TEORES DE ENXOFRE E ACEITABILIDADE DE AGUARDENTES DE CANA BRASILEIRAS

Considerando-se as indesejáveis características sensoriais dos compostos sulfurados e o papel negativo que podem representar na qualidade sensorial das aguardentes, foi realizado um estudo para verificar uma possível correlação entre os teores de enxofre presentes em amostras de aguardentes de cana e sua qualidade sensorial. Nesse sentido foram determinados os teores de enxofre de sete amostras de aguardentes de cana, sendo quatro adquiridas no comércio local, e três obtidas em laboratório, utilizando-se alambiques de cobre, de aço inoxidável e de alumínio. As amostras foram então submetidas a testes de aceitabilidade quanto ao aroma, sabor e impressão global, realizados por uma equipe de 30 provadores, em cabines individuais, utilizando-se escala hedônica de nove centímetros. Os resultados assim obtidos após serem submetidos à análise de variância, ao teste de médias de Tukey e à análise de regressão, revelaram haver correlação negativa significativa (p£ 0,05) entre os teores de enxofre e a aceitabilidade das amostras de aguardentes, em relação a todas as características avaliadas, ressaltando o papel negativo representado pelos compostos sulfurados presentes nas aguardentes de cana e indicando ser o método de Ni Raney uma possível opção a ser adotada no controle de qualidade das aguardentes de cana.

Cytotoxic and mutagenic evaluation of extracts from plant species of the Miconia genus and their influence on doxorubicin-induced mutagenicity: An in vitro analysis

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

In vivo assessment of DNA damage and protective effects of extracts from Miconia species using the comet assay and micronucleus test

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

A new approach to the granulation of beta-cyclodextrin inclusion complexes

Cyclodextrins (CDs) are annular oligosaccharides containing 6-12 glucose unities joined together by alpha-1,4 bonds. They have a conical-truncated shape with a lipophilic cavity in which different molecules can be included resulting in a stable inclusion complex. The cyclodextrins have been widely applied in pharmaceutical technology with the objective of increasing the solubility, stability and bioavailability of drugs in different pharmaceutical dosage forms, such as tablets. In order to obtain beta-CD tablets, liquid dispersions of drug/beta-CD are usually submitted to different drying processes, like spray-drying, freeze-drying or slow evaporation, being this dry material added to a number of excipients. However, such drying processes can generate particulate materials showing problems of flow and compressibility, needing their conversion into granulates by means of wetting with granulation liquid followed by additional drying. In this work, the main objective was to evaluate the preparation of tablets without the need of this additional drying step. For this purpose an aqueous dispersion containing acetaminophen/beta-CD complex and cornstarch was dried using a spouted bed and the obtained granules were compressed in tablets. Acetaminophen was used as model drug due to its low water solubility and the inexpensive and widely available cornstarch was chosen as excipient. Acetaminophen powder was added into a beta-cyclodextrin solution prepared in distilled water at 70 degrees C. Stirring was kept until this dispersion cooled to room temperature. Then cornstarch was added and the resulting dispersion was dried in spouted bed equipment. This material was compressed into tablets using an Erweka Korsh EKO tablet machine. This innovative approach allowed the tablets preparation process to be carried out with fewer steps and represents a technological reliable strategy to produce beta-cyclodextrin inclusion complexes tablets. (C) 2010 Elsevier By. All rights reserved.

Análise da aceitação de aguardentes de cana por testes afetivos e mapa de preferência interno

