteristics of developed microwave antennasoscillator on strip.

  2. Cadmium speciation assessed by voltammetry, ion exchange and geochemical calculation in soil solutions collected after soil rewetting.

    Science.gov (United States)

    Cornu, J Y; Parat, C; Schneider, A; Authier, L; Dauthieu, M; Sappin-Didier, V; Denaix, L

    2009-07-01

    Analytical techniques and speciation models have been developed to characterize the speciation of Cd in soil solution. They provide an estimate of operationally defined species of Cd that need to be compared, especially for soil solutions highly concentrated in organic matter as are the solutions collected after soil rewetting. This work deals with the comparison between the speciation of Cd measured by anodic stripping voltammetry (ASV) and ion exchange and the speciation of Cd calculated using Visual MINTEQ. The aim of this study was to quantify and explain the differences in Cd speciation observed between the three approaches. Cd speciation was assessed in soil solutions collected 4, 8, 24, 48, 96 and 144h after the rewetting of an air-dried contaminated soil. To optimize the computed speciation of Cd, other physico-chemical parameters were followed (e.g. pH, ionic strength and the concentrations of major anions, major cations and dissolved organic carbon) and a brief characterisation of dissolved organic matter (DOM) was performed. The discrepancy between model predictions and analytical measurements highlighted the need for caution in the interpretation of geochemical speciated data for Cd. The major result of this study was that a characterization of DOM based on its specific UV-absorbance at 254 nm improved the accuracy of model predictions. Another finding is that labile Cd complexes, even organic, may have been included in the electrochemically labile fraction of Cd measured by ASV.

  3. Direct electrodeposition of gold nanotube arrays of rough and porous wall by cyclic voltammetry and its applications of simultaneous determination of ascorbic acid and uric acid

    Energy Technology Data Exchange (ETDEWEB)

    Yang Guangming, E-mail: yangguangmingbs@126.com [Department of Resources and Environment, Baoshan University, Baoshan 678000 (China); Li Ling [Department of Resources and Environment, Baoshan University, Baoshan 678000 (China); Jiang Jinhe; Yang Yunhui [College of Chemistry and Chemical Engineering, Yunnan Normal University, Kunming 650092 (China)

    2012-08-01

    Gold nanotube arrays of rough and porous wall has been synthesized by direct electrodeposition with cyclic voltammetry utilizing anodic aluminum oxide template (AAO) and polycarbonate membrane (PC) during short time (only 3 min and 2 min, respectively). The mechanism of the direct electrodeposition of gold nanotube arrays by cyclic voltammetry (CV) has been discussed. The morphological characterizations of the gold nanotube arrays have been investigated by scanning electron microscopy (SEM). A simultaneous determination of ascorbic acid (AA) and uric acid (UA) by differential pulse voltammetry (DPV) was constructed by attaching gold nanotube arrays (using AAO) onto the surface of a glassy carbon electrode (GCE). The electrochemical behavior of AA and UA at this modified electrode has been studied by CV and differential pulse voltammetry (DPV). The sensor offers an excellent response for AA and UA and the linear response range for AA and UA were 1.02 Multiplication-Sign 10{sup -7}-5.23 Multiplication-Sign 10{sup -4} mol L{sup -1} and 1.43 Multiplication-Sign 10{sup -7}-4.64 Multiplication-Sign 10{sup -4} mol L{sup -1}, the detection limits were 1.12 Multiplication-Sign 10{sup -8} mol L{sup -1} and 2.24 Multiplication-Sign 10{sup -8} mol L{sup -1}, respectively. This sensor shows good regeneration, stability and selectivity and has been used for the determination of AA and UA in real human urine and serum samples with satisfied results. - Graphical abstract: The schematic diagram of formation of Au nanotube arrays (a) and the stepwise procedure of the sensor (b). Highlights: Black-Right-Pointing-Pointer Gold nanotubes array has been synthesized by cyclic voltammetry. Black-Right-Pointing-Pointer The mechanism of deposition of gold nanotube has been discussed. Black-Right-Pointing-Pointer A determination of ascorbic acid and uric acid was constructed by gold array. Black-Right-Pointing-Pointer A satisfied determination of samples can be obtained by this sensor.

  4. Transfusion and blood donation in comic strips.

    Science.gov (United States)

    Lefrère, Jean-Jacques; Danic, Bruno

    2013-07-01

    The representation of blood transfusion and donation of blood in the comic strip has never been studied. The comic strip, which is a relatively recent art, emerged in the 19th century before becoming a mass medium during the 20th century. We have sought, by calling on collectors and using the resources of Internet, comic strips devoted, wholly or in part, to the themes of transfusion and blood donation. We present some of them here in chronologic order, indicating the title, country of origin, year of publication, and names of authors. The theme of the superhero using transfusion to transmit his virtues or his powers is repeated throughout the 20th century in North American comic strips. More recently, comic strips have been conceived from the outset with a promotional aim. They perpetuate positive images and are directed toward a young readership, wielding humor to reduce the fear of venipuncture. Few comic strips denounce the abuse of the commercialization of products derived from the human body. The image of transfusion and blood donation given by the comic strips is not to be underestimated because their readership is primarily children, some of whom will become blood donors. Furthermore, if some readers are transfused during their lives, the impact of a memory more or less conscious of these childhood readings may resurface, both in hopes and in fears.

