Análise do teor e da qualidade dos lipídeos presentes em sementes de oleaginosas por rmn de baixo campo

To choose among the variety of oleaginous plants for biodiesel production, the oil content of several matrices was determined through different low-field ¹H nuclear magnetic resonance (NMR) experiments with varied pulse sequences, namely single-pulse, spin-echo, CPMG, and CWFP. The experiments that involved the first three sequences showed high correlation with each other and with the solvent extraction method. The quality of the vegetable oils was also evaluated on the basis of the existing correlation between the T2 values of the oils and their properties, such as viscosity, iodine index, and cetane index. These analyses were performed using HCA and PCA chemometric tools. The results were sufficiently significant to allow separation of the oleaginous matrices according to their quality. Thus, the low-field ¹H NMR technique was confirmed as an important tool to aid in the selection of oleaginous matrices for biodiesel production.

Preparação e caracterização do complexo de inclusão do óleo essencial de Croton zehntneri com β-ciclodextrina

Croton zehntneri, a plant native to northeastern Brazil, is widely used in folk medicine to treat gastrointestinal problems and has rich essential oil content. The essential oil of C. Zehntneri was analyzed by GC-MS, and its inclusion complex with β-cyclodextrin (β-CD) was characterized by both vibrational spectroscopy and differential scanning calorimetry (DSC). Estragol was the major component identified in the essential oil by the study. IR spectra indicated an interaction of β-CD with essential oil from C. zehntneri, a finding corroborated by the stability constant and scanning calorimetry. Microencapsulation within β-CD has the potential to mask sensory attributes and increase aqueous solubility of oils, thereby improving their applicability as drugs.

Estudo da cinética de oxidação de biodiesel b100 obtido de óleo de soja e gordura de porco: determinação da energia de ativação

The quality of biodiesel is extremely important for its commercialization and use; oxidation of biodiesel is a critical factor because it decreases the fuel storage time. A commercial biodiesel was mixed with synthetic antioxidants, according to a simplex-centroid experimental mixture design, and its stability was evaluated through induction period and activation energy. In all trials, addition of antioxidants increased activation energy in the mixtures containing tertiary butylhydroquinone (TBHQ). When a mixture containing 50% TBHQ and 50% butylated hydroxyanisole was used, synergistic effect was observed, and the major activation energy obtained was 104.43 kJ mol-1.

Avaliação de diferentes métodos para a determinação de cobre em óleo mineral isolante por espectrometria de absorção atômica com forno de grafite

This aim of this work was to compare two methods for copper determination in insulating oils from power transformers by GFAAS. The first method was extraction induced by emulsion breaking, which determined the preconcentration of copper in an aqueous solution and exhibited a limit of quantification of 0.27 µg L-1. Also, a second method based on the direct introduction of samples into GFAAS in the form of detergent emulsions, prepared with Triton X-114 and HNO3, was investigated. In this case, the limit of quantification was 1.7 µg L-1. Seven samples of used oils were successfully analyzed by both methods.

Caracterização físico-química do óleo essencial da Siparuna guianensis Aublet

Thermal and spectroscopic analyses of essential oil extracted from Siparuna guianensis Aublet, an aromatic plant belonging to medicinal ethnobotany family Siparunaceae, were carried out. The plant is known throughout the North and Northeast of Brazil by the name negramina and has wide application as a natural insect repellent. Thermogravimetric analyses were correlated with the Arrhenius Equation to provide kinetic parameters of evaporation, including activation energy and frequency factor. Differential scanning calorimetric analysis showed the presence of an exothermic oxidation peak, probably as a result of transformations and decomposition of the solid structure before melting.

Cristalização convencional de zeólitas e induzida por sementes

Seed-assisted synthesis of zeolites diminishes crystallization time and enables the industrial use of certain zeolites, which was conventionally unfeasible due to the complexity of synthesis and the cost of organic structure-directing agents. This study reports the primary results of zeolite crystallization in the presence of seeds, which are used as a substitute for organic compounds.