A aceitação de 11 amostras de aguardentes de cana envelhecidas e não envelhecidas foi avaliada por testes sensoriais afetivos e análises estatísticas uni e multivariada. As aguardentes estudadas compreenderam seis amostras comerciais de diferentes marcas, (sendo três não envelhecidas e três envelhecidas) e ainda outras cinco amostras correspondentes a zero, 12, 24, 36 e 48 meses de envelhecimento em um tonel de carvalho de 200L. As amostras foram avaliadas por 100 provadores consumidores do produto, recrutados por questionário de avaliação quanto à afetividade. Para os testes afetivos foi utilizada escala hedônica não estruturada de 9cm, sendo os dados obtidos avaliados por dois métodos estatísticos distintos: o Mapa de Preferência Interno (MDPREF) e a análise de variância univariada (ANOVA) com comparação de médias pelo teste de Tukey e análise de correlação. As amostras de aguardente envelhecidas por 12, 36 e 48 meses obtiveram maior aceitação, com médias ao redor de 7,0 na escala hedônica. A amostra com menor aceitação foi a correspondente ao tempo zero de envelhecimento (controle). As demais amostras obtiveram aceitação intermediária. A análise por MDPREF gerou em espaço multidimensional (onde as variações com relação aos dados de preferência foram extraídas em eixos ortogonais e para cada dimensão de preferência), coordenadas relativas aos produtos, que foram geradas em função da resposta dos consumidores. Os dados de aceitação de cada provador foram utilizados para o desenvolvimento de vetores individuais de preferência, resultando na construção de um mapa mutidimensional das amostras, em função dos dados de aceitação. No presente estudo o MDPREF foi gerado pelas primeira e segunda dimensões de preferência, as quais explicaram em conjunto 89,83% das variações observadas entre as amostras com relação à aceitação. O MDPREF confirmou os resultados da ANOVA, indicando uma maior preferência dos provadores pelas amostras de aguardentes envelhecidas. Os resultados sugerem também que aguardentes envelhecidas por mais de 24 meses em tonel de carvalho de 200L são preferidas pelos consumidores, em detrimento das comerciais não envelhecidas e mesmo das comerciais envelhecidas, que podem ser adicionadas de aguardente não envelhecida (processo denominado corte) e também ter correção da cor, conforme permite a Legislação Brasileira. O conteúdo de polifenóis totais e a intensidade de cor também foram determinados, e ambos apresentaram correlação linear positiva significativa (p<=0,05) com o aumento do tempo de envelhecimento das amostras.

Contribuição ao estudo da interrelação flúor-manganês em ratos

Devido a numerosas discrepâncias nos resultados de estudos experimentais relativos à interação flúor-manganês, propusemo-nos a verificar se a adição de manganês 5 água fluoretada (1 ppm), em diferentes proporções fluor-manganês, levaria a uma diferente fixaçao do halogênio. Para tanto, 24 ratos Wistar, recém-desmamados, foram mantidos em dieta padrão de caseína a 27%, recebendo na sua água de consumo: 1) H2O destilada (controle); 2) 1,0 ppm de flúor: 3) 1,0 ppm de flúor + 0,5 ppm de manganês (F:Mn = 2,0); 4) 1,0 ppm de flúor +1,0 ppm de manganês (F: Mn = 1,0). Foram anotados o peso ganho e o consumo de alimento e água, durante os 60 dias de experimento, após o qual as patas traseiras, dos animais sacrificados, foram autoclavadas e desossadas, e os femures retirados. Posteriormente, foram estes submetidos à secagem, extração da gordura, pulverização e analise do flúor fixado. Também foram efetuadas analises da composição centesimal da ração e de flúor e manganês nesta e nas diferentes águas de consumo. Os resultados de percentagem do flúor ingerido fixado nos femures, foram analisados estatisticamente pelo teste não-paramétrico de Kruskal-Wallis (níveis de 1% e 5%) mostrando que, para as proporções consideradas, o flúor na taxa de 1 ppm, o manganês, quando administrado após o desmame, parece não afetar a fixaçao do flúor. Contudo, faz-se necessário dar continuidade aos estudos com novas proporções e taxas mais elevadas de flúor e manganês.

Effects of calcium gluconate and PMSF in the treatment of acute intoxication of chicken by TOCP