  5. A Strip Cell in Pyroelectric Devices

    Directory of Open Access Journals (Sweden)

    An-Shen Siao

    2016-03-01

    Full Text Available The pyroelectric effect affords the opportunity to convert temporal temperature fluctuations into usable electrical energy in order to develop abundantly available waste heat. A strip pyroelectric cell, used to enhance temperature variation rates by lateral temperature gradients and to reduce cell capacitance to further promote the induced voltage, is described as a means of improving pyroelectric energy transformation. A precision dicing saw was successfully applied in fabricating the pyroelectric cell with a strip form. The strip pyroelectric cell with a high-narrow cross section is able to greatly absorb thermal energy via the side walls of the strips, thereby inducing lateral temperature gradients and increasing temperature variation rates in a thicker pyroelectric cell. Both simulation and experimentation show that the strip pyroelectric cell improves the electrical outputs of pyroelectric cells and enhances the efficiency of pyroelectric harvesters. The strip-type pyroelectric cell has a larger temperature variation when compared to the trenched electrode and the original type, by about 1.9 and 2.4 times, respectively. The measured electrical output of the strip type demonstrates a conspicuous increase in stored energy as compared to the trenched electrode and the original type, by of about 15.6 and 19.8 times, respectively.

  6. Low-resistance strip sensors for beam-loss event protection

    Energy Technology Data Exchange (ETDEWEB)

    Ullán, M., E-mail: Miguel.Ullan@imb-cnm.csic.es [Centro Nacional de Microelectrónica (IMB-CNM, CSIC), Campus Universitario de Bellaterra, 08193 Barcelona (Spain); Benítez, V.; Quirion, D.; Zabala, M.; Pellegrini, G.; Lozano, M. [Centro Nacional de Microelectrónica (IMB-CNM, CSIC), Campus Universitario de Bellaterra, 08193 Barcelona (Spain); Lacasta, C.; Soldevila, U.; García, C. [Instituto de Fisica Corpuscular (IFIC, CSIC-UV), Valencia (Spain); Fadeyev, V.; Wortman, J.; DeFilippis, J.; Shumko, M.; Grillo, A.A; Sadrozinski, H.F.-W. [Santa Cruz Institute for Particle Physics (SCIPP), University of California Santa Cruz (UCSC), Santa Cruz, CA (United States)

    2014-11-21

    AC-coupled silicon strip sensors can be damaged in case of a beam loss due to the possibility of a large charge accumulation in the bulk, developing very high voltages across the coupling capacitors which can destroy them. Punch-through structures are currently used to avoid this problem helping to evacuate the accumulated charge as large voltages are developing. Nevertheless, previous experiments, performed with laser pulses, have shown that these structures can become ineffective in relatively long strips. The large value of the implant resistance can effectively isolate the “far” end of the strip from the punch-through structure leading to large voltages. We present here our developments to fabricate low-resistance strip sensors to avoid this problem. The deposition of a conducting material in contact with the implants drastically reduces the strip resistance, assuring the effectiveness of the punch-through structures. First devices have been fabricated with this new technology. Initial results with laser tests show the expected reduction in peak voltages on the low resistivity implants. Other aspects of the sensor performance, including the signal formation, are not affected by the new technology.

  7. High energy H- ion transport and stripping

    Energy Technology Data Exchange (ETDEWEB)

    Chou, W.; /Fermilab

    2005-05-01

    During the Proton Driver design study based on an 8 GeV superconducting RF H{sup -} linac, a major concern is the feasibility of transport and injection of high energy H{sup -} ions because the energy of H{sup -} beam would be an order of magnitude higher than the existing ones. This paper will focus on two key technical issues: (1) stripping losses during transport (including stripping by blackbody radiation, magnetic field and residual gases); (2) stripping efficiency of carbon foil during injection.

  8. THE DEVELOPMENT OF FCC STRIPPING TECHNOLOGY

    Institute of Scientific and Technical Information of China (English)

    ZHANGZhen-qian

    2003-01-01

    This article briefly describes the major patents domestic and the abroad,and the current situation and achievements of FCC stripping technology in China.The develping trend of FCC stripping technology is presented,including further developments of FCC stripper to improve unit performance,combination of the stripper and pre-stripper within disengager to from a complete high-efficiency FCC stripping system.In addition to high efficiency,simple structure and easiness of installation and maintenance for a new FCC stripper are all of consideration.

  9. Saving Energy Through Advanced Power Strips (Poster)

    Energy Technology Data Exchange (ETDEWEB)

    Christensen, D.

    2013-10-01

    Advanced Power Strips (APS) look just like ordinary power strips, except that they have built-in features that are designed to reduce the amount of energy used by many consumer electronics. There are several different types of APSs on the market, but they all operate on the same basic principle of shutting off the supply power to devices that are not in use. By replacing your standard power strip with an APS, you can signifcantly cut the amount of electricity used by your home office and entertainment center devices, and save money on your electric bill. This illustration summarizes the different options.

  10. Fast Selective Detection of Pyocyanin Using Cyclic Voltammetry

    Directory of Open Access Journals (Sweden)

    Fatima AlZahra’a Alatraktchi

    2016-03-01

    Full Text Available Pyocyanin is a virulence factor uniquely produced by the pathogen Pseudomonas aeruginosa. The fast and selective detection of pyocyanin in clinical samples can reveal important information about the presence of this microorganism in patients. Electrochemical sensing of the redox-active pyocyanin is a route to directly quantify pyocyanin in real time and in situ in hospitals and clinics. The selective quantification of pyocyanin is, however, limited by other redox-active compounds existing in human fluids and by other metabolites produced by pathogenic bacteria. Here we present a direct selective method to detect pyocyanin in a complex electroactive environment using commercially available electrodes. It is shown that cyclic voltammetry measurements between −1.0 V to 1.0 V reveal a potential detection window of pyocyanin of 0.58–0.82 V that is unaffected by other redox-active interferents. The linear quantification of pyocyanin has an R2 value of 0.991 across the clinically relevant concentration range of 2–100 µM. The proposed method was tested on human saliva showing a standard deviation of 2.5% ± 1% (n = 5 from the known added pyocyanin concentration to the samples. This inexpensive procedure is suggested for clinical use in monitoring the presence and state of P. aeruginosa infection in patients.

