Application of voltammetric technique to the analysis of indanthrene dye in alkaline solution

The Indanthrene Olive Green B (C.I. Vat Green 3; C.I. 69500), VG3 dye, a vat dye bearing an anthraquinonoid group and a ketonic group, can be detected by differential pulse voltammetry in alkaline solution using glassy carbon electrode. on the adsorbed form the dyes are reduced into three cathodic steps at -0.54 V, -0.65 V and -0.93 V vs Ag/AgCl. The leuco form generated after previous electrolysis at controlled potential of -1 V can be detected by voltammetry due to its reoxidation peak at -0.08 V. An analytical method is proposed for determining the vat dye using modified glassy carbon electrode by electrochemical activation in alkaline medium. Linear relationship was observed between l(Pu) vs concentration from I X 10(-5) mol L-1 to 6.0 X 10(-4) mol L-1. The detection limit was calculated to be 9.3 X 10(-6) mol L-1. (c) 2005 Elsevier Ltd. All rights reserved.

Cathodic stripping voltammetric determination of cefaclor in pharmaceutical formulations

A sensitive method is described for the determination of cefaclor by cathodic stripping voltammetry at the hanging mercury drop electrode. cefaclor is accumulated at the electrode surface as a mercury salt, which is reduced at -0.67 V. The optimum accumulation potential and accumulation time were +0.15 V and up to 180 s, respectively. Linear calibration graphs were obtained between 3.9 mu g.L-1 to 39 mu g.L-1 and the limit of determination was evaluated to be 1.9 mu g.L-1. The method was applied successfully to the determination of cefaclor in pharmaceutical formulations.

Voltammetric determination of fenbendazole in veterinarian formulations

A versatile voltammetric method for quantitative determination of fenbendazole (FBZ) in commercial tablets has been proposed, where direct dissolution of tablets is carried out in 0.1 mol l(-1) tetrabutylamoniun tetrafluorborate containing dimethylformamide solutions. Linear sweep (LSV), square wave (SWV) and differential pulse (DPV) voltammetry techniques were applied to study FBZ at a glassy carbon electrode, exhibiting a well defined irreversible oxidation peak at 1.15 V vs. SCE. This methodology allows a precise quantitative determination of FBZ presenting detection limits of 5.2 x 10(-5) (LSV), 5.0 x 10(-6) (DPV) and 5.0 x 10(-5) mol l(-1) (SWV). (C) 2002 Elsevier B.V. B.V. All rights reserved.

Aspects of cathodic stripping voltammetry at the hanging mercury drop electrode and in non-mercury disposable sensors

Cathodic stripping voltammetry (CSV) and accumulation at the hanging mercury drop electrode are reviewed briefly. Proposals in a recent IUPAC technical report are considered. Three recent developments in CSV are discussed: the adaptation of CSV methods developed for use with the hanging mercury drop electrode for use with screen-printed carbon electrodes in disposable sensors, the use of reactive accumulation, and the chemometric use of kinetic methods of determination with pulse methods in CSV.

A square-wave voltammetric method for analysing the colour marker quinizarine in petrol and diesel fuels

This work presents an electroanalytical method based on square-wave voltammetry (SWV) for the determination of quinizarine (QNZ) in a mixture of Britton-Robinson buffer 0.08 mol L-1 with 30% of acetonitrile. The QNZ was oxidized at glassy carbon electrode in and the well-defined peak at +0.45 V vs. Ag/AgCl can be used for its determination as colour marker in fuel samples. All parameters were optimized and analytical curves can be constructed for QNZ concentrations ranging from 2.0 x 10(-6) mol L-1 to 1.4 x 10(-5) mol L-1, using f = 60 Hz and E-sw = 25 mV. The method offers a limit detection of 4.12 x 10(-7) mol L-1 and a standard deviation of 4.5% when six measurements of 1.25 x 10(-5) mol L-1 are compared. The method was successfully applied for determining QNZ in gasoline and diesel oil and the obtained results showed good agreement with those reported previously. (c) 2006 Elsevier Ltd. All rights reserved.

