Determinação das formas de nitrogênio e nitrogênio total em rochas-reservatório de petróleo por destilação com arraste de vapor e método do indofenol

Several extraction procedures are described for the determination of exchangeable and fixed ammonium, nitrate + nitrite, total exchangeable nitrogen and total nitrogen in certified reference soils and petroleum reservoir rock samples by steam distillation and indophenol method. After improvement of the original distillation system, an increase in worker safety, a reduction in time consumption, a decrease of 73% in blank value and an analysis without ammonia loss, which could possibly occur, were achieved. The precision (RSD < 8%, n = 3) and the detection limit (9 mg kg-1 NH4+-N) are better than those of published procedures.

Desenvolvimento de um equipamento para avaliação do efeito do etanol na pressão de vapor e entalpia de vaporização em gasolinas automotivas

The quality of the gasoline utilized for fueling internal combustion engines with spark ignition is directly affected by the gasoline's properties. Thus, the fuel's properties must be in perfect equilibrium to allow the engine to perform optimally, not only insofar as fuel consumption is concerned, but also in order to reduce the emission of pollutants. Vapor pressure and vaporization enthalpy are important properties of a gasoline determining the fuel's behavior under different operating conditions in internal combustion engines. The study reported here involved the development of a device to determine the vapor pressure and the vaporization enthalpy of formulations containing volumes of 5, 15 and 25% of ethanol in four base gasolines (G1, G2, G3 and G4). The chemical composition of these gasolines was determined using a gas chromatographer equipped with a flame ionization detector (FID).

Um novo método para quantificar mercúrio orgânico (Hg orgânico) empregando a espectrometria de fluorescência atômica do vapor frio

In this work a simple and sensitive procedure to extract organic mercury from water and sediment samples, using methylene chloride in acidic media followed by CVAFS quantification has been developed. The method was evaluated for possible interferents, using different inorganic mercury species and humic acid, no effects being observed. The detection limit for organic mercury was 160 pg and 396 pg for water and sediment samples respectively. The accuracy of the method was evaluated using a certified reference material of methylmercury (BCR-580, estuarine sediment). Recovery tests using methylmercury as surrogate spiked with 1.0 up to 30.0 ng L-1 ranged from 90 up to 109% for water samples, whereas for sediments, recoveries ranged from 57 up to 97%.

Influência do sulfato de condroitina na formação de filmes isolados de polimetacrilato: avaliação do índice de intumescimento e permeabilidade ao vapor d'água

Natural or modified chondroitin sulfate was incorporated in to polymethacrylate to obtain isolated films. The addition of polysaccharide to synthetic polymers occurred at different rates. Isolated films were micro and macroscopically characterized and swelling index and water vapor transmission were determined. Results indicated changed transparency and flexibility, coupled to their dependence on increase in polysaccharide concentration. A similar occurrence was reported in the permeability to water vapor and swelling degree. Films composed of modified chondroitin sulfate, 90:10 concentration, showed hydration levels, permeability and morphological properties which allow them to be applied as excipients in the development of new drug delivery systems.

Produção de hidrogênio a partir da reforma a vapor de etanol utilizando catalisadores Cu/Ni/gama-Al2o3

Cu/Ni/gamma-Al2O3 catalysts were prepared by an impregnation method with 2.5 or 5% wt of copper and 5 or 15% wt of nickel and applied in ethanol steam reforming. The catalysts were characterized by atomic absorption spectrophotometry, X-ray diffraction, temperature programmed reduction with hydrogen and nitrogen adsorption. The samples showed low crystallinity, with the presence of CuO and NiO, both as crystallites and in dispersed phase, as well as of NiO-Al2O3. The catalytic tests carried out at 400 ºC, with a 3:1 water/ethanol molar ratio, indicated the 5Cu/5Ni/Al2O3 catalyst as the most active for hydrogen production, with a hydrogen yield of 77% and ethanol conversion of 98%.

Remoção de chumbo(II) em sistemas descontínuos por carvões ativados com ácido fosfórico e com vapor

Adsorption of heavy metal cations by activated carbon is dependent on the capacity of the material in promoting adsorption and the time needed to reach equilibrium. Carbon samples were previously activated either by phosphoric acid treatment at 400 ºC or by steam at 800 ºC. The results of Pb(II) adsorption by these activated carbons have shown that equilibrium was typically reached within the first 5 min of contact between carbon and metal solution, with a maximum adsorption capacity higher than 69 mg g-1 for the vapor-activated sample. Temperature influences the sorption capacity, which corresponds to an endothermic process. Lead(II) retention is more pronounced at high temperature and low pH.

Remoção de chumbo(II) em sistemas contínuos por carvão ativado com vapor

Fixed-bed column studies were undertaken to evaluate the performance of a commercial Brazilian activated carbon in removing Pb(II) from aqueous environment. Breakthrough points were found out for the metal adsorption by varying different operating parameters like feed concentrations (10 and 20 mg L-1) and bed heights (0.5, 1.5 and 2.8 cm). A good agreement was observed between the experimental data and the values predicted by the bed depth service time (BDST) model. Regeneration of the exhausted columns was possible with HCl, and the adsorption capacity was maintained after three adsorption-desorption cycles.