  11. Cyclic voltammetry and RBS study of paint components

    Energy Technology Data Exchange (ETDEWEB)

    Bowman, Lynn [Center for Irradiation of Materials, Alabama A and M University, 4900 Meridian Street, P.O. Box 1447, Normal, AL 35762 (United States); Spencer, Dirk [Plant and Soil Science Department, Alabama A and M University, Normal, AL 35762-1447 (United States); Muntele, Claudiu [Center for Irradiation of Materials, Alabama A and M University, 4900 Meridian Street, P.O. Box 1447, Normal, AL 35762 (United States)]. E-mail: claudiu@cim.aamu.edu; Muntele, Iulia [Center for Irradiation of Materials, Alabama A and M University, 4900 Meridian Street, P.O. Box 1447, Normal, AL 35762 (United States); Ila, D. [Center for Irradiation of Materials, Alabama A and M University, 4900 Meridian Street, P.O. Box 1447, Normal, AL 35762 (United States)

    2007-08-15

    Heavy metals and metalloid ions are found in environmental matrices. The most toxic are lead, cadmium and mercury. These three heavy metals have no biological function and are toxic at all concentrations. Lead is one of the most insidious heavy metals and is introduced into the environment by many different means. It persists in both urban and rural settings, being found in paint chips, pottery, crystal and pharmaceutical and nutritional products. The analysis of heavy elements such as lead in soil is of particular importance [W.T. Sturges, R.M. Harrison, Sci. Total Environ. 44 (3) (1985) 225; M.L. Lepow, L. Bruckman, M. Gillette, S. Markowitz, R. Robino, J. Kapish, Environ. Res. 10 (3) (1975) 415; A.E. Daniels, J.R. Kominsky, P.J. Clark, J. Hazard. Mater. B 87 (2001) 117; G. Hutter, D. Moshman, J. Hazard. Mater. 40 (1995) 1]. In preparing the methods for lead detection in paint, we have used Rutherford backscattering spectrometry (RBS) in order to study the type and amount of heavy metal content in paint samples collected at various sites in the historic campus at A and M University (AAMU). We will show the results of our study with emphasis on comparison of what we learned about presence of lead in paints using our ion beam methods compared with the analysis of lead in paints using cyclic voltammetry.

  12. In vivo histamine voltammetry in the mouse premammillary nucleus.

    Science.gov (United States)

    Samaranayake, Srimal; Abdalla, Aya; Robke, Rhiannon; Wood, Kevin M; Zeqja, Anisa; Hashemi, Parastoo

    2015-06-07

    Histamine plays a major role in the mediation of allergic reactions such as peripheral inflammation. This classical monoamine is also a neurotransmitter involved in the central nervous system but its role in this context is poorly understood. Studying histamine neurotransmission is important due to its implications in many neurological disorders. The sensitivity, selectivity and high temporal resolution of fast scan cyclic voltammetry (FSCV) offer many advantages for studying electroactive neurotransmitters. Histamine has previously been studied with FSCV; however, the lack of a robust Faradaic electrochemical signal makes it difficult to selectively identify histamine in complex media, as found in vivo. In this work, we optimize an electrochemical waveform that provides a stimulation-locked and unique electrochemical signal towards histamine. We describe in vitro waveform optimization and a novel in vivo physiological model for stimulating histamine release in the mouse premammillary nucleus via stimulation of the medial forebrain bundle. We demonstrate that a robust signal can be used to effectively identify histamine and characterize its in vivo kinetics.

  13. Cyclic voltammetry of apple fruits: Memristors in vivo.

    Science.gov (United States)

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

    2016-12-01

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

  14. Fully printed flexible and disposable wireless cyclic voltammetry tag.

    Science.gov (United States)

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

    2015-01-29

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

  15. Fast Selective Detection of Pyocyanin Using Cyclic Voltammetry.

    Science.gov (United States)

    Alatraktchi, Fatima AlZahra'a; Andersen, Sandra Breum; Johansen, Helle Krogh; Molin, Søren; Svendsen, Winnie E

    2016-03-19

    Pyocyanin is a virulence factor uniquely produced by the pathogen Pseudomonas aeruginosa. The fast and selective detection of pyocyanin in clinical samples can reveal important information about the presence of this microorganism in patients. Electrochemical sensing of the redox-active pyocyanin is a route to directly quantify pyocyanin in real time and in situ in hospitals and clinics. The selective quantification of pyocyanin is, however, limited by other redox-active compounds existing in human fluids and by other metabolites produced by pathogenic bacteria. Here we present a direct selective method to detect pyocyanin in a complex electroactive environment using commercially available electrodes. It is shown that cyclic voltammetry measurements between -1.0 V to 1.0 V reveal a potential detection window of pyocyanin of 0.58-0.82 V that is unaffected by other redox-active interferents. The linear quantification of pyocyanin has an R² value of 0.991 across the clinically relevant concentration range of 2-100 µM. The proposed method was tested on human saliva showing a standard deviation of 2.5% ± 1% (n = 5) from the known added pyocyanin concentration to the samples. This inexpensive procedure is suggested for clinical use in monitoring the presence and state of P. aeruginosa infection in patients.