Indirect polarographic and cathodic stripping voltammetric determination of cefaclor as an alkaline degradation product

Cefaclor is not reducible at a mercury electrode, but it can be determined polarographically and by cathodic stripping voltammetry as its initial alkaline degradation product which is obtained in high yield by hydrolysis of cefaclor in Britton-Robinson (B-R) buffer pH 10 at 50 degrees C for 30 min (reduction peak at pH 10, -0.70 V). Differential pulse polarographic calibration graphs are linear up to at least 1 x 10(-4) mol l(-1). Recoveries of 93% of the cefaclor (n = 3) were obtained from urine spiked with 38.6 mu g ml(-1) using this polarographic method with 1 ml urine made up to 10 ml with pH 10 buffer. Using cathodic stripping voltammetry and accumulating at a hanging mercury drop electrode at -0.2 V for 30 s, linear calibration graphs were obtained from 0.35 to 40 mu g ml(-1) cefaclor in B-R buffer pH 10. A relative standard deviation of 4.2% (eta = 5) was obtained, and the limit of detection was calculated to be 2.9 ng ml(-1). Direct determination of cefaclor in human urine (1 ml of urine was made up to 10 ml with pH 10 buffer) spiked to 0.39 mu g ml(-1) was made (recovery 98.6%). (C) 1999 Elsevier B.V. B.V. All rights reserved.

Voltammetric sensor for sodium nitroprusside determination in biological fluids using films of poly-L-lysine

Sodium nitroprusside (NP), a commercial vasodilator, can be pre-concentrated on vitreous carbon electrode modified by films of 97.5%: 2.5% Poly-L-lysine (PLL): glutaraldehyde (GA). This coating gives acceptable anion exchange properties whilst giving the required improvement of adhesion to the glassy carbon electrode surface. Linear response range and detection limit on nitroprusside in B-R buffer pH 4.0, were 1 x 10(-6) to 2 x 10-(5) mol L-1 and 1 x 10(-7) mol L-1, respectively. The repeatability of the proposed sensor, evaluated in term of relative standard deviation, was measured as 4.1% for 10 experiments. The voltammetric sensor was directly applied to determination of nitroprusside in human plasma and urine samples and the average recovery for these samples was around 95-97% without any pre treatment.

Voltammetric assay of albendazole in pharmaceutical dosage forms

A simple, rapid inexpensive voltammetric method have been developed for the quantitative determination of albendazole (ABZ) as the pure assay, by direct dissolution of commercial tablets in HCl solutions. Studies with linear sweep (LSV), square-wave (SWV) and differential pulse voltammetry (DPV) were carried out ABZ in aqueous medium at a glassy carbon electrode. A well defined irreversible oxidation peak current was obtained at 1,00V vs. SCE. The method permits a precise quantitative determination of ABZ using the standard addition method. The detection limits for the three voltammetric techniques were found to be 3.0 x 10(-5) M (LSV), 6.2 x 10(-5) M (SWV) and 4.0 x 10(-5) M (DPV).

Conductive composites of natural rubber and carbon black for pressure sensors

Composites of natural rubber and carbon black have attracted great interest due to their technological applications. In this work natural rubber (NR) and carbon black (CB) were compounded, aiming the development of composites with good mechanical properties, processability and electrical conductivity for use as pressure sensors. The electrical conductivity changes from 10(-11) to 10(-2) S.cm(-1) depending on the percentage of CB in the composite. It was also observed that the conductivity varies reversibly and linearly with the applied pressure. The latter demonstrates that this material can be used as pressure sensors.

Determination of the relative contribution of phenolic antioxidants in orange juice by voltammetric methods

The electrochemical oxidation of caffeic, chlorogenic, sinapic, ferulic and p-coumaric acids was investigated by cyclic voltammetry on acetate buffer pH 5.6 on glassy carbon electrode and modified glassy carbon electrode. According to their voltammetric behavior, the antioxidant activity of these phenolic acids was evaluated and the results pointed to the following sequence: caffeic acid (E-a = +0.31 V) > chlorogenic acid (+ 0.38 V) > sinapic acid (+ 0.45 V) > ferulic acid (+ 0.53 V) >p-coumaric acid (+ 0.73 V). The results were confirmed by DPPH test, which evidenced the strongest antiradical activity for compounds possessing the cathecol moiety (caffeic and chlorogenic acids). Linear calibration graphs were obtained for their determination at concentrations from 1 x 10(-4) to 1 x 10(-3) mol L-1. The method was applied to orange juice. Selectivity was illustrated by the analysis of caffeic and chlorogenic acids electrodeposited on a glassy carbon electrode previously modified by electrochemical activation in the presence of ascorbic acid. (C) 2003 Elsevier B.V. All rights reserved.

