Metodologia analítica para a determinação de sulfato em vinhoto

In this way it is very important to know the sulfate concentration in vinasse samples before to make the biodigestor design. A previous developed and indirect method (Anal. Chim. Acta. 1996, 329, 197), was used to determine sulfate in samples of vinasse, after previous treatments, done in order to eliminate organic matter with hydrogen peroxide 30% and concentrated nitric acid mixture (3:1), under heating. Interferent cationic ions were isolated by using ion exchange columns. The results obtained for some samples from Araraquara and Penápolis are here presented. The phosphate concentration was also determined.

Estudo comparativo da seletividade de um método cinético-catalítico: a determinação de Cr(VI) pela oxidação da o-dianisidina pelo peróxido de hidrogênio

Selectivity studies for the determination of Cr(VI) using the catalytic oxidation of the o-dianisidine by hydrogen peroxide showed two distincts situations. In the first, when interferents were studied by a univariate procedure, Cr(III) and Cu(II) cause serious interferences even at the 2:1 proportion, relative to Cr(VI), while Fe(III) interfered at the 15:1 ratio and EDTA at the 10:1 ratio. On the other hand, when a multivariate investigation was performed, Cr(III) did not present any significant principal effects and its significant interaction effects were negative, in contrast to EDTA, that presented positive interaction effects although, like Cr(III), did not show significant interaction effects. In view of the interferent's action it become necessary to separate Cr(VI) by extraction with methylisobutylketone in a chloridric acid medium before its determination in vegetals and in wastewater from a cellulose industry samples. Using this procedure, the method precision is ±0,5% at the 10 ng/mL Cr(VI) concentration level. The detection and quantification limits, calculated by means of absorbance measurements of ten replicates of blank reagents were 1,1 and 3,2 ng/mL, respectively. The results obtained with real samples showed a relative standard deviation between 1,2% and 3,0% relative to their reference values.

Utilização de endoperóxidos de derivados de naftaleno como fontes químicas de oxigênio singlete em sistemas biológicos

Molecular oxygen, in the first excited state (singlet oxygen, ¹O2), has a substantial reactivity towards electron-rich organic molecules, such as biological targets, including unsaturated fatty acids, proteins, RNA and DNA. Considering the complexity of biological systems and the great variety of reactive species generated by photochemistry, efforts have been devoted to develop suitable ¹O2 generators based on the thermolysis of water soluble naphthalene endoperoxides. These compounds are chemically inert and have been employed as versatile sources of ¹O2. The synthesis is based on structural modifications in position 1,4 of dimethylnaphtalene, grafting hydrophilic substituents. The correspondent endoperoxide can be generated using photochemical method, or molybdate-catalyzed disproportionation of hydrogen peroxide.

Sistema antioxidante envolvendo o ciclo metabólico da glutationa associado a métodos eletroanalíticos na avaliação do estresse oxidativo

The most relevant advances on the analytical applications of glutathione determination based on glutathione redox cycle and the antioxidant system are given. The main enzymes that participate of the glutathione metabolism are the glutathione peroxidase and glutathione reductase. The glutathione peroxidase has a major role in the removal of hydrogen peroxide and lipid peroxides from the cells. These enzymes, operating in tandem with catalase and superoxide dismutase promote a scavenging of oxyradical products in tissues minimizing damages caused by these species. Reduced glutathione is the major intracellular thiol found in mammals and changes in the glutathione concentration in biological fluids or tissues may provide a useful marker in certain disorders like hemolytic anemia, myocardial oxidative stress and in the investigation of some kinds of cancers. Particular attention is devoted to the main advantages supplied by biosensors in which there is an incorporation of bioactive materials for the glutathione determination. The correlation between stability and sensitivity of some reduced glutathione electrochemical sensors is discussed.