Alteração do caráter hidrofílico de filmes de quitosana por tratamento de plasma de HMDS

Alteration in hydrophilicity feature of chitosan films by hexamethyldisilazane (HMDS) cold-plasma treatment is evaluated. All treated films were colorless and transparent with no apparent textural changes. The effect on surfaces was characterized through contact angle measurements, degree of swelling and water vapor permeation. A significant reduction in all of the hydrophilicity parameters was observed. It is assumed that the HMDS treatment forms nonpolar silicone type structures. The goal is to investigate the formation of a stable hydrophobic barrier in order to increase the chitosan films usefulness in packaging applications.

Validação de metodologia analítica para determinação de mercúrio total em amostras de urina por espectrometria de absorção atômica com geração de vapor frio (CV-AAS): estudo de caso

Mercury is a toxic metal used in a variety of substances over the course history. One of its more dubious uses is in dental amalgam restorations. It is possible to measure very small concentrations of this metal in the urine of exposed subjects by the cold vapor atomic absorption technique. The present work features the validation as an essential tool to confirm the suitability of the analytical method chosen to accomplish such determination. An initial analysis will be carried out in order to evaluate the environmental and occupational levels of exposure to mercury in 39 members of the auxiliary dental staff at public consulting rooms in the city of Araguaína (TO).

Reator de UV-Ozônio com lâmpada a vapor de mercúrio a alta pressão modificada para tratamento superficial de óxidos transparentes condutivos utilizados em dispositivos poliméricos eletroluminescentes

An UV-Ozone reactor was developed with an ignition tube extracted into HID mercury lamp used to irradiation on zinc oxide (ZnO) and fluorinated tin oxide (FTO) films for PLEDs devices. Different exposures times were used. In contact angle measurements revealed better results for ZnO and FTO by 15 and 5 min, respectively. In Diffuse Reflectance Infra-red Fourier Transformed (DRIFT) spectroscopy allowed the observation of water, hydrocarbon and carbon dioxide adsorbed on the untreated TCO surfaces. After the UV-Ozone treatment the contaminants were significantly reduced or eliminated and the PLEDs devices decreased threshold voltages in comparison with respectively untreated TCOs.

Organic and total mercury determination in sediments by cold vapor atomic absorption spectrometry: methodology validation and uncertainty measurements

The purpose of the present study was to validate a method for organic Hg determination in sediment. The procedure for organic Hg was adapted from literature, where the organomercurial compounds were extracted with dichloromethane in acid medium and subsequent destruction of organic compounds by bromine chloride. Total Hg was performed according to 3051A USEPA methodology. Mercury quantification for both methodologies was then performed by CVAAS. Methodology validation was verified by analyzing certified reference materials for total Hg and methylmercury. The uncertainties for both methodologies were calculated. The quantification limit of 3.3 µg kg-1 was found for organic Hg by CVAAS.

Formation of TiO2 photoanodes by simultaneous electrophoretic deposition of anatase and rutile particles for photoassisted electrolytic copper ions removal

The influence of Anatasa/Rutile ratio on TiO2 films, grown by electrophoretic deposition was studied in the photoassisted electrolytic copper ions removal from cyanide solutions. The proper dispersant dosage allowing the simultaneous electrophoretic deposition of Anatase and Rutile was chosen based on electrokinetic measurements; evidenced by the XRD spectra of the formed films. The evaluation of films photoassisted electrolytic copper ion removal showeds that it is possible to enhance the activity of Anatase films by adding some Rutile exploiting the synergetic interaction between these two materials, achieve by its proper deposition.

Efeito da adição de lantânio em catalisadores de Ni/ZrO2 aplicados na reação de reforma a vapor de etanol

The catalytic performance of Ni/ZrO2 catalysts loaded with different lanthanum content for steam reforming of ethanol was investigated. Catalysts were characterized by BET surface area, X-ray diffraction, UV-vis spectroscopy, temperature programmed reduction, and X-ray absorption fine structure techniques. Results showed that lanthanum addition led to an increase in the degree of reduction of both NiO and nickel surface species interacting with the support, due to the higher dispersion effect. The best catalytic performance at 450 ºC was found for the Ni/12LZ catalyst, which exhibited an effluent gaseous mixture with the highest H2 yield.

Efeito do teor de umidade sobre o pré-tratamento a vapor e a hidrólise enzimática do bagaço de cana-de-açúcar

The effect of moisture content in the steam treatment and enzymatic hydrolysis of sugarcane bagasse was evaluated. Steam treatment was perfomed at 195-210 ºC for 4-8 min using cane bagasse with moisture contents in the range 16-100 wt% (dry basis). Increased moisture contents not only had a positive influence in recovery of main cane biomass components but also resulted in better substrates for enzymatic hydrolysis. As a result, drying is not required for optimal pretreatment and enzymatic hydrolysis of sugarcane bagasse, which can be processed into second generation ethanol immediately after crushing and hot water washing.

Cristalización de zeolita beta mediante conversión asistida por vapor: influencia de los parámetros de síntesis

In the present work, beta zeolites were prepared by an alternative route called steam-assisted conversion (SAC). Several zeolites were synthesized using amorphous dry gels with a low SDA concentration (0.09 mol, TEAOH). Temperature and crystallization time were the main parameters studied. X-ray diffraction (XRD), infrared spectroscopy (IR) and scanning electron microscopy (SEM) were the characterization techniques employed. The zeolites prepared showed mixed phases such as beta, MTW and ZSM-5 while only one sample treated at 150ºC with 24 h of crystallization time showed a pure ZSM-5 phase (SAC-5). These preliminary results serve as a starting point for optimizing the synthesis of a specific type of zeolite using the SAC method.