To examine the efficacy of calcium gluconate (two doses of Ca-Glu 5 mg/kg i.v.) to alleviate the injurious effects of organophosphorus induced delayed neuropathy (OPIDN) in the presence or absence of phenylmethanesulfonyl fluoride (PMSF go mg/kg i.m.), 14 groups of four isabrown hens were used. To measure the lymphocyte neuropathy target esterase (LNTE)activity, groups receiving just distilled water (control), groups receiving just Tri-orto-cresyl phosphate (TOCP; 500 mg/kg p.o.) (Positive control), and other groups receiving TOCP and Ca-Glu or PMSF simultaneously or 12 hours later following intoxication by TOCP were used. They were sacrificed 12 and 24 hours after the administration of TOCP. To observe a 28-day time course of neurotoxicity scores and calcium plasma concentration, five groups were used. Regarding free Ca(2+)in the plasma, the positive control produced a characteristic profile time course up and down (luring 28 days, and some hens with maximum score of neurotoxicity in 28 days. The treatment, which prevented greater oscillation in free Ca(2+) in the plasma, presented a decrease in OPIDN in relation to the positive control. Twelve hours after the administration of TOCP, LNTE was 70-80% inhibited when compared with control, whereas the first decrease in the free Ca(2+) in the plasma was significantly different from the control only 24 hours after the administration of TOCP. In summary, the sooner the Ca-Glu is started, the less severe the neuropathy effects.

Reavaliação da eficiência de óleo de coco saponificado e de sua microemulsão como inibidores de corrosão em uma célula eletroquímica

An interesting development in surfactants science and technology is their application as corrosion inhibitors, since they act as protective films over anodic and cathodic surfaces. This work aims to investigate the efficiency of saponified coconut oil (SCO) as corrosion inhibitor and of microemulsified system (SCO + butanol + kerosene oil + distilled water), in saline medium, using an adapted instrumented cell, via techniques involving linear polarization resistance (LPR) and mass loss coupons (MLC). For this, curves of efficiency versus SCO concentration (ranging between 0 and 75 ppm) have been constructed. According to the obtained results, the following efficiency levels were reached with OCS: 98% at a 75 ppm concentration via the LPR method and 95% at 75 ppm via the MLC method. The microemulsified system, for a concentration of 15 ppm of SCO, obtained maximum inhibition of 97% (LPR) and 93% (MLC). These data indicate that it is possible to optimize the use of SCO in similar applications. Previous works have demonstrated that maximal efficiencies below 90% are attained, typically 65% as free molecules and 77% in microemulsified medium, via the LPR method in a different type of cell. Therefore, it can be concluded that the adapted instrumented cell (in those used methods) showed to be an important tool in this kind of study and the SCO was shown effective in the inhibition of the metal

Obtenção e aplicação de sistemas microemulsionados na recuperação avançada de petróleo

Due to the need of increasing production in reservoirs that are going through production decline, methods of advanced recovery have frequently been used in the last years, as the use of conventional methods has not been successful in solving the problem of oil drifting. In this work, the efficiency of different microemulsionated systems in the flow of oil from cores from Assu and Botucatu formations. Regarding drifting tests, cores were calcinated at a temperature of 1000°C, for 18 hours, with the aim of eliminating any organic compound present in it, increasing the resultant permeability. Following, the cores were isolated with resin, resulting in test specimens with the following dimensions: 3.8 cm of diameter and 8.7 cm of length. Cores were saturated with brine, composed of aqueous 2 wt % KCl, and oil from Guamaré treatment station (Petrobras/RN). A pressure of 20 psi was used in all tests. After core saturation, brine was injected again, followed by oil at constant flow rate. The system S3 - surfactant (anionic surfactant of short chain), isoamillic alcohol, pine oil, and water - presented the best drift efficiency, 81.18%, while the system S1E commercial surfactant, ethyl alcohol, pine oil, and distilled water presented low drift efficiency, 44,68%

Síntese, caracterização e aplicação do MCM-41 e A1-MCM-41 na pirólise do resíduo atmosférico de petróleo

