Screen-printed carbon electrode modified with poly-L-histidine applied to voltammetric determination of chromium (VI)

The present work reports the use of a screen-printed carbon electrode (SPCE) modified by poly-L-histidine film to determine chromium (VI). Stable films can be formed by direct addition of PH solution 1 % (w/v) on the electrode surface, followed by heating at 80°C during 5 min. Calibration curves can be constructed for Cr(VI) from 1.0 × 10-5 mol L-1 to 7.0 × 10-5 mol L-1 Cr (VI) in acetate buffer pH 4 using a preconcentration step of 60s at open circuit potential. A relative standard deviation of 3.2% was for five determination of 4.0 × 10 -5 mol L-1 Cr (VI). The method was successful applied to determination of Cr(VI) in wastewater samples from a leather dyeing industry. copyright The Electrochemical Society.

Voltammetric determination of sulfite using graphite paste electrode modified with nanoparticles of copper pentacyanonitrosylferrate

Copper Pentacyanonitrosylferrate (NCuNP) nanoparticles were prepared in formamide solvent. The material was characterized by Infrared (FTIR), X-Ray Diffraction (XRD) and Ultraviolet-Visible (UV-Vis) Spectroscopy. The Cyclic Voltammogram (CV) the modified graphite paste electrode with NCuNP exhibits two redox couples with (Eθ,)1 = 0.29 and (E θ,)2 = 0.86 V attribute at Cu(I)/Cu (II) and Fe(II)(CN)5NO/Fe(III)(CN) 5NO processes, respectively (KCl = 1.0 mol L-1; v = 20 mV s-1). The redox couple with (Eθ,)2 presents an electrocatalytic response for sulfite. The modified graphite paste electrode gives a linear response of 7.0 × 10-4 to 3.0 × 10-2 mol L-1 (r = 0.998), for sulfite determination with Detection Limit (DL) of 1.76 × 10-3 mol L-1 and an amperometric sensitivity of 3.38 mA/mol L-1 and relative standard desviations ± 3% (n=3). ©The Electrochemical Society.

Voltammetric Study of a Cubic Silsesquioxane Organically Modified with Imidazole and their Subsequent Reaction with Cadmium and Hexacyanoferrate (III)

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Voltammetric determination of ethyl acetate in ethanol fuel using a Fe 3+/Nafion®-coated glassy carbon electrode

A voltammetric method for the determination of ethyl acetate in ethanol fuel using a Fe3+/Nafion®-coated glassy carbon electrode (GCE) is proposed. The ethyl acetate present in the ethanol fuel was previously converted to acetohydroxamic acid via pretreatment with hydroxylamine chloride. The acetohydroxamic acid promptly reacted with the iron (III) present in the film, producing iron (III) acetohydroxamate, which presents a well-defined voltammetric peak current at -0.02 V. Optimization of the voltammetric parameters for the cyclic, linear sweep, square wave, and differential pulse modalities was carried out for this chemically-modified electrode. Square wave voltammetry afforded the best response for acetohydroxamic acid detection. The analytical curve for this species was linear from 9 to 100 μmol L 1 according to the following equation: ip (μA) = 0.27 + 2.55Cacetohydroxamic acid (μmol L 1), with linear correlation coefficient equal to 0.993. The technique presented limit of detection equal to 5.3 μmol L 1 and quantification limit of 17.6 μmol L 1. The proposed method was compared to the official method of ethyl acetate analysis (Gas Chromatography), and a satisfactory correlation was found between these techniques. © 2012 Elsevier Ltd. All rights reserved.

Electrochemical behavior and voltammetric determination of pyrazinamide using a poly-histidine modified electrode

Pyrazinamide (Pyrazinecarboxamide-PZA) is a drug that is used to treatment tuberculosis. In the present work, the voltammetric behavior of PZA was studied using a screen-printed modified electrode (SPCE). The modified electrode was constructed using poly-histidine films, and it showed an electrocatalytic effect, thus promoting a decrease in PZA reduction potential and improving the voltammetric response. Cyclic voltammetry and electrochemical impedance spectroscopy techniques have been employed in order to elucidate of the electrodic reaction. The results allowed the proposal that in the PZA reduction, a further chemical reaction occurs that corresponds to a second-order process which is subsequent to the electrode reaction. In addition, a sensitive voltammetric method was developed, and it was successfully applied for PZA determination in human urine samples. The best response was found using SPCE modified with poly-histidine prepared by histidine monomer electropolymerization (SPCE/EPH). The electroanalytical performance of the SPCE/EPH was investigated by linear sweep (LSV), differential pulse (DPV), and square wave voltammetry (SWV). A linear relationship between peak current and PZA concentrations was obtained from 9.0 × 10-7 to 1.0 × 10-4 mol L-1 by using DPV. The limit of detection at 5.7 × 10 -7 mol L-1 was estimated, and a relative standard deviation of the 5.0 × 10-6 mol L-1 of PZA of 10 measurement was 3.7%. © 2012 Elsevier B.V. All rights reserved.

