Utilização de microondas na avaliação da biomassa microbiana do solo

O presente trabalho teve por objetivo determinar o carbono e o nitrogênio presentes na biomassa microbiana, usando a irradiação do forno de microondas em substituição ao clorofórmio nos métodos fumigação-incubação e fumigação-extração. Foram utilizadas duas amostras de um Podzólico Vermelho-Escuro, submetidas aos procedimentos de incubação e de extração, após serem fumigadas com clorofórmio e irradiadas com microondas por diferentes períodos (2, 5, 10, 15, 20, 30, 40 e 50 min). Observou-se que a irradiação durante 2 min foi suficiente para estimar o C e o N presentes na biomassa microbiana nos procedimentos de incubação e extração, com valores semelhantes aos verificados pela fumigação com clorofórmio. A irradiação com microondas reduziu os coeficientes de variação nas amostras de solo submetidas ao procedimento de extração, comprovando ser o método irradiação-extração o mais adequado para a estimativa do C e do N microbianos.

Extração de micronutrientes em solo com solução de DTPA em forno de microondas com radiação focalizada

Neste trabalho, é proposto um procedimento alternativo para a extração de micronutrientes em amostras de solo para fins de avaliação da fertilidade. Amostras provenientes de programa colaborativo de análise de solos, com diferentes características físicas e químicas, foram submetidas à extração com ácido dietilenotriaminopentaacético (DTPA), empregando-se energia de microondas com radiação focalizada. Os resultados indicaram uma redução significativa no tempo requerido para extração de Cu, Mn e Zn. Os resultados apresentaram uma redução significativa no tempo de preparo das amostras: de 120 min, no procedimento convencional envolvendo agitação à temperatura ambiente, para 10 min, no procedimento assistido por microondas. Não foi possível estabelecer um procedimento único para a extração simultânea também de Fe, em virtude de sua maior liberação com essa forma de aquecimento. Entretanto, demonstrou-se que o aquecimento no forno de microondas tem potencial para utilização na extração de micronutrientes em análise de solo de rotina.

Decomposição de amostras de solos assistida por radiação microondas: estratégia para evitar a formação de fluoretos insolúveis

A decomposição de amostras que contêm elevados teores de Si, utilizando mistura com os ácidos nítrico e fluorídrico, pode provocar a precipitação de fluoretos de Al(III), Ca(II), Fe(III) e Mg(II) durante a digestão, impedindo a recuperação total desses elementos. Visando minimizar esse problema, foram testados quatro procedimentos aplicados a diferentes amostras de solos. O procedimento mais eficiente envolveu a decomposição assistida por radiação microondas, seguida pela separação do material sólido residual com elevado teor de Si do sobrenadante ácido. A fração residual foi solubilizada usando HF concentrado e, após complexação com ácido bórico, essa solução foi misturada à fase líquida do digerido. Os teores de metais nos digeridos foram determinados por espectrometria de emissão óptica em plasma induzido (ICP OES) e a exatidão foi demonstrada aplicando o procedimento proposto em amostras provenientes do programa colaborativo International Soil-Analytical Exchange (ISE, Wegening Agricultural University, Holanda) e em amostra certificada de solo proveniente do National Institute of Standard and Technology (NIST, SRM 2709), que apresentou respectivamente, os seguintes percentuais de recuperação: 100,0 ± 2,6; 99,5 ± 1,9; 108,5 ± 2,7; 94,6 ± 8,9; 92,2 ± 9,7; 95,7 ± 1,8; 96,7 ± 2,7; 95,2 ± 0,6; 103,6 ± 2,6 e 96,1 ± 1,6 para, Al, Ba, Ca, Cr, Cu, Fe, Mg, Mn, V e Zn.

AV37 - Diagrama funcional de un producto del ámbito industrial: el microondas

Aplicación práctica del método de análisis funcional de productos industriales. Análisis funcional para un microondas doméstico y alternativas de diseño derivadas

Adaptações em forno de microondas doméstico para utilização em laboratório

Domestic microwave oven was modified for laboratory applications. Electronic system was made for controlling magnetron irradiation time. Exhaustion and air circulation systems were installed to clean the internal oven atmosphere during operation. The cavity walls were coated with aluminized thermal paint to avoid chemical corrosion. These modifications allowed the usage of the oven for drying and processes using reflux.

Mecanização no preparo de amostras por microondas: o estado da arte

This review presents the latest advances of the mechanisation in sample preparation using microwave oven. The fundamental principles of microwaves field interaction with matter are presented, followed by the basic principles of microwave equipment construction. Hyphenation of microwave oven with flow injection analysis or robotic are discussed as well as some metodological difficulties and solutions by its implementation.

Uso de irradiação de microondas na determinação espectrofotométrica de cromo com EDTA

Cr(III) slowly forms a violet complex with EDTA at pH 2.5-5.0 under normal conditions. The complex formation can be accelerated by irradiating the reacting mixture with microwave energy. The complex Cr(III)-EDTA is completely formed within 3 minutes of microwave irradiation and followed by a simple and rapid method for spectrophotometric determination of chromium. The method may be successfully applied to determination of chromium in catalyst.

