Preparación de nanopartículas de plata en ausencia de polimeros estabilizantes

Silver nanoparticles (AgNPs) were prepared by means of the polyol method in the absence of stabilizing polymers. To accomplish this objective, AgNO3 was added to ethylene glycol in the presence of NaOH (1 mol.L-1), the suspension formed was irradiated with a microwave source for 60 seconds at a power of 465 watts. It was found that under these conditions AgNPs of sizes between 4-18 nm are formed. Also the results indicate that part of the ethylene glycol is oxidized to carbonyl compounds that reduce the Ag+. These organic compounds are adsorbed on the surfaces of AgNPs, forming a protective film that prevents their aggregation.

Utilização de argilas para purificação de biodiesel

This work describes the results of the purification of methyl biodiesel, obtained by oxidized soybean oil, using different methods. After the ester separation from the glycerin by decanting, the ester was purified each time with distillation, washing with water and adsorption with bauxite, bentonite and attapulgite. The removal of total contamination, unsaponifiable material, concentrations of free glycerin and soap were analyzed in the purified ester phase. The best result of purification was observed with the use of bentonite and bauxite, in the removal of soap and free glycerin respectively.

Reciclagem do crômio de resíduos químicos provenientes da determinação de carbono oxidável em fertilizantes orgânicos

This work proposes a separation, recovery and reuse procedure of chemical residues with chromium. This residue was generated by the determination of oxidizable carbon in organic fertilizers samples. The Cr(VI) of the residue was reduced with ethanol and precipitated with NaOH. The Cr(OH)3 precipitate was separated and oxidized to dichromate ions with hydrogen peroxide. This solution was used another time in organic carbon determination. The uses of recycled dichromate solution were appropriated in four successive recycling. The accuracy was proven using potassium hydrogen phthalate and ten organic fertilizer samples. The organic carbon results, determined with recycled solutions, were similar the conventional solution.

The importance of pre-treatment of spent hydrotreating catalysts on metals recovery

This work describes a three-step pre-treatment route for processing spent commercial NiMo/Al2O3 catalysts. Extraction of soluble coke with n-hexane and/or leaching of foulant elements with oxalic acid were performed before burning insoluble coke under air. Oxidized catalysts were leached with 9 mol L-1 sulfuric acid. Iron was the only foulant element partially leached by oxalic acid. The amount of insoluble matter in sulfuric acid was drastically reduced when iron and/or soluble coke were previously removed. Losses of active phase metals (Ni, Mo) during leaching with oxalic acid were compensated by the increase of their recovery in the sulfuric acid leachate.

Degradação eletroquímica da vinhaça usando eletrodo de diamante dopado com boro

The degradation of vinasses in aqueous solution from ethanol industry has been investigated by electrochemical oxidation using a boron doped diamond electrode (BDD). Samples of vinasses were electrolyzed in medium of (0.1 mol L-1) Na2SO4 solutions at controlled potentials of +2.4, +3.0 and +4.0 V (vs. Ag/AgCl) and exhibited considerable reduction of total organic carbon. The cyclic voltammetry studies indicate that the vinasses are oxidized irreversibly over the BDD at 2.0 V (vs. Ag/AgCl) in diffusion controlled process. From the experimental results it is clear that the BDD electrode can be a valuable tool to the electrochemical degradation of vinasses in practical applications

Recuperação de compostos de iodo de reagentes e soluções laboratoriais

This work presents simple routes to recover iodine compounds from oxidized laboratory chemicals and aqueous solutions (HI and KI) used in laboratory chemistry classes. These routes are based on the oxidation of iodide ions (I-) to iodine (I2) by an oxidant (H2O2) or reduction of oxidized iodine by red phosphorus or hydrazine. Both routes presented high yields. The oxidative route is of general use whereas the reductive one is appropriate for restoring original iodine reagents. Final wastes were generated in low amounts. This work is appropriate for teaching many laboratory techniques (e.g., distillation, titration and filtration) in the chemical laboratory.

New strategies for treatment and reuse of spent sulfidic caustic stream from petroleum industry

This work examines traditional and new routes for removal of H2S and other sulfur compounds from spent sufidic caustic (SSC). SH- (hydrogenosulfide) and S2- (sulfide) ions were quantitatively oxidized at 25 ºC using H2O2, NaOCl or a spent sulfochromic mixture. SH-/S2- ions were also removed via reaction with freshly prepared iron or manganese hydroxides, or after passing the SSC through strong basic anion exchange resins (OH- form). The treated caustic solution, as well as iron/manganese hydroxides, removed H2S from diesel samples at 25 ºC. SSC treatment via strong basic anion-exchange resins produced the treated caustic solution with the highest free alkalinity.

Aumento del contenido de ácidos húmicos en un carbón de bajo rango a través de la oxidación con aire y con peróxido de hidrogeno o ácido nítrico

Low-rank coals are an important source of humic acids, which are important in retention processes of water and nutrients in plants. In this study coal samples of Montelibano, Colombia, were oxidized with air at different temperatures and subsequently with H2O2 and HNO3. The materials were characterized by FTIR, proximate and elemental analysis, and quantification of humic acids. The oxidation process led to an increased content of oxygenated groups and humic acids in the carbonaceous structure. The solid oxidized with air at 200 ºC for 12 h and re-oxidized with HNO3 for 12 h showed the highest percentage of humic acids (85.3%).

