Marcelo Firmino de Oliveira

Voltammetric determination of persulfate anions using an electrode modified with a Prussian blue film

Abstract Prussian blue [PB, iron(III) hexacyanoferrate(II)] films are effective for the electrocatalysis of the persulfate (peroxodisulfate)/sulfate redox system. This has been exploited in the voltammetric determination of persulfate anions using a PB-modified platinum disc electrode. A linear correlation between electrocatalytic current and persulfate concentration was found for the range 5×10−5 to 3×10−3 mol dm−3, using 0.100 mol dm−3 potassium chloride as supporting electrolyte at pH 4. This analytical method has the advantages of speed and ease of operation in relation to traditional titrimetric methods for persulfate determination. The applicability of the method to the determination of persulfate in a commercial hair bleaching ‘booster’ product is demonstrated.

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 3.0×10−5M (LSV), 6.2× 10−5M (SWV) and 4.0×10−5M (DPV).

Determinação de zinco em álcool combustível opr voltametria de redissolução anódica

The presence of heavy metals in fuel ethanol is obtained in different steps as production and storage of ethanol, constituting an inorganic contamination. Quantitative analysis of these contaminants has been usually carried out by conventional techniques as atomic absorption spectrofotometry. According to high sensibility of stripping voltammetric techniques for quantification of heavy metals and a few number of realized works for this kind of matrix, the aim of this work was to develop an electroanalytical procedure for zinc determination in fuel ethanol. Electrochemical determination for zinc in aqueous media by linear sweep voltammetry exhibited an anodic peak current in a potential of -1,12V vs. SCE, presenting linear dependence against zinc concentration in an interval of 5,0x10-7 to 5,0x10-6 mol.L-1 with an amperommetric sensibility of 1,2x106 mA.mol-1.L and a detection limit of 2,6x10-7 mol.L-1. Zinc determination in fuel ethanol commercial sample was obtained by addiction of 200 mL of sample in a final volume of 20 mL of supporting electrolite. The concentration of zinc in the sample was obtained by standard addiction method, presenting a value of 5,7± 0,19x10-5 mol.L-1 in zinc.

Determination of 3,4-methylenedioxymethamphetamine (MDMA) in Confiscated Tablets by High-Performance Liquid Chromatography (HPLC) with Diode Array Detector

Chromatographic analysis by the HPLC technique with Diode Array Detector was employed for MDMA determination. A mobile phase of methanol/water (90:10v/v) allowed a peak signal for MDMA in 16 minutes. Optimized spectrophotometric signal was obtained at a wavelength of 240 nm. The analytical curve from 5.0 to 100.0ppm of MDMA was obtained, showing a linear correlation coefficient of 0.9997 and a detection limit of 2.94ppm. This methodology was employed at the dosage of confiscated samples of ecstasy in the Scientific Police Laboratory of Ribeirao Preto-SP city.

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).

Comportamento voltamétrico da redução de 2-furfuraldeído em etanol utilizando eletrodo de carbono vítreo

This study reports the electrochemical behavior of 2-furfuraldehide reduction in ethanol using glassy carbon electrode, aiming to correlate adequate experimental conditions for determination of this 2-furfuraldehide in fuel ethanol. Obtained voltammograms for 2-furfuraldehide in a scan rate of 100mV.s-1 present a cathodic peak current in a potential of -1,45V vs. SCE for aqueous medium and -1,71V vs. SCE for alcoholic medium, being observed no anodic currents in these reactional media. The relation of ipc with v1/2 showed linear behavior in both media, exhibiting a mass transport controlled by diffusion. The analysis of electrochemical parameters obtained in this work has exhibited an irreversible behavior for the electrodic process. The dependence of cathodic peak current against concentration showed linearity in the interval of 9,5x10-4 to 5,8x10-3 mol L-1 for both media. The sensitivity of method on the aqueous and alcoholic medium was 13,4 and 13,0 (x 10-3) mA mol-1 L respectively. The limits of detection (L.D.) for 2-furfuraldehide, on the aqueous and alcoholic medium was 0,70 e 0,80 (x 10-3) mol L-1 respectively.

Production of methyl and ethyl biodiesel fuel from pequi oil (Caryocar brasiliensis Camb.)

We studied the physical and chemical characteristics of methyl and ethyl esters (biodiesel) produced by transesterification of pequi oil (Caryocar brasiliensis Camb.) in the presence of potassium hydroxide. The oil extracted from pequi seed comprises 60% of the fruit content. Such characteristics as density, acidity, viscosity, and carbon residue of the biodiesel meet ANP (Brazilian National Petroleum Agency) standards. Our tests demonstrated the feasibility of utilizing pequi oil for biodiesel production.

Eletrodo modificado em filme de paládio para a determinação voltamétrica de fosfito

Phosphite ions constitute an important inorganic component as phosphorus source in soil fertilization, showing a large number of advantages in relation to phosphate. The determination of this compound in fertilizing products is realized by classical methods of analysis as gravimetry, in the form of magnesium pyrophosphate or by mercurous chloride formation. However, there are some disadvantages in these methods as the necessity of high times of digestion and possible toxic residue production. So, this work has the objective to propose an alternative electrochemical method for phosphite determination. Electrochemical modification on electrode surface by electrodeposition of palladium has exhibited catalytic effect for oxidation of phosphite to phosphate ions in 1,0mol.L-1 sulfuric acid aqueous medium, being obtained a linear dependence in relation to phosphite concentration from 5,0x10-6 to 5,0x10-4 mol.L-1 with an amperometric sensibility of 8,5x104 mA.mol-1.L and a detection limit of 3.67x10-6 mol.L-1. In the absence of palladium film on platinum electrode no anodic peak current is observed for phosphite oxidation.

Use of baru oil ( Dipteryx alata Vog.) to produce biodiesel and study of the physical and chemical characteristics of biodiesel/petroleum diesel fuel blends

We describe production of methyl and ethyl esters derived from baru oil (Dipteryx alata Vog.). Water and alcohols are removed from the biodiesel obtained by simple distillation. We study the acidity, density, iodine number, viscosity, water content, peroxide number, external appearance, and saponification number of the oil, its methyl and ethyl esters (biodiesels) and their blends (B5, B10, B15, B20, and B30) with commercial diesel fuel.

Quantification of Arsenic in Sugar Cane Brandy of Minas Gerais Using Carbon Paste Electrode Modified with Carbon Nanotubes

An eletroanalytical method for determination of arsenic in sugar cane brandy using an electrode consisting of carbon paste modified with carbon nanotubes (CNTPE) and mineral oil has been developed. The cyclic (CV) and linear sweep voltammetry modes (LSV) with cathodic stripping were employed for CNTPE containing mineral oil. The analytical curves were linear from 30.0 to 80.0 µg L -1 for LSV. The limit of detection (L.O.D.) was 10.45 μg L -1 and limit of quantification (L.O.Q.) was 34.33 μg L -1 . The developed method was applied to the determination of arsenic in tree commercial sugar cane brandy samples. The results were in good agreement with those obtained by HGAAS, showing that CNTPE containing mineral oil can be successfully employed to the simultaneous determination of arsenic in sugar cane brandy samples.