Romeu C. Rocha-Filho

Universidade Federal de São Carlos, São Carlos do Pinhal, São Paulo, Brazil

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Publications (102)271.1 Total impact

  • Gabriel F. Pereira · Romeu C. Rocha-Filho · Nerilso Bocchi · Sonia R. Biaggio
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    ABSTRACT: Galvanostatic electrolyses are performed in a filter-press reactor to investigate the electrochemical degradation of picloram (100 mg L−1, from a commercial herbicide formulation) using a boron-doped diamond (BDD) or β-PbO2 anode. The effect of pH (3, 6, or 10), applied current density (japl = 10, 30, or 50 mA cm−2), and absence or presence of Cl- ions (25 mM) in the supporting electrolyte (aqueous 0.10 M Na2SO4) is investigated, while the picloram concentration, solution chemical oxygen demand (COD) and total organic carbon content (TOC), and energy consumption are monitored as a function of electrolysis time. From the obtained results, it is clear that the electrochemical degradation of picloram is possible using either of the anodes, but with different overall performances. In general, the presence of Cl- ions in the supporting electrolyte (leading to electrogenerated active chlorine) has a positive effect on the performance of both anodes, except for TOC abatement using the BDD anode; the best electrodegradation performances are attained at pH values around 6, when HClO is the predominant active-chlorine species. Faster rates of initial electrodegradation of picloram and of solution TOC abatement are obtained as japl is increased, but, as expected, lower energy consumptions are always attained at the lowest value of japl. The performances of the two anodes are virtually the same in the initial degradation of picloram; however, the BDD anode greatly surpasses the β-PbO2 anode in the abatement of solution COD or TOC. This confirms the importance of the oxidation power of the anode, even when indirect oxidation by active chlorine plays a concomitant role.
    Electrochimica Acta 05/2015; DOI:10.1016/j.electacta.2015.05.134 · 4.50 Impact Factor
  • Gustavo Stoppa Garbellini · Romeu Cardozo Rocha-Filho · Orlando Fatibello-Filho
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    ABSTRACT: Voltammetric methods for the determination of the fluoroquinolone ciprofloxacin (CIP) were developed using a cathodically pretreated boron-doped diamond (BDD) electrode coupled with square-wave voltammetry (SWV) and differential pulse voltammetry (DPV). In cyclic voltammetric measurements, the CIP electrooxidation was an irreversible process controlled by diffusion of the analyte to the electrode surface. Analytical curves were obtained for CIP concentrations from 2.50 to 50.0 µmol L–1, for SWV, and from 0.500 to 60.0 µmol L–1, for DPV, with detection limits of 2.46 and 0.440 µmol L–1, respectively. On the other hand, adequate recovery values were obtained for the determination of CIP in synthetic urine samples by DPV. On the other hand, SWV was employed to evaluate the interaction between CIP and double-stranded dsDNA (calf thymus in aqueous solution). From the obtained results, we inferred that CIP binds to dsDNA by intercalation, with a binding constant calculated as 5.91 × 105 L mol–1. Thus, the cathodically pre-treated BDD electrode was successfully used for the determination of CIP in biological samples and for studies on the interaction of that fluoroquinolone with dsDNA.
    Analytical methods 03/2015; 7(8). DOI:10.1039/C5AY00625B · 1.94 Impact Factor
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    ABSTRACT: A simple, rapid, and low-cost electroanalytical method is reported for the simultaneous determination of aspartame (AS) and acesulfame-K (AK) in food products. This method involves coupling differential pulse voltammetry (DPV) with an anodically pretreated boron-doped diamond (AP-BDD) electrode and 0.30 mol L−1 H2SO4 as supporting electrolyte. Thus, a separation of about 500 mV of the oxidation peak potentials of AS and AK was attained and the detection limits obtained for their simultaneous determination were 1.60 µmol L−1 (for AS) and 280 µmol L−1 (for AK). The proposed DPV method was successfully applied in the simultaneous determination of these sweeteners in three types of commercial food products; in the case of AS, the obtained results are similar at 95 % confidence level to those obtained using a reference HPLC method. The proposed method is of great analytical interest, as it yields detection limits that are lower than those attained by the only other electroanalytical method proposed in the literature.