  16. OPTIMAL ELECTROPORATION CONDITION FOR SPERM MEDIATED GENE TRANSFER IN STRIPPED CATFISH (Pangasionodon hypophthalmus

    Directory of Open Access Journals (Sweden)

    Raden Roro Sri Pudji Sinarni Dewi

    2010-06-01

    Full Text Available The success of transgenic fish production has been achieved through eggs fertilization using electroporated sperms carrying exogenous DNA. This study was conducted in order to obtain the optimal electroporation condition for stripped catfish sperm. A plasmid containing green fluorescent protein (GFP gene driven by carp β-actin promoter was transferred into sperm using electrophoresis method towards transgenic stripped catfish (Pangasionodon hypophthalmus production. Electroporation was carried out using square wave shock with pulse length of 30 ms and pulse interval of 0.1 sec. Treatments are combination between voltage (50 V, 75 V, and 100 V and pulse number (1 and 3. Exogenous DNA concentration used was 10 μg/mL of Tris-EDTA. Results showed that increasing the voltage from 50 to 100 decreased sperm motility, while pulse number did not affect sperm motility. Voltage of 50 gave the best motility of sperm, although sperm viability relatively similar between treatments and control except at 100 V with 3 pulses number. Further, electroporation-treated sperms were able to fertilize eggs. Higher hatching rate of eggs was obtained in electroporation treatment at 50 V with pulse number of 1 and 3. The persistence of transferred GFP was detected in electroporated and incubated sperms (control. However, GFP was only detected in larvae from eggs that were fertilized by electroporated sperm. Thus, electroporation could be applied to produce transgenic stripped catfish.

  17. Inapproximability of maximal strip recovery

    CERN Document Server

    Jiang, Minghui

    2009-01-01

    In comparative genomic, the first step of sequence analysis is usually to decompose two or more genomes into syntenic blocks that are segments of homologous chromosomes. For the reliable recovery of syntenic blocks, noise and ambiguities in the genomic maps need to be removed first. Maximal Strip Recovery (MSR) is an optimization problem proposed by Zheng, Zhu, and Sankoff for reliably recovering syntenic blocks from genomic maps in the midst of noise and ambiguities. Given $d$ genomic maps as sequences of gene markers, the objective of \\msr{d} is to find $d$ subsequences, one subsequence of each genomic map, such that the total length of syntenic blocks in these subsequences is maximized. For any constant $d \\ge 2$, a polynomial-time 2d-approximation for \\msr{d} was previously known. In this paper, we show that for any $d \\ge 2$, \\msr{d} is APX-hard, even for the most basic version of the problem in which all gene markers are distinct and appear in positive orientation in each genomic map. Moreover, we provi...

  18. A video strip chart program

    Energy Technology Data Exchange (ETDEWEB)

    Jones, N.L. [Oak Ridge National Lab., TN (United States). Accelerator-Based Atomic Physics

    1994-12-31

    A strip chart recorder has been utilized for trend analysis of the Oak Ridge National Laboratory EN tandem since 1987. At the EN, the author could not afford the nice eight channel thermal pen recorder that was used at the 25 URC. He had to suffice with two channel fiber tip or capillary pen type recorders retrieved from salvage and maintained with parts from other salvaged recorders. After cycling through several machines that eventually became completely unserviceable, a search for a new thermal recorder was begun. As much as he hates to write computer code, he decided to try his hand at getting an old data acquisition unit, that had been retrieved several years ago from salvage, to meet his needs. A BASIC language compiler was used because time was not available to learn a more advanced language. While attempting to increase acquisition and scroll speed on the 6 MHz 80286 that the code was first developed on, it became apparent that scrolling only the first small portion of the screen at high speed and then averaging that region and histogramming the average provided both the speed necessary for capturing fairly short duration events, and a trend record without use of back scrolling and disk storage routines. This turned out to be quite sufficient.

  19. Plaque accumulations caused by interdental stripping.

    Science.gov (United States)

    Radlanski, R J; Jäger, A; Schwestka, R; Bertzbach, F

    1988-11-01

    Human enamel surfaces were stripped with orthodontic grinding and finishing materials, and evaluated with the scanning electron microscope (SEM). Even under in vitro conditions with the finest finishing strips, it was not possible to produce an enamel surface free of the furrows that result from the initial abrasion caused by the coarse strip. Enamel surfaces stripped gradually from coarse to superfine were left in the mouths of patients for 12 weeks and evaluated with the SEM. The edges of the furrows were found to be smoother but the furrows remained wide and deep enough to facilitate more plaque accumulations than those on untreated surfaces. The use of dental floss did not result in prevention of plaque accumulations along the bottom of the furrows.

  20. Finite element modeling of corneal strip extensometry

    CSIR Research Space (South Africa)

    Botha, N

    2012-12-01

    Full Text Available numerically modelled in several studies, this study focusses on accurately modelling the strip extensiometry test. Two methods were considered to simulate the experimental conditions namely, a single phase and a two phase method. A finite element model...

