Accumulation Step (accumulation + step)

Distribution by Scientific Domains

Selected Abstracts

Electrode Modified with Cobalt Cyclohexylbutyrate for the Determination of Low Molecular Weight Thiol Group Bearing Compounds Using Catalytic Stripping Voltammetry

Petr Jakubec
Abstract Glassy carbon electrode, modified with cobalt(II) cyclohexylbutyrate monohydrate immobilized in polystyrene matrix is usable for determination of thiol group bearing compounds both in oxidized and reduced forms using catalytic stripping voltammetry. The measurements are carried out in acetate buffer (pH,4.3) containing Tween 40. After the accumulation step at ,850,mV vs. Ag/AgCl a peak at ,170,mV is observed on linear sweep voltammogram, the height of which is proportional to the concentration of added thiol. Addition of carbon nanotubes into polystyrene film enhances the sensitivity of the modified electrode. The detection limit is 110,6,mol dm,3 for all studied thiols. The electrode can be regenerated by exposing it to the potential between 300,600,mV. [source]

Working Electrodes from Amalgam Paste for Electrochemical Measurements

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

Trace Determination of Chromium by Square-Wave Adsorptive Stripping Voltammetry on Bismuth Film Electrodes

Eleni Chatzitheodorou
Abstract This works reports the use of adsorptive stripping voltammetry (AdSV) for the trace determination of chromium on a rotating-disk bismuth-film electrode (BFE). During the reductive accumulation step, all the chromium species in the sample were reduced to Cr(III) which was complexed with cupferron and the complex was accumulated by adsorption on the surface of a preplated BFE. The stripping step was carried out by using a square-wave (SW) potential-time voltammetric signal. Electrochemical cleaning of the bismuth film was employed, enabling the same bismuth film to be used for a series of measurements in the presence of dissolved oxygen. The experimental variables as well as potential interferences were investigated and the figures of merit of the method were established. Using the selected conditions, the 3, limit of detection for chromium was 100,ng L,1 (for 120,s of preconcentration) and the relative standard deviation was 3.6% at the 2,,g L,1 level (n=8). Finally, the method was applied to the determination of chromium in real samples with satisfactory results. [source]

Surface-Grafted Multiporphyrin Arrays as Light-Harvesting Antennae to Amplify Photocurrent Generation

Mitsuhiko Morisue Dr.
Abstract Organized multiporphyrin arrays were developed on the conductive surface by a novel coordination-directed molecular architecture aiming at efficient photoelectric conversion. The basic strategy employs the mutual coordination of two imidazolylporphyrinatozinc(II) units to form a cofacial dimer. Thus, meso,meso -linked bis(imidazolylporphyrinatozinc) (Zn2(ImP)2) was organized onto imidazolylporphyrinatozinc on the gold substrate as a self-assembled monolayer. The organized Zn2(ImP)2 bearing allyl side chains was covalently linked by ring-closing olefin metathesis catalyzed with Grubbs catalyst. Alternating coordination/metathesis reactions allow the stepwise accumulation of multiporphyrin arrays on the gold electrode. A successive increase in absorption over a wide wavelength range occurred after each accumulation step of Zn2(ImP)2 on the gold electrode, and cathodic photocurrent generation was enhanced in the aqueous electrolyte system, containing viologen as an electron carrier. The significant increase of the photocurrent indicates that the multiporphyrin array works as a "light-harvesting antenna" on the gold electrode. [source]

Electroanalytical Determination of Promethazine Hydrochloride in Pharmaceutical Formulations on Highly Boron-Doped Diamond Electrodes Using Square-Wave Adsorptive Voltammetry

Francisco, Wirley
Abstract The electrochemical oxidation of promethazine hydrochloride was made on highly boron-doped diamond electrodes. Cyclic voltammetry experiments showed that the oxidation mechanisms involved the formation of an adsorbed product that is more readily oxidized, producing a new peak with lower potential values whose intensity can be increased by applying the accumulation potential for given times. The parameters were optimized and the highest current intensities were obtained by applying +0.78,V for 30 seconds. The square-wave adsorptive voltammetry results obtained in BR buffer showed two well-defined peaks, dependent on the pH and on the voltammetric parameters. The best responses were obtained at pH,4.0, frequency of 50,s,1, step of 2,mV, and amplitude of 50,mV. Under these conditions, linear responses were obtained for concentrations from 5.9610,7 to 4.7610,6,mol L,1, and calculated detection limits of 2.6610,8,mol L,1 (8.51,,g L,1) for peak 1 and of 4.6110,8,mol L,1 (14.77,,g L,1) for peak 2. The precision and accuracy were evaluated by repeatability and reproducibility experiments, which yielded values of less than 5.00% for both voltammetric peaks. The applicability of this procedure was tested on commercial formulations of promethazine hydrochloride by observing the stability, specificity, recovery and precision of the procedure in complex samples. All results obtained were compared to recommended procedure by British Pharmacopeia. The voltammetric results indicate that the proposed procedure is stable and sensitive, with good reproducibility even when the accumulation steps involve short times. It is therefore very suitable for the development of the electroanalytical procedure, providing adequate sensitivity and a reliable method. [source]