Uso analítico de tecidos e de extratos brutos vegetais como fonte enzimática

This article describes the current status of several analytical methodologies using vegetal tissue and crude extracts as enzymatic source. In this divulgation paper the obtention of vegetal crude extract and/or tissue and selected enzymatic procedures are presented emphasizing its characteristics and peculiarities. Examples of many biosensors and/or flow injection procedures using vegetal tissues or crude extracts for the determination of many analytes, such as amines, ascorbic acid, ethanol, glutamate, hydrogen peroxide, oxalic acid, pectins, phenolic compounds and urea of biologic, environmental, food, pharmaceutical and industrial interests are also given and discussed.

Desenvolvimento de um dispositivo de baixo custo para medidas por quimiluminescência

A simple and low cost device (ca. US$ 150) that comprises two photodiodes fixed in lab-made Perspex flow cell is proposed for chemiluminescence measurements. The characteristics of the device (large observation window and reduced thickness) allow maximizing the amount of the emitted radiation detected. A sensitivity improvement of ca. 50 % was observed by employing two photodiodes for signal measurements. The performance of the device was assessed by the oxidation of luminol by hydrogen peroxide, yielding a linear response within the range of 2.50 to 500 µmol L-1 H2O2. The detection limit was estimated as 0.8 µmol L-1 hydrogen peroxide which is comparable with those obtained by using equipments based on photomultipliers.

Peróxido de hidrogênio: importância e determinação

A brief discussion about the hydrogen peroxide importance and its determination is presented. It was emphasized some consideration of the H2O2 as reagent (separated or combined), uses and methods of analysis (techniques, detection limits, linear response intervals, sensor specifications). Moreover, it was presented several applications, such as in environmental, pharmaceutical, medicine and food samples.

Efeitos da beta-polinitração na eficiência catalítica de rutenioporfirinas em reações de oxidação de cicloexano

Rutheniumporphyrins, especially with several nitro groups in b-positions, were used in the cyclohexane oxidation in the presence of iodosylbenzene, hydrogen peroxide and sodium hypochlorite as oxygen donors, under mild conditions. The beta-polynitrated complexes were able to promote the catalytic cyclohexane oxidation. They show an exceptionally high catalytic efficiency and resistance to attack by strong oxidizing agents. The cyclohexane oxidation was monitored by gas chromatography and the results showed that the beta-polynitrated rutheniumporphyrins are better catalysts when compared to other complexes not beta-polynitrated. In all cases, the 2-phenylsubstituted complexes were more efficient than 4-phenylsubstituted complexes. The importance of the ortho effect to oxidation was shown.

Um experimento de análise em fluxo envolvendo reações enzimáticas e quimiluminescência

An experiment is proposed to introduce some fundamentals of flow analysis, chemiluminescence and kinetic monitoring of enzymatic reactions in undergraduate courses. Chemiluminescence detection is performed with a simple spectrophotometer equipped with a lab-made spiral flow cell constructed from a polyethylene tube. The hydrogen peroxide produced by the glucose oxidation in the presence of glucose oxidase is continuously monitored by the reaction with luminol in alkaline media in a flow injection system. The exercise allows also the discussion of important analytical features and the comparison with different optical methods of analysis.

Degradação de corantes reativos pelo sistema ferro metálico/peróxido de hidrogênio

In this work the degradation of aqueous solutions of reactive azo-dyes is reported using a combined reductive/advanced oxidative process based in the H2O2/zero-valent iron system. At optimized experimental conditions (pH 7, H2O2 100 mg L-1, iron 7 g L-1) and using a continuous system containing commercial iron wool, the process afforded almost total discolorization of aqueous solutions of three reactive azo-dyes (reactive orange 16, reactive black 5 and brilliant yellow 3G-P) at a hydraulic retention time of 2.5 min. At these conditions the hydrogen peroxide is almost totally consumed while the released total soluble iron reaches a concentration compatible with the current Brazilian legislation (15 mg L-1).