  1. Compositional Analysis of Electrodeposited Cu-Se Compound Semiconductor Thin Films Using Combined Voltammetry and Flow-Electrochemical Quartz Crystal Microgravimetry

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Wooju; Jeong, Seonghan; Myung, Noseung [Konkuk Univ., Chungju (Korea, Republic of); Rajeshwar, Krishnan [Univ. of Texas at Arlington, Arlington (United States); Lee, Chiwoo [Korea Univ., Seoul (Korea, Republic of)

    2013-10-15

    A novel method which is species selective for the compositional analysis of electrodeposited Cu-Se semiconductor films was developed using combined voltammetry and flow-EQCM. The amounts of free Se and Se in Cu{sub 2}Se were obtained from the frequency changes at constant potentials of -0.8 V and -3 V, respectively. Potential steps to -0.8 V and -1.3 V were employed to reduce free Se to Se{sub 2}{sup -} and Cu{sub 2}Se to Cu + Se{sub 2}{sup -}, respectively. Resultant total Cu was anodically stripped at +0.8 V and the free Cu content was calculated using the difference in frequency changes observed during the stripping of total Cu and Se in Cu{sub 2}Se. The results showed that the amounts of free Se, free Cu and the targeted Cu{sub 2}Se varied with deposition potential as well as film thickness. The ternary compound semiconductor CuInSe{sub 2} (CIS) has attracted great interest due to its unique properties and wide applications.

  2. Strip Casting of High Performance Structural Alloys

    Institute of Scientific and Technical Information of China (English)

    S S Park; J G Lee; Nack J Kim

    2004-01-01

    There exists a great need for the development of high performance alloys due to increasing demands for energy conservation and environmental protection. Application of strip casting shows a strong potential for the improvement of properties of existing alloys and also for the development of novel alloy systems with superior properties. The present paper reviews our Center's activities in the development of high performance alloys by strip casting. Examples include (1) Al alloys, (2) wrought Mg alloys, and (3) bulk metallic glass (BMG) alloys.

  3. Speed Control and Coiling Temperature Control of Strip

    Institute of Scientific and Technical Information of China (English)

    CAI Xiao-hui; ZHANG Dian-hua; WANG Guo-dong; LIU Xiang-hua; FAN Lei

    2004-01-01

    Considering the strip speed during controlled laminar cooling on Baosteel 1580 hot strip mill in China, the influence of strip speed fluctuation on coiling temperature control for the tail and "neck" of the strip was analyzed. The optimization strategies were put forward and proved effective in operation.

  4. Excess Production Capacity Squeezes Profits of Brass Strip Enterprises

    Institute of Scientific and Technical Information of China (English)

    2012-01-01

    <正>Between 2003 and 2006,under the backdrop of rapid growth of domestic demand for brass strip and soaring copper price,brass strip manufacturers made a fortune.And brass strip manufacturers mushroomed in Zhejiang,Anhui and Jiangsu.Large brass strip manufacturers

  5. Process development of thin strip steel casting

    Energy Technology Data Exchange (ETDEWEB)

    Sussman, R.C.; Williams, R.S.

    1990-12-01

    An important new frontier is being opened in steel processing with the emergence of thin strip casting. Casting steel directly to thin strip has enormous benefits in energy savings by potentially eliminating the need for hot reduction in a hot strip mill. This has been the driving force for numerous current research efforts into the direct strip casting of steel. The US Department of Energy initiated a program to evaluate the development of thin strip casting in the steel industry. In earlier phases of this program, planar flow casting on an experimental caster was studied by a team of engineers from Westinghouse Electric corporation and Armco Inc. A subsequent research program was designed as a fundamental and developmental study of both planar and melt overflow casting processes. This study was arranged as several separate and distinct tasks which were often completed by different teams of researchers. An early task was to design and build a water model to study fluid flow through different designs of planar flow casting nozzles. Another important task was mathematically modeling of melt overflow casting process. A mathematical solidification model for the formation of the strip in the melt overflow process was written. A study of the material and conditioning of casting substrates was made on the small wheel caster using the melt overflow casting process. This report discusses work on the development of thin steel casting.

  6. Process development of thin strip steel casting

    Energy Technology Data Exchange (ETDEWEB)

    Sussman, R.C.; Williams, R.S.

    1990-12-01

    An important new frontier is being opened in steel processing with the emergence of thin strip casting. Casting steel directly to thin strip has enormous benefits in energy savings by potentially eliminating the need for hot reduction in a hot strip mill. This has been the driving force for numerous current research efforts into the direct strip casting of steel. The US Department of Energy initiated a program to evaluate the development of thin strip casting in the steel industry. In earlier phases of this program, planar flow casting on an experimental caster was studied by a team of engineers from Westinghouse Electric corporation and Armco Inc. A subsequent research program was designed as a fundamental and developmental study of both planar and melt overflow casting processes. This study was arranged as several separate and distinct tasks which were often completed by different teams of researchers. An early task was to design and build a water model to study fluid flow through different designs of planar flow casting nozzles. Another important task was mathematically modeling of melt overflow casting process. A mathematical solidification model for the formation of the strip in the melt overflow process was written. A study of the material and conditioning of casting substrates was made on the small wheel caster using the melt overflow casting process. This report discusses work on the development of thin steel casting.

  7. Optimizing the Temporal Resolution of Fast-Scan Cyclic Voltammetry

    Science.gov (United States)

    2012-01-01

    Electrochemical detection with carbon-fiber microelectrodes has become an established method to monitor directly the release of dopamine from neurons and its uptake by the dopamine transporter. With constant potential amperometry (CPA), the measured current provides a real time view of the rapid concentration changes, but the method lacks chemical identification of the monitored species and markedly increases the difficulty of signal calibration. Monitoring with fast-scan cyclic voltammetry (FSCV) allows species identification and concentration measurements but often exhibits a delayed response time due to the time-dependent adsorption/desorption of electroactive species at the electrode. We sought to improve the temporal resolution of FSCV to make it more comparable to CPA by increasing the waveform repetition rate from 10 to 60 Hz with uncoated carbon-fiber electrodes. The faster acquisition led to diminished time delays of the recordings that tracked more closely with CPA measurements. The measurements reveal that FSCV at 10 Hz underestimates the normal rate of dopamine uptake by about 18%. However, FSCV collection at 10 and 60 Hz provide identical results when a dopamine transporter (DAT) blocker such as cocaine is bath applied. To verify further the utility of this method, we used transgenic mice that overexpress DAT. After accounting for the slight adsorption delay time, FSCV at 60 Hz adequately monitored the increased uptake rate that arose from overexpression of DAT and, again, was similar to CPA results. Furthermore, the utility of collecting data at 60 Hz was verified in an anesthetized rat by using a higher scan rate (2400 V/s) to increase sensitivity and the overall signal. PMID:22708011

  8. Multivariate curve resolution-alternating least squares assisted by voltammetry for simultaneous determination of betaxolol and atenolol using carbon nanotube paste electrode.

