Influência dos parâmetros de processo na deposição de nitreto de titânio por plasma em gaiola catódica

Titanium nitride films were grown on glass using the Cathodic Cage Plasma Deposition technique in order to verify the influence of process parameters in optical and structural properties of the films. The plasma atmosphere used was a mixture of Ar, N2 and H2, setting the Ar and N2 gas flows at 4 and 3 sccm, respectively and H2 gas flow varied from 0, 1 to 2 sccm. The deposition process was monitored by Optical Emission Spectroscopy (OES) to investigate the influence of the active species in plasma. It was observed that increasing the H2 gas flow into the plasma the luminescent intensities associated to the species changed. In this case, the luminescence of N2 (391,4nm) species was not proportional to the increasing of the H2 gas into the reactor. Other parameters investigated were diameter and number of holes in the cage. The analysis by Grazing Incidence X-Ray Diffraction (GIXRD) confirmed that the obtained films are composed by TiN and they may have variations in the nitrogen amount into the crystal and in the crystallite size. The optical microscopy images provided information about the homogeneity of the films. The atomic force microscopy (AFM) results revealed some microstructural characteristics and surface roughness. The thickness was measured by ellipsometry. The optical properties such as transmittance and reflectance (they were measured by spectrophotometry) are very sensitive to changes in the crystal lattice of the material, chemical composition and film thicknesses. Therefore, such properties are appropriate tools for verification of this process control. In general, films obtained at 0 sccm of H2 gas flow present a higher transmittance. It can be attributed to the smaller crystalline size due to a higher amount of nitrogen in the TiN lattice. The films obtained at 1 and 2 sccm of H2 gas flow have a golden appearance and XRD pattern showed peaks characteristics of TiN with higher intensity and smaller FWHM (Full Width at Half Maximum) parameter. It suggests that the hydrogen presence in the plasma makes the films more stoichiometric and becomes it more crystalline. It was observed that with higher number of holes in the lid of the cage, close to the region between the lid and the sample and the smaller diameter of the hole, the deposited film is thicker, which is justified by the most probability of plasma species reach effectively the sample and it promotes the growth of the film

Influência da vermiculita expandida na formulação de pastas leves para evitar a migração de gás em cimentação de poços petrolíferos

The gas migration during the cementing of wells is one of the main problems of oil wells engineering. Its occurrence can cause severe problems since shortly to loss of control of the well after cementation. Recently, 20/04/2010 In an accident of major proportions in the Gulf of Mexico, among other factors, faulty cementing operation provided the gas migration, causing the accident, in which 11 people died and 17 were injured occurred. Besides the serious consequences that can be caused by gas migration, remediation of the problem, which is made by injecting cement in damaged areas, usually involves additional costs and is not always effective. Therefore, preventing gas migration to be preferred. Some methods are used to prevent the migration of the pressurized gas as the annular space, application of pressure pulses, reducing the height of the cement column compressible cement pastes of low permeability, pastes and to control free filtered water, and binders of thixotropic cement expandable and flexible. Thus, the cement pastes used to prevent gas migration must meet the maximum these methods. Thus, this study aimed to formulate a cement paste to prevent gas migration, using the expanded vermiculite, and evaluate the behavior of the folder trials necessary for use in oil wells. Free water content, rheological properties, compressive strength, loss of liquid phase sedimentation of solids, specific weight, thickening time and gas migration: The following tests were performed. The results show that meets the specifications paste formulated for use in oil wells and the use of expanded vermiculite contribute to the absorption of free water, thixotropy and low density. The absorption of free water is proven to result in zero percentage test free water content, thixotropy is observed with the high value of the initial gel strength (Gi) in testing rheological properties and low density is proven in test weight specific

Desenvolvimento de uma formulação cólon específica visando o tratamento da colite ulcerativa