In present work, mesoporous materials of the M41S family were synthesized, which were discovered in the early 90s by researchers from Mobil Oil Corporation, thus allowing new perspectives in the field of catalysis. One of the most important members of this family is the MCM-41, which has a hexagonal array of mesopores with pore diameters ranging from 2 to 10 nm and a high surface area, enabling it to become very promising for the use as a catalyst in the refining of oil in the catalytic cracking process, since the mesopores facilitate the access of large hydrocarbon molecules, thereby increasing the production of light products, that are in high demand in the market. The addition of aluminum in the structure of MCM-41 increases the acidity of the material, making it more beneficial for application in the petrochemical industry. The mesoporous materials MCM-41 and Al-MCM-41 (ratio Si / Al = 50) were synthesized through the hydrothermal method, starting with silica gel, NaOH and distilled water. CTMABr was used as template, for structural guiding. In Al-MCM-41 the same reactants were used, with the adding of pseudoboehmite (as a source of aluminum) in the synthesis gel. The syntheses were carried out over a period of four days with a daily adjustment of pH. The optimum conditions of calcination for the removal of the organic template (CTMABr) were discovered through TG / DTG and also through analysis by XRD, FTIR and Nitrogen Adsorption. It was found that both the method of hydrothermal synthesis and calcination conditions of the studies based on TG were promising for the production of mesoporous materials with a high degree of hexagonal array. The acidic properties of the materials were determined by desorption of n-butylamine via thermogravimetry. One proved that the addition of aluminum in the structure of MCM-41 promoted an increase in the acidity of the catalyst. To check the catalytic activity of these materials, a sample of Atmospheric Residue (RAT) that is derived from atmospheric distillation of oil from the Pole of Guamaré- RN was used. This sample was previously characterized by various techniques such as Thermogravimetry, FTIR and XRF, where through thermal analysis of a comparative study between the thermal degradation of the RAT, the RAT pyrolysis + MCM-41 and RAT + Al- MCM-41. It was found that the Al-MCM-41 was most satisfactory in the promotion of a catalytic effect on the pyrolysis of the RAT, as the cracking of heavy products in the waste occurred at temperatures lower than those observed for the pyrolysis with MCM-41, and thereby also decreasing the energy of activation for the process and increasing the rates of conversion of residue into lighter products

Hidrólise e caracterização de poliacrilamida hidrofobicamente modificada: avaliação da aplicabilidade na recuperação de petróleo

The hydrolysis reaction in alkaline conditions of the commercial polymer poly(acrylamide-co-metacrylate of 3,5,5-trimethyl-hexane) called HAPAM, containing 0.75 % of hydrophobic groups, was carried out in 0.1 M NaCl and 0.25M NaOH solutions, varying the temperature and reaction time. The polymers were characterized by 1H and 13C Nuclear Magnetic Resonance (NMR), Elemental Analysis and Size Exclusion Chromatography (SEC). The values of the hydrolysis degree were obtained by 13C NMR. The viscosity of HAPAM and HAPAM-10N-R solutions was evaluated as a function of shear rate, ionic strength and temperature. At high polymer concentration (Cp), the viscosity of HAPAM solutions increased with the ionic strength and decreased with the temperature. The viscosity of HAPAM-10N-R solutions increased significantly in distilled water, due to repulsions between the carboxylate groups. At high Cp, with the increase of ionic strength and temperature, occurred a decrease of viscosity, due to mainly the high hydrolysis degree and the low amount of hydrophobic groups. These results indicated that the studied polymers have properties more suitable for the application in Enhanced Oil Recovery (EOR) in low salinity and moderate temperature reservoirs

Estudo da digestão de sedimento de curtume visando a extração do cromo por microemulsão