Study of an organically modified clay: Selective adsorption of heavy metal ions and voltammetric determination of mercury(II)

In this work, a hydrophilic clay, Na-montmorillonite from Wyoming, USA, was rendered organophilic by exchanging the inorganic interlayer cations for hexaclecyltrimethylammonium ions (HDTA), with the formulae of [(CH3)(3)N(C16H33)](+) ion. Based on fact that organo-clay has high affinities for non-ionic organic molecules, 1,3,4-thiadiazole-2,5-dithiol was loaded oil the HDTA-montmorillonite surface, resulting in the 1,3,4-thiadiazole-2,5-dithiol-HDTA-montmorillonite complex (TDD-organo-clay).The following properties of TDD-organo-clay are discussed: selective adsorption of heavy metal ions measured by batch and chromatographic column techniques, and utilization as preconcentration agent in a chemically modified carbon paste electrode (CMCPE) for determination of mercury(II).The main point of this paper is the construction of a selective sensor, a carbon paste electrode modified with TDD-organo-clay, its properties and its application to the determination of mercury(II) ions, as this element belongs to the most toxic metals. The chemical selectivity of this functional group and the selectivity of voltammetry were combined for preconcentration and determination. (c) 2005 Elsevier B.V. All rights reserved.

Transport and sensors properties of nanostructured antimony-doped tin oxide films

Tin oxide thin films doped with 7 mol% antimony oxide multilayer were prepared by the polymeric precursor method. Morphological characterization revealed films with round-shaped grains, nanometric size (similar to 13 nm), and low roughness. These films display high transmittance (similar to 80%) in the visible range of transmittance spectra, which is desirable for transparent conductive oxide films. Analysis on electrical resistivity versus temperature data showed two different conduction mechanisms toward the temperature range. The gas sensor properties measurement of the thicker thin film revealed good sensibility for the NOx. (c) 2006 Elsevier B.V. All rights reserved.

Studies of the voltammetric behavior and determination of diazo reactive dyes at mercury electrode

The electrochemical reduction of two reactive dyes: Procion Red HE-3B 9 (RR120) and Procion Green HE-4BD (RG19) was investigated using cyclic voltammetry, differential pulse and DC, polarography, chronoamperometry and controlled potential electrolysis at mercury electrodes. The bis-azo groups of the RR120 dye are reduced together in one single step of four electrons, the bis-azo groups of the RG19 dye are reduced in two steps owing to the difference in the electron densities promoted by the different substituents in the benzene rings adjacent to the azo groups. The bis-monochlorotriazine reactive groups in both dyes are reduced only in acidic medium in their protonated form, leading to the reduction of the triazine groups. The reduction mechanism of both reactive dyes is discussed. Both dyes can be quantified in aqueous medium by differential pulse polarography in the concentration range of 1 x 10(-7) mol L-1 to 1 x 10(-5) mol L-1 by monitoring the reduction of the chromophore group or the reactive group.

Regeneration of poly-L-lysine modified carbon electrodes in the accumulation and cathodic stripping voltammetric determination of the cromoglycate anion

Cromoglycate is accumulated on a poly-L-lysine (PLL) modified carbon electrode best from pH 4 solution, where it is anionic and the PLL is cationic, and at which pH the cromoglycate gives a good reduction peak at -0.82 V. The PLL film can be regenerated readily by washing the electrode with 3 M sodium hydroxide solution, in which the PLL is deprotonated. Regeneration of the film is not required as frequently when larger amounts of PLL are incorporated into it. This allows standard addition procedures to be carried out without regenerating the electrode. Linear calibration graphs have been obtained typically in the range 0.1 - 1.5 mug ml(-1). Detection limits have been calculated to be 10 ng ml(-1). The standard addition method has been applied satisfactorily to diluted urine solutions. (C) 2003 Elsevier B.V. B.V. All rights reserved.

A new method for extending the range of conductive polymer sensors for contact force

This paper describes a technique for extending the force range of thin conductive polymer force sensors used for measuring contact force. These sensors are conventionally used for measuring force by changing electrical resistance when they are compressed. The new method involves measuring change in electrical resistance when the flexible sensor, which is sensitive to both compression and bending, is sandwiched between two layers of spring steel, and the structure is supported on a thin metal ring. When external force is applied, the stiffened sensor inside the spring steel is deformed within the annular center of the ring, causing the sensor to bend in proportion to the applied force. This method effectively increases the usable force range, while adding little in the way of thickness and weight. Average error for loads between 10 N and 100 N was 2.2 N (SD = 1.7) for a conventional conductive polymer sensor, and 0.9 N (SD = 0.4) using the new approach. Although this method permits measurement of greater loads with an error less than 1 N, it is limited since the modified sensor is insensitive to loads less than 5 N. These modified sensors are nevertheless useful for directly measuring normal force applied against handles and tools and other situations involving forceful manual work activities, such as grasp, push, pull, or press that could not otherwise be measured in actual work situations.