    Analytical methods 01/2015; 7(5). DOI:10.1039/C4AY03047H · 1.94 Impact Factor
  • João Pedro Silva · Sonia R. Biaggio · Nerilso Bocchi · Romeu C. Rocha-Filho
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    ABSTRACT: The spinel LiMn2O4 was obtained by a microwave-assisted solid-state reaction between LiOH·H2O and ε-MnO2 in a practical setup using a domestic microwave oven. XRD analyses showed that the spinel LiMn2O4 was obtained as a single phase after only 3 min of microwave heating. SEM micrographs revealed particles having a prismatic morphology and sizes in the 0.5–1.5 μm range. The characteristic voltammetric profile of the spinel LiMn2O4 was obtained for the synthesized material, while its charge − discharge tests presented good electrochemical stability and a significant initial specific capacity (95 mA h g− 1) at a high discharge rate (C/1). These results indicate that a rapid and facile microwave-assisted synthesis can yield the spinel LiMn2O4 with adequate properties to be used as a cathode material in lithium-ion batteries.
    Solid State Ionics 12/2014; 268:42–47. DOI:10.1016/j.ssi.2014.09.025 · 2.11 Impact Factor
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    ABSTRACT: The electrodegradation of the Acid Yellow 49 dye (100 mg L-1 in 0.1 mol L-1 Na2SO4) was investigated using boron-doped diamond (BDD), Ti-Pt/beta-PbO2, and Ti/RuO2-TiO2 (DSA (R)) anodes. Galvanostatic electrolyses (5, 15 or 30 mA cm(-2)) were carried out in an electrochemical flow system, with a filter-press reactor. Best performances were attained with the BDD anode and worst with the DSA (R) anode. The dye solution was adequately decolorized using an electrical charge per unit volume of dye solution (Q(apl)) slightly higher than 0.60 A h L-1, applied with the BDD anode at a current density of only 5 mA cm-2. At this current density, COD and TOC abatements of 37% and 20% were attained with Q(apl) values of only 0.60 and 1.20 A h L-1, respectively; this indicates the feasibility of abating the organic load of the dye solution by simply increasing the value of Q(apl).
    International journal of electrochemical science 11/2014; 10:1361-1371. · 1.96 Impact Factor
  • Carla Dalmolin · Sonia R. Biaggio · Nerilso Bocchi · Romeu C. Rocha-Filho
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    ABSTRACT: The room-temperature ionic liquid (RTIL) 1-butyl-3-methylimidazolium tetrafluoroborate, BMIM BF4, was employed as electrolyte in the electrosynthesis of thin polypyrrole (PPy) films on a Pt substrate, and the resulting PPy electrodes were electrochemically characterized. Electrochemical impedance spectroscopy (EIS) was used to comparatively investigate the electric behavior of PPy produced in the RTIL and the one produced in a traditional acetonitrile/lithium salt system, and charge–discharge curves in the range 2.0–4.0 V (vs. Li/Li+) were obtained in a 1.0 M LiBF4 propylene carbonate solution. Although a reduction of the specific capacity for the PPy obtained in the RTIL was observed, compared to that of the PPy film synthesized in the acetonitrilic electrolyte, its chronopotentiometric profile presented a plateau in the 2.7 V region. This is a remarkable result, considering that a linear decrease in this profile is usually observed for the majority of conducting polymer cathodes. PPy films obtained in BMIM BF4 presented globular morphology, with a special arrangement of nanoparticles constituting the globules; the EIS results indicated that this nanoscale structure may be contributing to a better definition of the redox characteristics during the PPy charge–discharge processes, as it happens for the well-organized structure of some metal oxides.