Leather tanneries generate effluents with high content of heavy metals, especially chromium, which is used in the mineral tanning process. Microemulsions have been studied in the extraction of heavy metals from aqueous solutions. Considering the problems related with the sediment resulting from the tanning process, due to its high content in chromium, in this work this sediment was characterized and microemulsion systems were applied for chromium removal. The extraction process consists in the removal of heavy metal ions present in an aqueous feeding solution (acid digestion solution) by a microemulsion system. First three different solid sludge digestion methods were evaluated, being chosen the method with higher digestion capacity. For this digestion method, seeking its optimization, was evaluated the influence of granule size, temperature and digestion time. Experimental results showed that the method proposed by USEPA (Method A) was the most efficient one, being obtained 95.77% of sample digestion. Regarding to the evaluated parameters, the best results were achieved at 95°C, 14 Mesh granule size, and 60 minutes digestion time. For chromium removal, three microemulsion extraction methods were evaluated: Method 1, in a Winsor II region, using as aqueous phase the acid digestion solution; Method 2, in a Winsor IV region, being obtained by the addition of the acid digestion solution to a microemulsion phase, whose aqueous phase is distilled water, until the formation of Winsor II system; and Method 3, in a Winsor III region, consisting in the formation of a Winsor III region using as aqueous phase the acid digestion solution, diluted in NaOH 0.01N. Seeking to optimize the extraction process only Method 1 (Systems I, II, and VIII) and Method 2 (System IX) were evaluated, being chosen points inside the interest regions (studied domains) to study the influence of contact time and pH in the extraction percentiles. The studied systems present the following compositions: System I: Surfactant Saponified coconut oil, Cosurfactant 1-Butanol, Oil phase Kerosene, Aqueous phase 2% NaCl solution; System II: Aqueous phase Acid digestion solution with pH adjusted using KOH (pH 3.5); System VIII: Aqueous phase - Acid digestion solution (pH 0.06); and System IX Aqueous phase Distilled water (pH 10.24), the other phases of Systems II, VIII and IX are similar to System I. Method 2 showed to be the more efficient one regarding chromium extraction percentile (up to 96.59% - pH 3.5). Considering that with Method 2 the microemulsion region only appears in the Winsor II region, it was studied Method 3 (System X) for the evaluation and characterization of a triphasic system, seeking to compare with a biphases system. System X is composed by: Surfactant Saponified coconut oil, Cosurfactant 1-Butanol, Oil phase Kerosene, Aqueous phase Acid digestion solution diluted with water and with its pH adjusted using 0.01N NaOH solution. The biphasic and triphasic microemulsion systems were analyzed regarding its viscosity, extraction efficiency and drop effective diameter. The experimental results showed that for viscosity studies the obtained values were low for all studied systems, the diameter of the drop is smaller in the Winsor II region, with 15.5 nm, reaching 46.0 nm in Winsor III region, being this difference attributed to variations in system compositions and micelle geometry. In chromium extraction, these points showed similar results, being achieved 99.76% for Winsor II system and 99.62% for Winsor III system. Winsor III system showed to be more efficient due to the obtaining of a icroemulsion with smaller volume, with the possibility to recover the oil phase in excess, and the use of a smaller proportion of surfactant and cosurfactant (C/S)

Síntese, caracterizaçao e propriedades catalicas da peneira molecular nanoestruturada modificada com lantanio

The nanostructured molecular sieve SBA-15 was synthesized by the hydrothermal method, and modified with lanthanum with Si/La molar ratios of 25, 50, 75 and 100. The materials were evaluated as catalysts for the cracking of n-hexane model reaction. Type SBA- 15 and LaSBA-15 mesoporous materials were synthesized using tetraetilortosilicato as a source of silica, hydrochloric acid, heptahydrate lanthanum chloride and distilled water. Pluronic P123 triblock. polymer was used as structure template. The syntheses were carried out by 72 hours. The obtained SBA-15 samples were previously analyzed by thermogravimetry, in order to check the conditions of calcination for removal of organic template. Then, the calcined materials were characterized by X-ray diffraction, infrared spectroscopy, adsorption and desorption of nitrogen, scanning electron microscopy and X-ray microanalysis by dispersive energy. The acidity of the samples was determined using adsorption of n-bulinamina and desorption followed by thermogravimetry. It was found that the hydrothermal synthesis method was suitable for the synthesis of the SBA-15 mesoporous materials, with an excellent degree of hexagonal ordering. The reactions of catalytic cracking of n-hexane were carried out using a fixed bed continuous flow microreactor, coupled on-line to a gas chromatograph. From the catalytic evaluation, it was observed that the mesoporous materials containing lanthanum showed different results for the reaction of cracking of nhexane compared to the unmodified mesoporous material SBA-15. As a result of cracking was obtained as main products hydrocarbons in the range of C1 to C5. The catalyst that showed better properties in relation to the acidity and catalytic activity was LaSBA-15 with the ratio Si/La = 50

Influência da densidade de carga e da massa molar da poliacrilamida na reologia de sistemas microemulsionados

