Biodiesel de soja: taxa de conversão em ésteres etílicos, caracterização físico-química e consumo em gerador de energia

Biodiesel was produced by the transesterification of neutral soybean oil and anhydrous ethanol using NaOH as catalyst. Combinations of biodiesel and diesel in the proportions of 0, 5, 10, 20, 40, 60, 80 and 100% were tested, respectively, as fuel in an energy generator. The average consumption and mixture performance were analysed. The tests showed a reduction in Diesel oil consumption when mixed with up to 20% of biodiesel. The quality characteristics of these fuels were analyzed.

Determinação de arsênio em águas contaminadas usando fluorescência de raios-X por energia dispersiva

This work proposes a simple, fast and inexpensive method to determine As in natural waters, using X-ray fluorescence. 50 µL of each sample containing 100 mg L-1 of yttrium as internal standard were deposited over a 2.5 µm thickness MylarTM film. The samples were dried at 50 °C for 2 h. X-ray spectra were obtained using an EDXRF apparatus. The accuracy was determined by analyte addition/recovery and by comparison with Hydride Generation Atomic Absorption Spectrometry (HG AAS). A recovery of about 100% was obtained and the results were in good agreement with HG AAS. The method showed a relative standard deviation of 6.8% and a detection limit of 10.5 µg L-1 of As.

Determinação de bromato em melhoradores de farinha por cromatografia de troca iônica com detecção espectrofotométrica

KBrO3 is registered by the FAO/OMS as a genotoxic and carcinogenic compound. In spite of this, KBrO3 is still employed by Brazilian bakeries. Nowadays ion exchange chromatography (IEC) is the most rapid and trustful method for BrO3- analysis. When at high concentrations, chloride ions can interfere in the BrO3- analysis, if the detection is performed by electrical conductivity. On the other hand, spectrophotometric detection, presented here is based on the absorption of BrO3- in the ultraviolet region (210 - 230 nm) where the absortion of chloride ions is very low, thus making possible the qualitative and quantitative analysis of BrO3- in flour improver samples.

Um equipamento de eletroforese capilar com detecção condutométrica construído em laboratório

A new construction of a capillary electrophoresis instrument with a universal conductivity detector (oscillometric detector) is described. The performance of the electrophoresis equipment was evaluated through the separation and detection of inorganic anions and cations in aqueous solutions. The results reproduced those found in the literature for the investigated probe ions, showing an efficient separation and good repeatability.

Oxidação de proteínas por oxigênio singlete: mecanismos de dano, estratégias para detecção e implicações biológicas

Proteins are potential targets for singlet molecular oxygen (¹O2) oxidation. Damages occur only at tryptophan, tyrosine, histidine, methionine, and cysteine residues at physiological pH, generating oxidized compounds such as hydroperoxides. Therefore, it is important to understand the mechanisms by which ¹O2, hydroperoxides and other oxidized products can trigger further damage. The improvement and development of new tools, such as clean sources of ¹O2 and isotopic labeling approaches in association with HPLC/mass spectrometry detection will allow one to elucidate mechanistic features involving ¹O2-mediated protein oxidation.

Desempenho físico-químico de metais e estruturas de concreto de redes de distribuição de energia: estudo de caso na região de Manaus

The influence of natural aging furthered by atmospheric corrosion of parts of electric transformers and materials, as well as of concrete poles and cross arms containing corrosion inhibitors was evaluated in Manaus. Results for painted materials, it could showed that loss of specular gloss was more intensive in aliphatic polyurethane points than in acrylic polyurethane ones. No corrosion was observed for metal and concrete samples until 400 days of natural aging. Corrosion in steel reinforcement was noticed in some poles, arising from manufacturing faults, such as low cement content, water/cement ratio, thin concrete cover thickness, etc. The performance of corrosion inhibitors was assessed by many techniques after natural and accelerated aging in a 3.5% saline aqueous solution. The results show the need for better chemical component selection and its concentration in the concrete mixture.

O emprego da termogravimetria para determinar a energia de ativação do processo de combustão de óleos combustíveis

Activation energy (Ea) is a parameter that can be applied to make predictions about the quality of oils to be used in an ICO engine. In this study, Ea was determined by thermogravimetry following two different procedures: ASTM E 1641 and Model-free kinetics. The energies were calculated in the low temperature oxidation (LTO) region for three Brazilian fuel oils (denominated A, B and C) and the results were equal using both methods: 43 kJ mol-1 (alpha=0.1 to 0.9) for oil A, 48 kJ mol-1 (alpha=0.1 to 0.5) and 65 kJ mol-1 (alpha=0.5 to 0.9) for oil B, and 58 kJ mol-1 (alpha=0.1 to 0.5) and 65 kJ mol-1 (alpha=0.5 to 0.9) for oil C. It was concluded that, among the oils studied, sample A was potentially the best option concerning the behavior in the LTO region.

Biossensor enzimático para detecção de fungicidas ditiocarbamatos: estudo cinético da enzima aldeído desidrogenase e otimização do biossensor

Initially, all major factors that affect the rate of the AldH-catalyzed reaction (enzyme concentration, substrate concentration, temperature and pH) were investigated. Optimal activity was observed between pH values of 7.5 and 9.5 in the temperature range of 25 to 50 ºC. Kinetic parameters, such as Km (2.92 µmol L-1) and Vmax (1.33 10-2 µmol min-1) demonstrate a strong enzyme-substrate affinity. The sensors were based on screen-printed electrodes modified with the Meldola Blue-Reinecke salt (MBRS) combination. Operational conditions (NAD+ and substrate contents, enzyme loading and response time) were optimized. Also, two enzyme immobilization procedures were tested: entrapment in poly(vinyl alcohol) bearing styrylpyridinium groups (PVA-SbQ) and crosslinking with glutaraldehyde. Chronoamperometry was employed to observe the biosensor responses during enzymatic hydrolysis of propionaldehyde and also to construct inhibition curves with maneb and zineb fungicides. Best results were found with the following conditions: [NAD+] = 0.25 mmol L-1; [propionaldehyde] = 80 µmol L-1; enzyme loading = 0.8 U per electrode; response time = 10 min, and inhibition time = 10 min. Current intensities around 103 ± 13 nA with the sensors and good stability was obtained for both immobilization procedures. Detection limits, calculated using 10% inhibition were 31.5 µg L-1 and 35 µg L-1 for maneb and zineb, respectively. Results obtained with other MBRS-modified electrodes consisting of mono and bi-enzymic sensors were compared. The ability to catalyze NADH oxidation by MB was also highlighted.