    Materials Chemistry and Physics 09/2014; 147(s 1–2):99–104. DOI:10.1016/j.matchemphys.2014.04.015 · 2.13 Impact Factor
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    ABSTRACT: The electrochemical degradation of a real textile effluent was carried out using Ti–Pt/β-PbO2 and Ti/Ti0.7Ru0.3O2 (DSA®) anodes in a filter-press flow cell, in the presence and absence of chloride ions, varying the pH (3, 7, 11) and temperature (25 °C and 45 °C) of the effluent, and monitoring the removal of its turbidity and chemical oxygen demand (COD). The best experimental conditions for turbidity and COD removal were attained in neutral and basic conditions, independently of temperature. Higher COD removal values were attained with the Ti–Pt/β-PbO2 anode, as a consequence of its higher oxidation power; the electric charge applied per unit volume of effluent significantly decreased in the presence of chloride ions, when instantaneous current efficiencies as high as 0.5 were attained in the initial electrooxidation stages. Under these conditions, the electric energy consumption necessary to oxidize the real textile effluent was as low as 50 kW h m−3. The use of chloride ions enabled higher COD removal efficiencies using the Ti–Pt/β-PbO2 and DSA® anodes than a purely mass-transport controlled process due to indirect oxidation processes mediated by the active chloro species.
    Chemical Engineering Journal 09/2014; 251:138–145. DOI:10.1016/j.cej.2014.04.032 · 4.32 Impact Factor
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    ABSTRACT: The growth of oxides on the surfaces of pure Ti and two of its ternary alloys, Ti-6Al-4V and Ti-6Al-7Nb, by micro-arc oxidation (MAO) in a pH 5 phosphate buffer was investigated. The primary aim was to form thick, porous, and aluminum-free oxide layers, because these characteristics favor bonding between bone and metal when the latter is implanted in the human body. On Ti, Ti-6Al-4 V, and Ti-6Al-7Nb, the oxides exhibited breakdown potentials of about 200 V, 130 V, and 140 V, respectively, indicating that the oxide formed on the pure metal is the most stable. The use of the MAO procedure led to the formation of highly porous oxides, with a uniform distribution of pores; the pores varied in size, depending on the anodizing applied voltage and time. Irrespective of the material being anodized, Raman analyses allowed us to determine that the oxide films consisted mainly of the anatase phase of TiO2, and XPS results indicated that this oxide is free of Al and any other alloying element.
    Materials Science and Engineering C 08/2014; 41:343–348. DOI:10.1016/j.msec.2014.04.068 · 3.09 Impact Factor
  • Ricardo F. Brocenschi · Romeu C. Rocha-Filho · Boris Duran · Greg M. Swain
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    ABSTRACT: We report on the use of flow injection analysis with amperometric detection (FIA-EC) to evaluate the potential of using diamond electrodes for the analysis of three estrogenic compounds: estrone, 17-β-estradiol, and estriol. Amperometric detection was performed using a cathodically pretreated boron-doped diamond electrode that offered low background current, relatively low limits of detection, and good response reproducibility and stability. For all three compounds, response linearity was observed over the concentration range tested, 0.10 to 3.0μmolL(-1), the sensitivity was ca. 10mALmol(-1), and the minimum concentration detection (S/N≥3) was 0.10μmolL(-1) (~27μgL(-1)). The response variability with multiple injections was ca. 10% (RSD) over 20 injections. For estrone, the oxidation reaction on diamond does not proceed through an adsorbed state like it does on glassy carbon. After an initial current attenuation, the diamond electrode exhibited a stable response (oxidation current) for 3 days of continuous use, indicative of minimal surface contamination or fouling by reaction intermediates and products. The method for estrone was assessed using spiked city tap and local river water. Estrone recoveries in spiked city and river water samples presented standard deviations of less than 10%. In summary, the FIA-EC method with a diamond electrode enables sensitive, reproducible, stable, quick, and inexpensive determination of estrogenic compounds in water samples.
    Talanta 08/2014; 126:12–19. DOI:10.1016/j.talanta.2014.02.047 · 3.51 Impact Factor
  • José M. Aquino · Romeu C. Rocha-Filho · Nerilso Bocchi · Sonia R. Biaggio
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    ABSTRACT: Hybrid thermal heating induced by a microwave oven was unprecedentedly used to successfully attain rapid and facile crystallization into the anatase phase of amorphous TiO2 nanotubes grown on a Ti substrate. Amorphous TiO2 nanotubes were obtained by anodic oxidation of a Ti foil either in aqueous or organic medium. Afterward, these TiO2 nanotubes were thermally treated by hybrid heating in a common commercial microwave oven. The as-grown amorphous nanotubes were characterized by SEM and XRD, whereas the evolution of the nanotubes crystallization with thermal treatment time was followed by XRD. The crystallization into the anatase phase of the amorphous TiO2 nanotubes occurred after only 2 or 3 min of hybrid thermal treatment, which is very short and convenient as compared with several hours that are needed when conventional thermal treatment is used.