    Science.gov (United States)

    Khoobi, Asma; Ghoreishi, Sayed Mehdi; Masoum, Saeed; Behpour, Mohsen

    2013-12-01

    In the present work differential pulse voltammetry coupled with multivariate curve resolution-alternating least squares (MCR-ALS) was applied for simultaneous determination of betaxolol (Bet) and atenolol (Ate) in 0.20 M Britton-Robinson (B-R) buffer solution at the surface of a multi-walled carbon nanotube modified carbon paste electrode (MWCNT/CPE). Characterization of the modified electrode was carried out by electrochemical impedance spectroscopy (EIS) and cyclic voltammetry (CV). A strategy based on experimental design was followed. Operating conditions were improved with central composite rotatable design (CCRD) and response surface methodology (RSM), involving several chemical and instrumental parameters. Then second order data were built from variable pulse heights of DPV and after correction in potential shift analyzed by MCR-ALS. Analytical parameters such as linearity, repeatability, and stability were also investigated and a detection limit (DL) of 0.19 and 0.29 μM for Bet and Ate was achieved, respectively. The proposed method was successfully applied in simultaneous determining the two analytes in human plasma.

  9. Electrolyte Effects on the Cyclic Voltammetry of TCNQ (Tetracyanoquinodimethane) and TCNE (Tetracyanoethylene).

    Science.gov (United States)

    1986-07-30

    to form two radical anions. In this note we report a study by cyclic voltammetry of the reductions of TCNQ and TCNE to their radical anions and dianions at platinum and glassy carbon electrodes in acetonitrile.

  10. Theory of linear sweep voltammetry with diffuse charge: unsupported electrolytes, thin films, and leaky membranes

    CERN Document Server

    Yan, David; Pugh, Mary C; Dawson, Francis P

    2016-01-01

    Linear sweep and cyclic voltammetry techniques are important tools for electrochemists and have a variety of applications in engineering. Voltammetry has classically been treated with the Randles-Sevcik equation, which assumes an electroneutral supported electrolyte. No general theory of linear-sweep voltammetry is available, however, for unsupported electrolytes and for other situations where diffuse charge effects play a role. In this paper, we provide a historical review of previous models and experiments and present a comprehensive mathematical theory of voltammetry in electrochemical cells with diffuse charge. We solve the time-dependent Poisson-Nernst-Planck (PNP) equations with generalized Frumkin-Butler-Volmer (FBV) boundary conditions, and show theoretical and simulated current-voltage curves for liquid and solid thin films, cells with blocking electrodes, and membranes with fixed background charge. The full range of dimensionless parameters is considered, including the dimensionless Debye screening ...

  11. Novel photoresist stripping technology using steam-water mixture*

    Institute of Scientific and Technical Information of China (English)

    Wang Lei; Hui Yu; Gao Chaoqun; Jing Yupeng

    2011-01-01

    A novel wet vapor photoresist stripping technology is developed as an alternative to dry plasma ashing and wet stripping. Experiments using this technology to strip hard baked SU-8 photoresist, aurum and chromium film are carried out. Then the images of stripping results are shown and the mechanism is analyzed and discussed.The most striking result of this experiment is that the spraying mixture of steam and water droplets can strip photoresist and even metal film with ease.

  12. Robotic voltammetry with carbon nanotube-based sensors: a superb blend for convenient high-quality antimicrobial trace analysis

    Directory of Open Access Journals (Sweden)

    Theanponkrang S

    2015-01-01

    Full Text Available Somjai Theanponkrang,1,2 Wipa Suginta,2,3 Helge Weingart,4 Mathias Winterhalter,4 Albert Schulte1,2 1School of Chemistry, 2Biochemistry–Electrochemistry Research Unit, Institute of Science, 3School of Biochemistry, Suranaree University of Technology, Nakhon Ratchasima, Thailand; 4Life Sciences, School of Engineering and Science, Jacobs University Bremen, Bremen, Germany Abstract: A new automated pharmacoanalytical technique for convenient quantification of redox-active antibiotics has been established by combining the benefits of a carbon nanotube (CNT sensor modification with electrocatalytic activity for analyte detection with the merits of a robotic electrochemical device that is capable of sequential nonmanual sample measurements in 24-well microtiter plates. Norfloxacin (NFX and ciprofloxacin (CFX, two standard fluoroquinolone antibiotics, were used in automated calibration measurements by differential pulse voltammetry (DPV and accomplished were linear ranges of 1–10 µM and 2–100 µM for NFX and CFX, respectively. The lowest detectable levels were estimated to be 0.3±0.1 µM (n=7 for NFX and 1.6±0.1 µM (n=7 for CFX. In standard solutions or tablet samples of known content, both analytes could be quantified with the robotic DPV microtiter plate assay, with recoveries within ±4% of 100%. And recoveries were as good when NFX was evaluated in human serum samples with added NFX. The use of simple instrumentation, convenience in execution, and high effectiveness in analyte quantitation suggest the merger between automated microtiter plate voltammetry and CNT-supported electrochemical drug detection as a novel methodology for antibiotic testing in pharmaceutical and clinical research and quality control laboratories. Keywords: antibiotics, electroanalysis, automation, microtiter plates, pharmaceutical screening, pharmacoanalytics