CARACTERIZAÇÃO E ATIVIDADE CATALÍTICA DE K2CO3/AL2O3 NA TRANSESTERIFICAÇÃO DO ÓLEO DE GIRASSOL COM AQUECIMENTO CONVENCIONAL E MICRO-ONDAS

Commercial and synthetic mesoporous aluminas impregnated with potassium carbonate were characterized by X-ray diffraction (XRD), nitrogen physisorption, infrared spectroscopy and 27Al MAS NMR. The activities in the transesterification reaction of sunflower oil with methanol for biodiesel production were evaluated. 27Al MAS NMR spectra evidenced the presence of AlIV and AlVI in the samples, and also of AlV sites in the mesoporous synthesized alumina, which disappeared after impregnation with potassium salt followed by calcination. All aluminas containing potassium were active for biodiesel production from sunflower seed oil, with high conversions by both conventional heating and microwave irradiation.

COMPOSIÇÃO QUÍMICA E TEMPERATURA DE CRISTALIZAÇÃO DE ÉSTERES OBTIDOS DE QUATRO ÓLEOS VEGETAIS EXTRAÍDOS DE SEMENTES DE PLANTAS DO CERRADO

The seed oils from four plants (Scheelea phalerata, Butia capitata, Syagrus romanzoffiana, Terminalia cattapa) found in Mato Grosso do Sul were extracted at good yields. Alkaline transesterification of these seed oils to esters using methanol and ethanol was studied and also produced good yields. Oleic acid (30.5/32.3%), lauric acid (30.7/32.9%) methyl and ethyl esters, were the main components of transesterification of the oils from Scheelea phalerata and Syagrus romanzoffiana. Lauric acid (42.2%), capric acid (15.9%) and caprylic acid (14.6%) methyl and ethyl esters were the main ester components of transesterification of the oil from Butia capitata. Oleic acid (37.8%), palmitic acid (33.5%) and linoleic acid (22.6%) methyl and ethyl esters were the main components of transesterification of oil from Terminalia catappa. Based on differential scanning calorimetry (DSC) studies, the first crystallization peak temperature of esters was observed. Esters derived from oils of the family Arecaceae (Scheelea phalerata, Butia capitata, Syagrus romanzoffiana) showed the lowest points of crystallization, despite having high levels of saturated fat. Esters of Terminalia cattapa oil, rich in unsaturated fat, showed the highest crystallization temperature. This difference in behavior is probably related to the high concentration of esters derived from lauric acid and palmitic acid.

AVALIAÇÃO DAS NORMAS DE ENSAIO APLICADAS NA QUANTIFICAÇÃO DE PCBs EM ÓLEO ISOLANTE

Polychlorinated biphenyls (PCBs) were widely used between 1940 and 1970 as an insulating fluid for transformers and capacitors. However, they are bioaccumulative and potentially carcinogenic and, according to the 2001 Stockholm Convention, must be eliminated by 2025. In Brazil, they have been gradually eliminated but contaminated equipment remains. The Brazilian official standard for PCBs content in oil analysis is the ABNT NBR 13882 and there is also the IEC 61619 International Standard, both based on GC-ECD quantification. This work identified the inefficiency of these analytical methods and highlights potential failures which generated discrepancies on quantification of these contaminants. It was observed that the IEC 61619 is superior to ABNT NBR 13882 in analytical criteria, but has problems with the inefficiency of the adsorbent material used in pretreatments for removal of oxidation products from oil where these adsorbents adsorbed some PCBs molecules, causing errors in quantification.

DESENVOLVIMENTO DE UMA TÉCNICA ULTRASSÔNICA PARA AVALIAR TEORES DE ÓLEO E GRAXA EM EFLUENTES DE BIOCOMBUSTÍVEIS

Ultrasound as a metrology tool has many applications in health care, industrial, and chemical analyses. Ultrasonic techniques are rapid, low-cost, non-invasive, and highly repeatable. Although ultrasound can be used to measure emulsions, no effort had been made thus far to optimize its sensitivity for metrological analysis. In this work, a technique for analyzing oil in water was validated. The wave velocity and attenuation were chosen as the ultrasonic parameters. The technique was implemented in the boundary region established by law for effluents from industrial plants involved with biofuel manufacturing. A technical effort of this study was to establish stable emulsions in concentrations close to the desired limit of study. The phase behaviours of pseudo-ternary oil, sodium chloride, and sodium lauryl sulphate were studied. The composition in the widest region of the diagram allowed for the formation of a stable emulsion, from which the ultrasound measurement was carried out. An analytical curve was obtained using ultrasonic attenuation to determine the content of oils and greases in wastewater ranging 15–240 ppm. The speed of sound did not appear to be an applicable parameter for this application. The technique was demonstrated to be an important alternative solution for the continuous monitoring of wastewater with regard to oil concentrations.