    Materials Letters 07/2014; 126:52–54. DOI:10.1016/j.matlet.2014.04.005 · 2.27 Impact Factor
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    ABSTRACT: A square-wave voltammetry method for the determination of hydroxychloroquine (HCQ) in pharmaceutical and synthetic urine samples with a cathodically pretreated (CPT) boron-doped diamond (BDD) electrode was successfully developed. Using cyclic voltammetry, the HCQ oxidation was shown to be a one-electron diffusion-controlled process. The obtained SWVanalytical curve (I-pa/mu a = 0.033 + 1.24 [HCQ/mu mol L-1)]) for HCQ determination (using 0.1 mol L-1 H2SO4 as supporting electrolyte) presented a linear response from 0.1 to 1.9 mu mol L-1, with a detection limit of 0.06 mu mol L-1, the best value attained yet with an unmodified electrode. The proposed method was successfully applied in the determination of HCQ in pharmaceutical (tablets) samples, with results similar at a 95% confidence level to those obtained using a reference spectrophotometric method. Additionally, adequate recovery results were obtained for the determination of HCQ in doped synthetic urine samples. The novel proposed method is inexpensive and fast, with no need of sample pretreatment. (c) 2014 Elsevier B.V. All rights reserved.
    Journal of electroanalytical chemistry 04/2014; 719. DOI:10.1016/j.jelechem.2014.01.037 · 2.87 Impact Factor
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    ABSTRACT: Oxidation of anthraquinonic dye Acid Blue 62 by electrolysis with conductive-diamond electrodes is studied in this work. COD, TOC, and color have been selected to monitor the degradation of the molecule as a function of several operating inputs (current density, pH, temperature, and NaCl concentration). Results show that the electrochemical oxidation of this model of large molecules follows a first order kinetics in all the conditions assessed, and it does not depend on the pH and temperature. The occurrence of chloride ions in wastewaters increases the rate of color and COD removal as a consequence of the mediated oxidation promoted by the chlorinated oxidizing species. However, chloride occurrence does not have an influence on the mineralization rate. First-order kinetic-constants for color depletion (attack to chromophores groups), oxidation (COD removal), and mineralization (TOC removal) were found to depend on the current density and to increase significantly with its value. A single model was proposed to explain these changes in terms of the mediated oxidation processes. Rate of mineralization remained very close to that expected for a purely mass transfer-controlled process. This was explained assuming that mediated oxidation does not have a significant influence on the mineralization in spite it has some effect on intermediate oxidation stages. The efficiency of the oxidation was found to depend mainly on the concentration of COD being negligible the effect of the other inputs assessed except for the occurrence of chloride ions. Opposite, the efficiency of mineralization depends on concentration of TOC and current density and it did not depend on the chloride occurrence. This observation was found to have an important influence on the power required to remove a given percentage of the initial TOC or COD. To decrease COD efficiently, the occurrence of chloride in the solution is very important, while to remove TOC efficiently, it is more important to work at low current densities and chloride effect is negligible. Energy consumption could be decreased by folds using the proper conditions.
    Environmental Science and Pollution Research 03/2014; 21(14). DOI:10.1007/s11356-014-2784-0 · 2.76 Impact Factor
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    ABSTRACT: The Direct Black 22 dye was electrooxidized at 30 mA cm(-2) in a flow cell using a BDD or beta-PbO2 anode, varying pH (3, 7, 11), temperature (10, 25, 45 degrees C), and [NaCl] (0 or 1.5 g L-1). In the presence of NaCl, decolorization rates were similar for all conditions investigated, but much higher than predicted through a theoretical model assuming mass-transport control; similar behavior was observed for COD removal (at pH 7, 25 degrees C), independently of the anode. With no NaCl, COD removals were also higher than predicted with a theoretical model, which suggests the existence of distinct dye degradation pathways.