  13. Voltammetry and In Situ Scanning Tunneling Microscopy of Cytochrome c Nitrite Reductase on Au(111)-Electrodes

    DEFF Research Database (Denmark)

    Gwyer, James; Zhang, Jingdong; Butt, Julea

    2006-01-01

    of the density and orientational distribution of NrfA molecules are disclosed. The submonolayer coverage resolved by in situ STM is readily reconciled with the failure to detect nonturnover signals in cyclic voltammetry of the NrfA films. The molecular structures show a range of lateral dimensions...... a direct approach to correlate electrocatalytic and molecular properties of the protein layer, a long-standing issue in protein film voltammetry....

  14. Frequency-Dependent Modulation of Dopamine Release by Nicotine and Dopamine D1 Receptor Ligands: An In Vitro Fast Cyclic Voltammetry Study in Rat Striatum.

    Science.gov (United States)

    Goutier, W; Lowry, J P; McCreary, A C; O'Connor, J J

    2016-05-01

    Nicotine is a highly addictive drug and exerts this effect partially through the modulation of dopamine release and increasing extracellular dopamine in regions such as the brain reward systems. Nicotine acts in these regions on nicotinic acetylcholine receptors. The effect of nicotine on the frequency dependent modulation of dopamine release is well established and the purpose of this study was to investigate whether dopamine D1 receptor (D1R) ligands have an influence on this. Using fast cyclic voltammetry and rat corticostriatal slices, we show that D1R ligands are able to modulate the effect of nicotine on dopamine release. Nicotine (500 nM) induced a decrease in dopamine efflux at low frequency (single pulse or five pulses at 10 Hz) and an increase at high frequency (100 Hz) electrical field stimulation. The D1R agonist SKF-38393, whilst having no effect on dopamine release on its own or on the effect of nicotine upon multiple pulse evoked dopamine release, did significantly prevent and reverse the effect of nicotine on single pulse dopamine release. Interestingly similar results were obtained with the D1R antagonist SCH-23390. In this study we have demonstrated that the modulation of dopamine release by nicotine can be altered by D1R ligands, but only when evoked by single pulse stimulation, and are likely working via cholinergic interneuron driven dopamine release.

  15. Effects of a combination of 3,4-methylenedioxymeth amphetamine and caffeine on real time stimulated dopamine release in the rat striatum: Studies using fast cyclic voltammetry.

    Science.gov (United States)

    O'Connor, J J; O'Boyle, K M; Lowry, J P

    2017-08-24

    It is well documented that caffeine exacerbates the hyperthermia associated with acute exposure to 3,4-methylenedioxymethamphetamine (MDMA) in rats. Previous reports have also indicated that MDMA-related enhancement of dopamine release is exacerbated in the presence of caffeine. In the present study we have examined whether the effects of MDMA on real-time stimulated dopamine release, in the absence of uptake inhibition, are accentuated in the presence of caffeine. Isolated striatal slices from adult male Wistar rats were treated acutely with MDMA, caffeine, or a combination, and their effects on single and 5pulse stimulated dopamine release monitored using the technique of fast cyclic voltammetry. Caffeine at 10 or 100μM had no significant effect on single pulse stimulated dopamine release. However 100μM caffeine caused a significant peak increase in 5pulse stimulated dopamine release. Both 1 and 30μM MDMA gave rise to a significant increase in both single and 5-pulse dopamine release and reuptake. A combination of 100μM caffeine and 1 or 30μM MDMA did not significantly enhance the effects of MDMA on single or 5pulse dopamine release and reuptake when compared to that applied alone. Utilizing single action potential dependent dopamine release, these results do not demonstrate a caffeine-enhanced MDMA-induced dopamine release. Copyright © 2017 Elsevier B.V. All rights reserved.

  16. Depletive stripping chronopotentiometry : a major step forward in electrochemical stripping techniques for metal ion speciation analysis

    NARCIS (Netherlands)

    Town, R.M.; Leeuwen, van H.P.

    2004-01-01

    A comparative evaluation of the utility of the various modes of stripping chronopotentiometry (SCP) for trace metal speciation analysis is presented in the broad context of stripping voltammetric techniques. The remarkable fundamental advantages of depletive SCP at scanned deposition potential (SSCP

  17. A digital X-ray imaging system based on silicon strip detectors working in edge-on configuration

    Energy Technology Data Exchange (ETDEWEB)

    Bolanos, L. [CEADEN, Calle 30 502 e/ 5ta y 7ma Avenida, Playa, Ciudad Habana (Cuba); Boscardin, M. [IRST, Fondazione Bruno Kessler, Via Sommarive 18, Povo, 38100 Trento (Italy); Cabal, A.E. [CEADEN, Calle 30 502 e/ 5ta y 7ma Avenida, Playa, Ciudad Habana (Cuba); Diaz, M. [InSTEC, Ave. Salvador Allende esq. Luaces, Quinta de los Molinos, Ciudad Habana (Cuba); Grybos, P.; Maj, P. [Faculty of Electrical Engineering, Automatics, Computer Science and Electronics, Department of Measurement and Instrumentation, AGH University of Science and Technology, Al. Mickiewicza 30, 30-059 Cracow (Poland); Prino, F. [Istituto Nazionale di Fisica Nucleare, Sezione di Torino, Via P. Giuria 1, 10125 Torino (Italy); Ramello, L. [Dipartimento di Scienze e Tecnologie Avanzate, Universita del Piemonte Orientale, Via T. Michel 11, 15100 Alessandria (Italy)], E-mail: luciano.ramello@mfn.unipmn.it; Szczygiel, R. [Faculty of Electrical Engineering, Automatics, Computer Science and Electronics, Department of Measurement and Instrumentation, AGH University of Science and Technology, Al. Mickiewicza 30, 30-059 Cracow (Poland)