Emprego de compostos organometálicos mononucleares de paládio(II) na ativação de macrófagos peritoneais de camundongos

The immune responses are mediated by a variety of cells that, when activated, produce a number of molecules. Macrophages are the first cells to take part in the immune response releasing many compounds in the extracellular environment such as H2O2. Taking into account this aspect we evaluated the activation of an immunological system, in vitro, by determining the H2O2 released in cultures of peritoneal macrophage cells from Swiss mice in the presence of organopalladated compounds of the type [Pd(dmba)(X)(dppp)], dmba = N,N-dimethylbenzylamine, dppp = 1,3-bis(diphenylphosphine)propane, X = Cl, N3, NCO, NCS. An excellent activation of macrophages by the [Pd(dmba)(X)(dppp)] compounds was observed and the influence of the X ligand on the immune response could be verified.

Remoção de cor em soluções de corantes reativos por oxidação com H2O2/UV

This paper summarizes the result of a degradation test of two azo-reactive dyes (Reactive Blue 214, Reactive Red 243) under UV irradiation in the presence of H2O2. Five different doses of hydrogen peroxide (0 mM, 5 mM, 10 mM, 20 mM and 30 mM) at constant initial concentration of the substrate (100 mg/L) were used. The radiation source were three 15 W-lamps. Complete destruction of the color of the solutions was attained in 40-50 min of irradiation. UV/H2O2 proved capable of complete discoloration and degradation of the above azo reactive dyes.

Decoloración de alginato de sodio extraído de las algas pardas marinas del género Sargassum con el uso de peróxido de hidrógeno

Hydrogen peroxide bleaching of sodium alginate from seaweeds oh the Sargassum genus was studied. The influence of H2O2 concentration (percentage of H2O2 on a dry weight alginate basis, w/w) and NaOH/H2O2 ratio (% NaOH/% H2O2, both referred to a dry weight alginate basis, w/w) on the molecular weight, color removal and content of Fe3+ ions of bleached alginate samples was investigated by UV and IR spectroscopies, colorimetric determination of Fe3+ ions and vapor pressure osmometry. Higher yield, purity and molecular weight of alginate were obtained using 3% (or less) of hydrogen peroxide and a NaOH/H2O2 ratio of 1.2 for bleaching.

Recuperação de cobalto e de lítio de baterias íon-lítio usadas

The "active mass" (cathode + anode + electrolyte) of spent Li-ion batteries was submitted to one of the following procedures: (a) it was calcined (500 ºC) and submitted to extraction with water to recover lithium salts. The residual solid was treated with sulfuric acid containing hydrogen peroxide. Cobalt was recovered as sulfate; (b) the "active mass" was treated with potassium hydrogen sulfate (500 ºC) and dissolved in water. Cobalt was precipitated together with copper after addition of sodium hydroxide. Lithium was partially recovered as lithium fluoride. Co-processing of other battery components (aluminum and copper foils) affected negatively the behavior of the recovery procedures. Previous segregation of battery components is essential for an efficient and economical processing of the "active mass".

Extraction, purification and biochemical characterization of a peroxidase from Copaifera langsdorffii leaves

The aim of this work is to obtain, purify and characterize biochemically a peroxidase from Copaifera langsdorffii leaves (COP). COP was obtained by acetone precipitation followed by ion-exchange chromatography. Purification yielded 3.5% of peroxidase with the purification factor of 46.86. The COP optimum pH is 6.0 and the temperature is 35 ºC. COP was stable in the pH range of 4.5 to 9.3 and at temperatures below 50.0 ºC. The apparent Michaelis-Menten constants (Km) for guaiacol and H2O2 were 0.04 mM and 0.39 mM respectively. Enzyme turnover was 0.075 s-1 for guaiacol and 0.28 s-1 for hydrogen peroxide. Copaifera langsdorffii leaves showed to be a rich source of active peroxidase (COP) during the whole year. COP could replace HRP, the most used peroxidase, in analytical determinations and treatment of industrial effluents at low cost.