    Química Nova 01/2014; 37(8). DOI:10.5935/0100-4042.20140219 · 0.66 Impact Factor
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    ABSTRACT: Boron-doped diamond (BDD) films are excellent electrode materials, whose electrochemical activity for some analytes can be tuned by controlling their surface termination, most commonly either to predominantly hydrogen or oxygen. This tuning can be accomplished by e.g. suitable cathodic or anodic electrochemical pretreatments. Recently, it has been shown that amorphous carbon nitride (a-CNx) films may present electrochemical characteristics similar to those of BDD, including the influence of surface termination on their electrochemical activity toward some analytes. In this work, we report for the first time a complete electroanalytical method using an a-CNx electrode. Thus, an a-CNx film deposited on a stainless steel foil by DC magnetron sputtering is proposed as an alternative electrode for the simultaneous determination of dopamine (DA) and ascorbic acid (AA) in synthetic biological samples by square-wave voltammetry. The obtained results are compared with those attained using a BDD electrode. For both electrodes, a same anodic pretreatment in 0.1molL(-1) KOH was necessary to attain an adequate and equivalent separation of the DA and AA oxidation potential peaks of about 330mV. The detection limits obtained for the simultaneous determination of these analytes using the a-CNx electrode were 0.0656μmolL(-1) for DA and 1.05μmolL(-1) for AA, whereas with the BDD electrode these values were 0.283μmolL(-1) and 0.968μmolL(-1), respectively. Furthermore, the results obtained in the analysis of the analytes in synthetic biological samples were satisfactory, attesting the potential application of the a-CNx electrode in electroanalysis.
    Analytica chimica acta 10/2013; 797:30-9. DOI:10.1016/j.aca.2013.08.018 · 4.52 Impact Factor
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    ABSTRACT: A sensitive, simple, and rapid electrochemical method was developed for the determination of albendazole (ABZ) in anthelminthic pharmaceutical formulations using differential pulse voltammetry (DPV) with a cathodically pretreated boron-doped diamond (BDD) electrode and 0.05 mol L−1 H2SO4 as supporting electrolyte. The electrochemical behavior of ABZ obtained with cyclic voltammetry (CV) showed two oxidation peaks at 0.95 and 1.30 V vs. Ag/AgCl (3.0 mol L−1 KCl). The total number of electrons (four) transferred during the oxidation process was estimated from the scan rate dependence of this CV response. The proposed method resulted in an analytical curve ranging from 0.0797 to 8.36 μmol L−1, with a detection limit (based on 3-sigma) of 0.0625 μmol L−1. This novel DPV method was successfully applied to determine ABZ in three pharmaceutical formulations (tablets), with results similar to those obtained using a reference HPLC method.
    Journal of electroanalytical chemistry 10/2013; 707:15-19. DOI:10.1016/j.jelechem.2013.08.018 · 2.87 Impact Factor
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    ABSTRACT: 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-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 mmol L-1 in a BR buffer solution (pH 2.0), with a detection limit of 0.90 mmol L-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.
    Journal of the Brazilian Chemical Society 09/2013; 24(9):1504-1511. DOI:10.5935/0103-5053.20130190 · 1.25 Impact Factor
  • Laís T. Duarte · Sonia R. Biaggio · Romeu C. Rocha-Filho · Nerilso Bocchi
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    ABSTRACT: Oxide films were formed on the biocompatible alloy Ti–13Nb–13Zr in a phosphate buffer at open-circuit potential (Eoc), potentiodynamically up to 8 V, or by micro-arc oxidation (MAO) at 300 V. Their electrochemical properties were assessed in a phosphate buffer saline solution (PBS). EIS and SEM results showed that the Eoc and potentiodynamically formed oxide films were compact and behave as a monolayer, while the MAO oxide was a bilayered film (compact inner and porous outer layers). Open-circuit potential and EIS resistance values indicated that the MAO oxide provides the best corrosion protection for the alloy in PBS.