Efeito de bioprotetores em patógenos de sementes e na emergência e rendimento de grãos de milho

Um experimento de laboratório e dois de campo, conduzidos nas localidades de Passo Fundo, RS, e Pato Branco, PR, foram realizados com o objetivo de avaliar os efeitos da microbiolização de sementes sobre os patógenos de sementes e sobre a germinação e rendimento de grãos de milho (Zea mays). Em laboratório, a maioria dos bioprotetores reduziu significativamente o nível de patógenos de sementes. Nos experimentos de campo, no ano de 1997, em Passo Fundo, RS, somente Trichoderma harzianum (T-22) melhorou significativamente a emergência e o rendimento de grãos do milho . Todos os bioprotetores melhoraram significativamente a emergência em Pato Branco (PR). Paenibacillus macerans (144), T. harzianum (T-22), Flavimonas oryzihabitans e Pseudomonas putida biótipo B também proporcionaram aumento significativo no rendimento de grãos em relação à testemunha. O tratamento com T. harzianum proporcionou aumento significativo na emergência de plântulas e no rendimento de grãos de milho. Esse aumento foi de 615 kg/ha acima do rendimento da testemunha, sem tratamento.Em 1998, em Passo Fundo, P. macerans (144), F. oryzihabitans e Agrobacterium radiobacter proporcionaram os melhores aumentos na germinação. Com exceção de F. oryzihabitans e de Bacillus subtilis, todos os bioprotetores proporcionaram aumentos significativos no rendimento de grãos. Em Pato Branco, P. putida biótipo B 63, F. oryzihabitans e Pseudominas putida biótipo A (M 970841) proporcionaram as melhores germinações de sementes de milho. Paenibacilus macerans (144), T. harzianum (T-22), F. oryzihabitans, A. radiobacter e B. subtilis aumentaram significativamente o rendimento de grãos. A microbiolização de sementes apresenta-se como uma alternativa tec nológica para o tratamento de sementes de milho no Brasil.

Sobrevivência de Fusarium moniliforme em sementes de milho mantidas em duas condições de armazenamento

Dentre os fungos transportados pelas sementes de milho (Zea mays), Fusarium moniliforme se destaca pela freqüência e altas porcentagens com que ocorre, sendo considerado um dos principais responsáveis pelas podridões de sementes e reduções do estande. O presente trabalho teve como objetivo verificar o efeito do armazenamento de sementes de milho durante 12 meses, em câmara fria (14 °C e 40% UR) e ambiente não controlado (sem monitoramento da temperatura e umidade relativa), sobre a sobrevivência de F. moniliforme. Verificou-se que nas sementes conservadas em câmara fria, o tempo de armazenamento teve menor efeito sobre a sobrevivência do fungo, em comparação ao ambiente não controlado. Em alguns lotes, com incidências iniciais do fungo de 28, 34 e 59%, em condição ambiente, a sobrevivência foi bastante baixa, encontrando-se ao final de 12 meses, incidências de 2, 4 e 5%, respectivamente; em câmara fria, as incidências de F. moniliforme encontradas nos mesmos lotes foram 25, 30 e 58%. A análise de regressão indicou efeito linear do tempo de armazenamento sobre a sobrevivência do fungo, em todos os lotes avaliados, obtendo-se coeficientes de determinação acima de 0,90, quando as sementes foram mantidas em condição ambiente.

Controle da ferrugem da folha e da mancha bronzeada da folha de trigo pelo uso de fungicidas em tratamento de sementes

The control of leaf rust and tan spot of wheat by seed treatment with fungicides was evaluated during 1998 in Passo Fundo, RS. Except for treatments including triadimenol and iprodione, leaf rust and tan spot severity in above ground parts of wheat plants was drastically reduced by the fluquinconazole fungicide used.