Processing of spent NiW/Al2O3 catalysts

Spent oxidized (500 ºC, 5 h) commercial NiW/Al2O3 catalysts were processed using two different routes: a) fusion with NaOH (650 ºC, 1 h), the roasted mass was leached in water; b) leaching with HCl or H2SO4 (70 ºC, 1-3 h). HCl was the best leachant. In both routes, soluble tungsten was extracted at pH 1 with Alamine 336 (10 vol.% in kerosene) and stripped with 2 mol L-1 NH4OH (25 ºC, one stage, aqueous/organic ratio = 1 v/v). Tungsten was isolated as ammonium paratungstate at very high yield (> 97.5%). The elements were better separated using the acidic route.

Caracterização potenciométrica de substâncias húmicas extraídas de solos da Antártica Marítima

Monitoring of soil carbon storage may indicate possible effects of climate change on the terrestrial environment and it is therefore necessary to understand the influence of redox potential and chemical characteristics of humic substances (HS) of Antarctic soil. Five soils from King George Island were used. HS were extracted, quantified and characterized by potentiometry and the content of total carbon and nitrogen determined. HS of these soils had greater aliphatic character, low content of phenolic groups, lower acidity and lower formal standard electrode potential, compared to HS of soils from other regions, suggesting they are more likely to be oxidized.

ASYMMETRIC SULFOXIDATION OF ALBENDAZOLE TO RICOBENDAZOLE BY FUNGI: EFFECT OF pH

Albendazole (ABZ) is an anthelmintic drug used for the treatment of infectious diseases in veterinary and human medicine. This drug is a prochiral drug that after administration, is rapidly oxidized in the pharmacologically active sulfoxide metabolite, which is also known as ricobendazole (ABZSOX). ABZSOX has a stereogenic center and possibly two enantiomers, (+)-ABZSOX and (-)-ABZSOX. In the present work, we investigate the pH effect on the asymmetric stereoselective sulfoxidation of ABZ into ABZSOX by employing the fungi Nigrospora sphaerica, Papulaspora immera Hotson, and Mucor rouxii. The results show a possibility of obtaining the pure enantiomers of the ricobendazole drug using fungi as biocatalytic agents. The three fungi showed a high degree of enantioselectivity expressed by enantiomeric excess. In addition, M. rouxii can be used as an alternative to obtain the (+)-ABZSOX enantiomer (ee 89.8%).

COMPREENSÃO MATEMÁTICA DA DIFUSÃO NO CONTEXTO ELETROQUÍMICO

The aim of this study was to explain in detail the mathematical methods used to deal with diffusion equations, mainly for students and researchers interested in electrochemistry and related areas. Emphasis was placed on the deduction and resolution of diffusion equations, as well as addressing cartesian, spherical and cylindrical coordinates. Different aspects of mass transfer processes were discussed including the importance of the resolution of Fick's laws equations to understand and derive parameters of the electroactive species (e.g., diffusion coefficients, formal electrode potentials) from the electrochemical techniques. As an example, the resolution of diffusion equations for a reversible reduction process of soluble oxidized species was presented for the chronopotentiometry technique. This study is envisaged to broaden the understanding of these frequently used methods, in which mathematical deductions are not always completely understood.

Effect of alcohol concentration and electrode composition on the ethanol electrochemical oxidation

The electrochemical oxidation on platinum and platinum rhodium bimetallic electrodes was studied by Differential Electrochemical Mass Spectrometry for several ethanol concentrations in solution. It is found that increasing the ethanol concentration the production of the partially oxidized products (acetaldehyde) increases as the concentration increases. On the other hand, addition of 25% at. of rhodium increases the full oxidation to CO2. Another interesting result observed is a correlation between the intensity of the dehydrogenations peak at 0.3 V vs. RHE and the CO2 yield for the different ethanol concentration studied.

Flow injection spectrophotometric determination of adrenaline using a solid-phase reactor containing triiodide ions immobilized in an anion-exchange resin

A flow injection spectrophotometric procedure with on-line solid-phase reactor containing ion triiodide immobilized in an anion-exchange resin is proposed for the determination of adrenaline (epinephrine) in pharmaceutical products. Adrenaline is oxidized by triiodide ion immobilized in an anionic-exchange resin yielding adrenochrome which is transported by the carrier solution and detected at a wavelength of 488 nm. Adrenaline was determined in three pharmaceutical products in the 6.4 x 10-6 to 3.0 x 10-4 mol L-1 concentration range with a detection limit of 4.8 x 10-7 mol L-1. The recovery of this analyte in three samples ranged from 96.0 to 105 %. The analytical frequency was 80 determinations per hour and the RSDs were less than 1 % for adrenaline concentrations of 6.4 x 10-5 and 2.0 x 10-4 mol L-1 (n=10). A paired t-test showed that all results obtained for adrenaline in commercial formulations using the proposed flow injection procedure and a spectrophotometric batch procedure agree at the 95% confidence level.

Electrochemical evaluation of lipophilic antioxidants from Iryanthera juruensis fruits (Myristicaceae)

TLC autographic assays revealed in the hexane extract of Iryanthera juruensis (Myristicaceae) the presence of two compounds, with antioxidant properties towards beta-carotene. They were isolated and identified as 3-methyl-sargachromenol (1) and sargachromenol (2). Further investigation of the hexane extract led to isolations of 3-methyl-sargaquinoic acid (3) and sargaquinoic acid (4). The electrochemical behaviour of these compounds was studied in CH2Cl2/Bu4NBF4 at glassy carbon electrode. The phenolic group in both tocotrienols 1 and 2 are oxidized at +0.23V and +0.32V and their oxidation potentials are correlated with the observed antioxidant activities and oxidation mechanism of alpha-tocopherol. The reductive voltametric behaviour of quinone function in both plastoquinones 3 and 4 is discussed.