    Corrosion Science 07/2013; 72:35–40. DOI:10.1016/j.corsci.2013.02.007 · 3.69 Impact Factor
  • Sheila C. Canobre · Nerilso Bocchi · Romeu C. Rocha-Filho · Sonia R. Biaggio
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    ABSTRACT: Carbon fiber (CF) composites of organometallic intercalated polyaniline (Pani) and polypyrrole (Ppy) doped with polystyrene sulfonate (PSS) were electrochemically synthesized and tested as electrodes for lithium-ion batteries. From the results obtained by cyclic voltammetry, X-ray photoelectron spectroscopy, and energy-dispersive X-ray spectroscopy, it was concluded that the incorporation of copper(II) ions in the polymeric composite was successfully attained by adsorption of Cu2+ ions and 2,5-dimercapto-1,3,4-thiadiazole (DMcT) monomers on the carbon microfibers. The experimental electrochemical impedance response of the obtained Pani(DMcT–Cu ion)/CF composite was simulated by adequate equivalent electrical circuits. After 20 charge/discharge cycles, the experimental discharge specific capacity of the Pani(DMcT–Cu ion)/CF composite was 118 mA h g−1 (100% coulombic efficiency) using a 1 mol L−1 LiClO4 solution in propylene carbonate, and 110 mA h g−1 when a polymeric electrolyte was used. In the charge/discharge tests of the Ppy-PSS/Pani/CF composite as anode, a high discharge specific capacity of 225 mA h g−1 was obtained after 20 cycles. The resulting Ppy-PSS/Pani/CF/polymeric electrolyte/Pani(DMcT–Cu ion)/CF battery presented a specific capacity of 62 mA h g−1 and could be charged up to 2.0 V, yielding an energy density 425 W h g−1, with a coulombic efficiency of about 98%.
    Materials Chemistry and Physics 04/2013; 139(1):47–54. DOI:10.1016/j.matchemphys.2012.11.045 · 2.13 Impact Factor
  • Rogério A. Davoglio · Sonia R. Biaggio · Nerilso Bocchi · Romeu C. Rocha-Filho
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    ABSTRACT: Thin films of polypyrrole (Ppy) and poly-2,5-dimercapto-1,3,4-thiadiazole (poly(DMcT)) are electrochemically deposited on pieces of carbon fiber (CF) cloth, yielding flexible and high surface area composites that are characterized as electrodes for supercapacitors. A bilayered polymeric composite (CF/poly(DMcT)/Ppy) is obtained by depositing a nanometric layer of Ppy on CF already supporting a poly(DMcT) film. Electrochemical stability tests indicate that the Ppy film acts as a barrier that prevents the loss of the poly(DMcT) electroactive material, thus improving the charge-storage characteristics of the bilayered film even after 1000 cycles. Specific capacitance values of 460 ± 50 and 1130 ± 100 F g−1 are observed for electrodes made of the CF/Ppy and CF/poly(DMcT)/Ppy composites, respectively. Comparatively to similar Ppy composite materials used for supercapacitors, the bilayered film electrode here reported presents a significantly improved specific capacitance value.
    Electrochimica Acta 03/2013; 93:93–100. DOI:10.1016/j.electacta.2013.01.062 · 4.50 Impact Factor
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    ABSTRACT: The determination of bezafibrate (BZF) using square-wave voltammetry (SWV) and a cathodically pretreated boron-doped diamond electrode is proposed. Cyclic voltammetry results showed one irreversible oxidation peak for BZF at 1.20V (vs. Ag/AgCl (3.0molL(-1) KCl)) in a 0.04molL(-1) Britton-Robinson (BR) buffer solution (pH 2.0). Under optimized SWV conditions, a linear analytical curve is obtained for the BZF concentration range 0.10-9.1μmolL(-1) in the BR buffer solution (pH 2.0), with a detection limit of 0.098μmolL(-1). The obtained recoveries range from 93.4 to 108%. The proposed novel method was successfully applied in the determination of the BZF content in several pharmaceutical formulations (tablets) and the results are in close agreement (at a 95% confidence level) with those obtained using a comparative spectrophotometric method.
    Talanta 01/2013; 103:201-6. DOI:10.1016/j.talanta.2012.10.033 · 3.51 Impact Factor