The knowledge of the rheological behavior of microemulsionated systems (SME) is of fundamental importance due to the diversity of industrial applications of these systems. This dissertation presents the rheological behavior of the microemulsionated system formed by RNX 95/alcohol isopropyl/p-toulen sodium sulfonate/kerosene/distilled water with the addition of polyacrylamide polymer. It was chosen three polymers of the polyacrylamide type, which differ in molar weight and charge density. It was studied the addition of these polymers in relatively small concentration 0,1% in mass and maximum concentration of 2,0%. It was made analysis of flow to determine the appearing viscosities of the SME and rheological parameters applying Bingham, Ostwald de Waale and Herschell-Buckley models. The behavior into saline environment of this system was studied for a solution of KCl 2,0%, replacing the distilled water. It was determined the behavior of microemulsions in relation with the temperature through curves of flow in temperatures of 25 to 60ºC in variations of 5ºC. After the analysis of the results the microemulsion without the addition of polymer presented a slight increase in its viscosity, but it does not mischaracterize it as a Newtonian fluid. However the additive systems when analyzed with low concentration of polymer adjusted well to the applied models, with a very close behavior of microemulsion. The higher concentration of the polymer gave the systems a behavior of plastic fluid. The results of the temperature variation point to an increase of viscosity in the systems that can be related to structural changes in the micelles formed in the own microemulsion without the addition of polymer

Avaliação das propriedades físico-químicas de sistemas a base de carboximetilcelulose e poli (N-isopropilacrilamida) em soluções aquosas para aplicação na indústria do petróleo

Sustainable development is a major challenge in the oil industry and has aroused growing interest in research to obtain materials from renewable sources. Carboxymethylcellulose (CMC) is a polysaccharide derived from cellulose and becomes attractive because it is water-soluble, renewable, biodegradable and inexpensive, as well as may be chemically modified to gain new properties. Among the derivatives of carboxymethylcellulose, systems have been developed to induce stimuli-responsive properties and extend the applicability of multiple-responsive materials. Although these new materials have been the subject of study, understanding of their physicochemical properties, such as viscosity, solubility and particle size as a function of pH and temperature, is still very limited. This study describes systems of physical blends and copolymers based on carboxymethylcellulose and poly (N-isopropylacrylamide) (PNIPAM), with different feed percentage compositions of the reaction (25CMC, 50CMC e 75CMC), in aqueous solution. The chemical structure of the polymers was investigated by infrared and CHN elementary analysis. The physical blends were analyzed by rheology and the copolymers by UV-visible spectroscopy, small-angle X-ray scattering (SAXS), dynamic light scattering (DLS) and zeta potential. CMC and copolymer were assessed as scale inhibitors of calcium carbonate (CaCO3) using dynamic tube blocking tests and chemical compatibility tests, as well as scanning electron microscopy (SEM). Thermothickening behavior was observed for the 50 % CMC_50 % PNIPAM and 25 % CMC_75 % PNIPAM physical blends in aqueous solution at concentrations of 6 and 2 g/L, respectively, depending on polymer concentration and composition. For the copolymers, the increase in temperature and amount of PNIPAM favored polymer-polymer interactions through hydrophobic groups, resulting in increased turbidity of polymer solutions. Particle size decreased with the rise in copolymer PNIPAM content as a function of pH (3-12), at 25 °C. Larger amounts of CMC result in a stronger effect of pH on particle size, indicating pH-responsive behavior. Thus, 25CMC was not affected by the change in pH, exhibiting similar behavior to PNIPAM. In addition, the presence of acidic or basic additives influenced particle size, which was smaller in the presence of the additives than in distilled water. The results of zeta potential also showed greater variation for polymers in distilled water than in the presence of acids and bases. The lower critical solution temperature (LCST) of PNIPAM determined by DLS corroborated the value obtained by UV-visible spectroscopy. SAXS data for PNIPAM and 50CMC indicated phase transition when the temperature increased from 32 to 34 °C. A reduction in or absence of electrostatic properties was observed as a function of increased PNIPAM in copolymer composition. Assessment of samples as scale inhibitors showed that CMC performed better than the copolymers. This was attributed to the higher charge density present in CMC. The SEM micrographs confirmed morphological changes in the CaCO3 crystals, demonstrating the scale inhibiting potential of these polymers