Uma demonstração simples e visual do efeito do aquecimento com microondas em reações de poliadição

Polyaddition of commercial monomers is easily performed on a domestic microwave oven. The rate of polymerization depends on the structure of the monomer, power and time of irradiation. This methodology can easily be used to demonstrate the acceleration of organic reactions promoted by microwaves.

Aquecimento em forno de microondas / desenvolvimento de alguns conceitos fundamentais

The microwave oven became a common domestic equipment, due mainly to the short time spent to heat foods. One of the most interesting characteristics of the microwave oven is the selective heating. Different from the conventional oven, where the heating is not selective, the heating by microwave depends on the chemical nature of the matter. Many Students of Chemistry have no knowledge of the principles involved in this selective heating, in spite of the daily microwave oven use. The heating by microwave is feasible for chemistry courses. In discussions about the microwave absorption by the matter it is possible to explore chemical properties like: heat capacity, chemical bound, molecular structure, dipole moments, polarization and dielectric constant. This paper presents the basic principles involved in the microwave heating. It is proposed a simple and inexpensive experiment that could be developed in general chemistry courses, to illustrate the relationship between heating and the chemical properties of some solvents. Experiments to check the power of the microwave oven are also proposed.

Microondas em síntese orgânica

The application of microwave heating to organic synthesis is presented in a concise manner. Issues such as the history of the microwave oven, dielectric heating, reactions techniques (dry reactions, MORE chemistry), domestic ovens, microwave reactors, microwave effect and control of selectivities are discussed. Selected examples from the literature showed faster reactions, improved yields, less thermal degradations and cleaner reactions.

Digestão fotoquímica, assistida por microondas, de águas naturais: aplicação em estudos de partição e especiação do cobre

The efficiency of a new procedure for the digestion of natural waters, based on a microwave-activated photochemical reactor was evaluated in this work. Fluorescence spectra showed a 99% reduction in the emission of a 40 mg L-1 humic acid solution after 15 min of UV irradiation. In the presence of H2O2, only 3 min were necessary to accomplish a reduction of almost 100% in the emission and 6 min to reduce the concentration of dissolved organic carbon by 95%. The copper recovery from synthetic samples containing commercial humic acid, from soil suspensions, as well as from natural waters varied between 91.5 and 106.6%. The digestion of dissolved and unfiltered samples was successfully accomplished in 6 and 12 min, respectively. No contaminations or sample losses were observed. Results of copper speciation in natural waters showed that this metal is predominantly bound to natural ligands. Only 3-6% of the total recoverable copper is present in the labile form.

Experimentos didáticos envolvendo radiação microondas

Theoretical and practical aspects of the use of microwave-assisted strategies in chemistry are introduced for students using simple and safe experiments employing a domestic oven. Three procedures are proposed for evaluating the distribution of microwave radiation inside the microwave oven cavity: (1) variation of the volume of marshmallows; (2) drying of filter paper wetted with Co(II) solution, and (3) variation of water temperature, after microwave-assisted heating. These experiments establish the position with the highest incidence of microwave radiation in the oven cavity, which was chosen for the synthesis of salicylic acid acetate. This synthesis was performed in 5 min of heating and the yield was around 85%. All experiments can be carried out in a 4 h lab-session using low-cost instrumentation.

O uso do forno de microondas na síntese orgânica em fase sólida

Solid-phase organic synthesis (SPOS) has been considered the main strategy for the construction of combinatorial libraries, because its simplicity leads to faster synthetic procedures. In addition to that, a series of reports in the specialized literature show great advantages in the use of microwave activation, when compared to classical heating, for instance: shorter reaction times, in some cases from several hours to a few minutes, increase of selectivity and product yields, energy economy and reduction and/or elimination of solvent. This review describes the use of microwave ovens/reactors in solid phase organic synthesis, describing the advantages, equipment and reactions using both techniques.

Decomposição de argilas em forno de microondas e determinação simultânea dos seus constituintes principais por espectrometria de emissão óptica em plasma indutivamente acoplado

In this work a closed-vessel microwave-assisted acid decomposition procedure for clays was developed. Aluminum, Ca, Fe, K, Mg, Na, Si, and Ti were determined in clay digestates by inductively coupled plasma optical emission spectrometry. The most critical parameter for total decomposition of clays was the composition of the reagent mixture. The applied power and the heating time exerted a less critical influence. Best decomposition conditions were attained using a reagent mixture containing 4 mL aqua regia plus 3 mL HF and the heating program was implemented in 12 min. The accuracy of the results was demonstrated using two standard reference materials and a paired t-test showed a good agreement between determined and certified values at a 95% confidence level.

Planejamento fatorial aplicado à digestão de amostras de feijão assistida por radiação microondas

The use of factorial design was evaluated for optimization of focused-microwave-assisted digestion of bean samples. Calcium, Fe, Mg, Mn and Zn percentual recoveries were determined in digestates after focused-microwave-assisted digestion according to factorial design procedures. A cavity microwave digestion was carried out to certify the elemental compositions obtained. The accuracy was checked using a standard reference material, the NIST SRM 8433 - Corn Bran. Results are in agreement with certified values at the 95% confidence limit when the Student t-test was used. Volumes of nitric and sulfuric acid, temperature, and the interplay between HNO3 and H2SO4 initial volumes were significant variables according to P-values in the analysis of variance (ANOVA).