A new hybrid polyhedral cubic silsesquioxane chemically modified with 4-amino-5-(4-pyridyl)-4H-1,2,4-triazole-3-thiol (APTT) and copper hexacyanoferrate(III) for voltammetric determination of nitrite

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

A cubic silsesquioxane modified with purpald®: Preparation, characterization and a voltammetric application for determination of sulfite

A novel composite formed by interaction of a octa(3-chloropropyl)octasilsesquioxane modified with Purpald®, and its subsequent reaction with silver and hexacyanoferrate (III) (AgHSP), was synthesized and initially characterized by Fourier transform infrared spectra (FTIR) and cyclic voltammetry. The cyclic voltammogram of the modified graphite paste electrode with AgHSP, showed one redox couple with formal potential Eθ'=0.64V (vs Ag/AgCl, KNO3, 1.0 mol L-1; v = 20 mV s-1), attributed to the Fe2+(CN)6/ Fe3+(CN)6 process. The redox couple presents an electrocatalytic response for determination of sulfite. The modified electrode showed a linear response from 7.0×10-5 to 1.0×10-3 mol L-1 with the corresponding equation Y(μA) = 18.05 + 29.983×103 [sulfite], and a correlation coefficient of r=0.999. The method showed a detection limit of 0.115×10-4 mol L-1 with a relative standard deviation of ± 4% (n = 3) and amperometric sensitivity of 29.983×10-3A mol L-1. The modified electrode showed a excellent stability and good reproducibility during experiments. © 2013 by ESG.

Sensitive voltammetric sensor for fast detection of mycolic acids present in mycobacteria

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Cost-effective composite electrode for the fast voltammetric screening and determination of riboflavin (B2) and pyridoxine (B6) in pharmaceuticals

Different solid composites made by mechanical dispersions of graphite particles into heated paraffin (from 65 to 80% graphite, in mass) were prepared and assessed in order to optimize their use in electrochemical and electroanalytical procedures for bioanalysis. Besides these, composites were also evaluated by thermoanalytical techniques aiming to study their conservation and long-term stability (over eight months without special care), among others. Best results were found at 80% m/m graphite in paraffin. Such electrode combines low-cost, stability, sensitivity, ease of maintenance and clearance, besides the possibilities of manufacture in many different forms and shapes (with or without modifications) and applicability in a wide range of pH. Electrochemical studies by different voltammetric techniques involving vitamins from complex B (riboflavin and pyridoxine) leaded to a better understanding about their electrooxidative processes onto carbon-composite electrodes, specially regarding reversibility and pH-dependence. Data were also acquired and optimized with analytical purposes, being square-wave voltammetry in pH 4.2 chosen by its many advantages. Good linearity between peak responses as function of concentration were reached from 5 to 43 μmol L-1 for riboflavin (peak at -0.257 V) and up to 8.5 × 10-4 mol L -1 for pyridoxine (peak at +1.04 V), best studied conditions; limits of detection (at an S/N of 3) for both analites showed to be circa 1.0 mol L-1. Different commercial samples were analyzed for riboflavin (EMS® complex B syrup) and pyridoxine (Citoneurin 5000 Merck® ampoules) providing 96.6% and 98.7% recoveries, respectively.

Simple, Direct and Simultaneous Stripping Voltammetric Determination of Lead and Copper in Gasoline Using an In Situ Mercury Film Electrode

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

A cubic silsesquioxane modified with purpald (r) : preparation, characterization and a voltammetric application for determination of sulfite

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

A novel hybrid composite formed by reaction of 4,5-diphenyl-2-imidazolethiol with hexacyanoferrate (iii) and subsequent reaction with copper (ii): preparation, characterization and a voltammetric application for determination of l-glutatione

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Enhancement of voltammetric determination of quinizarine based on the adsorption at surfactant-adsorbed-layer in disposable electrodes

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Voltammetric sensor for simultaneous determination of p-phenylenediamine and resorcinol in permanent hair dyeing and tap water by composite carbon nanotubes/chitosan modified electrode

p-Phenylenediamine (PPD) and resorcinol (RSN) are hair dye precursors of permanent dyeing more used worldwide. The present work describes a simple and economic voltammetric sensor for simultaneous determination of both components in commercial hair dyeing and tap water at low concentrations. PPD and RSN are oxidized at + 0.17 and + 0.61 V vs. Ag/AgCl at glassy carbon electrode coated by composites of multiwall carbon nanotubes with chitosan (MWNTs-CHT/GCE), which anodic currents density normalized are 10% and 70% higher in relation to the unmodified electrode, respectively. The calibration curve for simultaneous determination of PPD and RSN showed linearity between 0.55 and 21.2 mg L-1 with detection limits of 0.79 and 0.58 mg L-1 to PPD and RSN, respectively. The relative standard deviations found for ten determinations were of 0.73 and 2.35% to 2.70 mg L-1, and 0.87 and 1.08% to 15.96 mg L-1 to PPD and RSN, respectively. The voltammetric sensor was applied to determination of PPD and RSN in tap water and commercial hair dyeing samples and the average recovery for these samples was around 97%. The products generated from PPD and RSN reaction such as was p-quinonediimine and bandrowski base were detected by LC-MS/MS and UV-vis spectrophotometry. (C) 2014 Published by Elsevier B.V.

A study of the main oxidation products of natural pyrite by voltammetric and photoelectrochemical responses

(Photo)electrochemical experiments on pyrite electrodes in acetic acid-acetate buffer (pH = 4.5) are conducted to clarify the main oxidation reactions and the nature of the products. Electrochemical reactions in the -0.40 to 1.25 V (SHE) potential range are studied, and the production of iron (III) polysulfide from anodically formed iron oxides and polysulfides is discussed. Charges experimentally obtained are considered for the estimation of the most likely stoichiometry of the metallic polysulfide. The photoselectivity of the pyrite corrosion process indicates that the oxidation reactions of Fe2+ and S-2(2-) an not consecutive. The changes in stoichiometry and/or annihilation of crystalline structure defects are responsible for the observed photosensitivity of pyrite. A description of light effects on the interfacial behaviour and stability of pyrite is presented in terms of conduction and valence band energies, and thermodynamic potentials. (C) 2001 Elsevier Science B.V. All rights reserved.