    2009-09-21

    We present the energy resolution and imaging performance of a digital X-ray imaging system based on a 512-strip silicon strip detector (SSD) working in the edge-on configuration. The SSDs tested in the system are 300 {mu}m thick with 1 or 2-cm-long strips and 100 {mu}m pitch. To ensure a very small dead area of the SSD working in edge-on configuration, the detector is cut perpendicular to the strips at a distance of only 20 {mu}m from the end of the strips. The 512-strip silicon detector is read out by eight 64-channel integrated circuits called DEDIX [Grybos et al., IEEE Trans. Nucl. Sci. NS-54 (2007) 1207]. The DEDIX IC operates in a single photon counting mode with two independent amplitude discriminators per channel. The readout electronic channel connected to a detector with effective input capacitance of about 2 pF has an average equivalent noise charge (ENC) of about 163 el. rms and is able to count 1 Mcps of average rate of input pulses. The system consisting of 512 channels has an excellent channel-to-channel uniformity-the effective threshold spread calculated to the charge-sensitive amplifier inputs is 12 el. rms (at one sigma level). With this system a few test images of a phantom have been taken in the 10-30 keV energy range.

  18. Effect of Load Distribution on Strip Crown in Hot Strip Rolling

    Institute of Scientific and Technical Information of China (English)

    Hongshuang DI; Jianzhong XU; Dianyao GONG; Xianghua LIU; Guodong WANG; Xiaoming HE; Liying BA

    2004-01-01

    In order to establish precision model, a software to calculate the strip crown of four-high hot rolling mill was developed by using affecting function method according to the strip crown calculation theory. The effect of work roll diameter, unit width rolling load, roll bending force, work roll crown, initial strip crown and reduction, etc, on load distribution effect rate was simulated by using the software. The results show that the load distribution effect rate increases with the increase of strip width, work roll diameter, unit width rolling load, roll bending force, work roll crown, initial strip crown and reduction. Based on the simulation results, base value of load distribution effect rate and fitting coefficients of six power polynomial of load distribution effect rate modification coefficient were determined considering all of the above parameters. A simplified mathematical model for calculating load distribution effect rate was established.

  19. Area specific stripping factors for AGS. A method for extracting stripping factors from survey data

    Energy Technology Data Exchange (ETDEWEB)

    Aage, H.K.; Korsbech, U. [Technical Univ. of Denmark (Denmark)

    2006-04-15

    In order to use Airborne Gamma-ray Spectrometry (AGS) for contamination mapping, for source search etc. one must to be able to eliminate the contribution to the spectra from natural radioactivity. This in general is done by a stripping technique. The parameters for performing a stripping have until recently been measured by recording gamma spectra at special calibration sites (pads). This may be cumbersome and the parameters may not be correct when used at low gamma energies for environmental spectra. During 2000-2001 DTU tested with success a new technique for Carborne Gamma-ray Spectrometry (CGS) where the spectra from the surveyed area (or from a similar area) were used for calculating the stripping parameters. It was possible to calculate usable stripping ratios for a number of low energy windows - and weak source signals not detectable by other means were discovered with the ASS technique. In this report it is shown that the ASS technique also works for AGS data, and it has been used for recent Danish AGS tests with point sources. (Check of calibration of AGS parameters.) By using the ASS technique with the Boden data (Barents Rescue) an exercise source was detected that has not been detected by any of the teams during the exercise. The ASS technique therefore seems to be better for search for radiation anomalies than any other method known presently. The experiences also tell that although the stripping can be performed correctly at any altitude there is a variation of the stripping parameters with altitude that has not yet been quite understood. However, even with the oddly variations the stripping worked as expected. It was also observed that one might calculate a single common set of usable stripping factors for all altitudes from the entire data set i.e. some average a, b and c values. When those stripping factors were used the stripping technique still worked well. (au)

  20. Modeling of continuous strip production by rheocasting

    Science.gov (United States)

    Matsumiya, T.; Flemings, M. C.

    1981-03-01

    A process was experimentally and mathematically modeled for continuous and direct production of metal strip from its molten state by the use of Rheocasting. The process comprises 1) continuous production of a Rheocast semisolid alloy, and 2) direct shaping of the semisolid into strip. Sn-15 pct Pb was used as the modeling alloy. Crack formation and surface quality of the strip produced depend on fraction solid and deformation force. Continuous, sound strip could be obtained with good surface quality when fraction solid was between 0.50 and 0.70 and deformation force did not exceed a given maximum. Sheet thickness depends on deformation force, fraction solid, rotor rate of Rheocaster and production line speed. At constant deformation force, sheet thickness increases as fraction solid increases, rotor rate decreases and line speed is reduced. Sheet thickness is larger in the center than in the edge, but the difference is reduced by applying edgers. Some segregation of lead toward the edges is observed, and the segregation increases as amount of deformation is increased. A mathematical model for heat flow, solidification and deformation was constructed. The model predicts the point of completion of solidification in the strip and sheet thickness as a function of deformation force and line speed. Calculations are in good agreement with experimental results.