Desenvolvimento e validação de um método analítico para a determinação de histamina em vinhos utilizando cromatografia líquida de alta eficiência com detecção por fluorescência

A rapid and efficient method for the analysis of histamine in wines using HPLC with fluorescence detection after derivatization was developed and validated. The method LOD and LOQ values were 0.25 and 0.50 mg L-1 respectively. The repeatability and intermediary precision for the instrument and for the method presented RSD values of 3.7 and 2.9%, and 6.0 and 5.6%, respectively. The recoveries were 95.5 and 89.9% for the fortification levels of 2 and 10 mg L-1. The method was applied to determine the histamine content in Cabernet Sauvignon wines, which presented values between 1.2 and 5.7 mg L-1.

Análise arqueométrica de cerâmica Tupiguarani da região central do Estado do Rio Grande do Sul, Brasil, usando fluorescência de raios X por dispersão de energia (EDXRF)

Energy dispersive X-ray fluorescence methodology (EDXRF) was used to determine Al, Ba, Ca, Cr, Fe, K, Mn, Pb, Rb, S, Si, Sr, Ti, V, Zn in pottery sherds from seven archaeological sites in the central region of Rio Grande do Sul State, Brazil. The potteries' chemical fingerprints from Ijuí River, Ibicuí Mirim River, Vacacaí Mirim River and Jacuí River were identified. Interactions between sites from the Jacuí River, Vacacaí Mirim River and Ibicui Mirim River could have occurred because some samples from these sites are overlapping in a principal component analysis (PCA) graphic. The pottery provenance could be the same.

Mapeamento das interações proteína-ligante através de técnicas de RMN de ¹H utilizando detecção do ligante

NMR is a valuable screening tool for the binding of ligands to proteins providing structural information on both protein and ligands and is thus largely applied to drug-discovery. Among the recent NMR techniques to probe weak binding protein-ligand complexes we have critically evaluated the advantages and disadvantages of STD (Saturation Transfer Difference), WaterLOGSY (Water Ligand Observation with Gradient Spectroscopy), NOE pumping and DOSY-NOESY (Diffusion-Ordered NOESY) using a mixture of BSA (bovine serum albumin) plus salicylic acid, caffeine, citric acid, adipic acid and D-glucose.

Determinação da diferença entre o valor real e o teórico do triglicerídeo ECN 42 para a detecção de adulteração em azeites de oliva comercializados no Brasil

The difference between the actual ECN 42 triacylglyceride content in vegetable oils, obtained by HPLC analysis, and the theoretical value calculated from the fatty acid composition was applied to detect the addition of seed oils with high contents of linoleic acid to olive oils commercialized in Brazil. The results indicate that samples analyzed were probably adulterated with low commercial value seed oils, rich in linoleic acid, like soybean, sunflower or corn.

Dessorção iônica e degradação de filmes de polipirrol dopado com dodecilsulfato induzidas por elétrons de alta energia

Electron stimulated ion desorption (ESID) and degradation studies of polypyrrole doped with dodecylsulfate (PPy/DS) deposited on FTO were performed using time-of-flight mass spectrometry (TOF-MS) for ion analysis. The results suggest a strong contribution from fragments of the dodecylsulfate hydrocarbon chain to the mass spectra. In the 650-1500 eV energy range the ion yield curves show maxima at about 600, 1200 and 1400 eV, which can be related to carbon, nitrogen and oxygen-containing fragments, respectively, and interpreted in terms of the Auger Stimulated Ion Desorption (ASID) mechanism. Degradation studies indicate rapid loss of heavier hydrocarbons and an increase of bulk and substrate fragments. Some degradation profiles suggest formation of new species.

Nanocompósitos cerâmicos a partir do processo de moagem mecânica de alta energia

Pb/Ti, Sn and Mg-based nanocomposite materials were prepared by the high-energy mechanical milling of commercial powders. The surface of these ceramic compounds was strongly influenced by the doping, diameter of the milling spheres and time of the mechanical milling (amorphization process). Such milling leads to the formation of nanocrystalline materials. The mechanical processing parameters of these compounds were investigated through Brunauer, Emmett and Teller isotherms, wide angle X-ray diffraction, transmission electron microscopy and CO2 adsorption.

Detecção de contaminantes em espécie bioindicadora (Corbicula fluminea) - Rio Ribeira de Iguape - SP

The study assessed heavy metal concentrations in the tissue samples of Corbiculafluminea, by ICP-OES. In the tissues, average levels of 23.99 µg/g of Cu, 144.21 µg/g of Zn, 0.71 µg/g of Cd, 7.10 µg/g of Cr and 2.41 µg/g of Pb were detected ahowing that this last value is high and above the ANVISA reference (2.00 µg/g) for fish and other products. The results suggest that natural processes occuring in the Ribeira de Iguape River are not sufficient for purification so that metals remain in the water and can accumulate in the trophic chain.