Micro and nanoparticulate systems as drug delivery carriers have achieved successful therapeutic use by enhancing efficacy and reducing toxicity of potent drugs. The improvement of pharmaceutical grade polymers has allowed the development of such therapeutic systems. Microencapsulation is a process in which very thin coatings of inert natural or synthetic polymeric materials are deposited around microsized particles of solids or around droplets. Products thus formed are known as microparticles. Xylan is a natural polymer abundantly found in nature. It is the most common hemicellulose, representing more than 60% of the polysaccharides existing in the cell walls of corn cobs, and is normally degraded by the bacterial enzymes present in the colon of the human body. Therefore, this polymer is an eligible material to produce colon-specific drug carriers. The aim of this study was to evaluate the technological potential of xylan for the development of colon delivery systems for the treatment of inflammatory bowel diseases. First, coacervation was evaluated as a feasible method to produce xylan microcapsules. Afterwards, interfacial cross-linking polymerization was studied as a method to produce microcapsules with hydrophilic core. Additionally, magnetic xylan-coated microcapsules were prepared in order to investigate the ability of producing gastroresistant systems. Besides, the influence of the external phase composition on the production and mean diameter of microcapsules produced by interfacial cross-linking polymerization was investigated. Also, technological properties of xylan were determined in order to predict its possible application in other pharmaceutical dosage forms

Fermentação alcoólica utilizando líquido da casca de coco verde como fonte de nutrientes

The liquid of the rind of green coconut (LCCV), an effluent stream from the industrial processing of green coconut rind, is rich in sugars and is a suitable feedstock for fermentation. The first step of this study was to evaluate the potential of natural fermentation of LCCV. As the literature did not provide any information about LCCV and due to the difficulty of working with such an organic effluent, the second step was to characterize the LCCV and to develop a synthetic medium to explore its potential as a bioprocess diluent. The third step was to evaluate the influence of initial condensed and hydrolysable tannins on alcoholic fermentation. The last step of this work was divided into several stages: in particular to evaluate (1) the influence of the inoculum, temperature and agitation on the fermentation process, (2) the carbon source and the use of LCCV as diluent, (3) the differences between natural and synthetic fermentation of LCCV, in order to determine the best process conditions. Characterization of LCCV included analyses of the physico-chemical properties as well as the content of DQO, DBO and series of solids. Fermentation was carried out in bench-scale bioreactors using Saccharomyces cerevisiae as inoculum, at a working volume of 5L and using 0.30% of soy oil as antifoam. During fermentations, the effects of different initial sugars concentrations (10 - 20%), yeast concentrations (5 and 7.5%), temperatures (30 - 50°C) and agitation rates (400 and 500 rpm) on pH/sugars profiles and ethanol production were evaluated. The characterization of LCCV demonstrated the complexity and variability of the liquid. The best conditions for ethanol conversion were (1) media containing 15% of sugar; (2) 7.5% yeast inoculum; (3) temperature set point of 40°C and (4) an agitation rate of 500 rpm, which resulted in an ethanol conversion rate of 98% after 6 hours of process. A statistical comparison of results from natural and synthetic fermentation of LCCV showed that both processes are similar

Análise técnica e econômica do processo de obtenção de espaguetes com adição de farinha de trigo integral e farinha de linhaça

This work studies the fabrication of spaghetti through the process at high temperatures through the use of flour added to flour and flaxseed meal, with the aim of evaluating the final product quality and estimate the cost of production. The values of moisture, ash, protein, wet gluten, gluten index, falling number and grain of flour and mixtures to test to be the possible use in mass manufacturing and technological criteria for compliance with current legislation. Spaghetti noodles type were manufactured by adding 10% and 20% flour and 10% and 20% flaxseed meal with performance of physical-chemical, sensory and rheological properties of the products. Further analysis was performed on the product acceptance and estimation of production cost in order to create subsidies to enable the introduction of products with greater acceptance and economic viability in the market by the food industry. On the rheology of the product test was cooking the pasta, specifying the volume increase, cooking time and percentage of solid waste. In the sensory evaluation was carried out the triangular test of product differentiation with 50 trained judges and acceptance testing by a hedonic scale with evaluation of the aspects color, taste, smell and texture. In defining the sensory profile of the product was performed with ADQ 9 judges recruited and trained at the factory, using unstructured scale of 9 cm, assessing the attributes of flavor of wheat, flax flavor, consistency, texture of raw pasta, raw pasta color and color of cooked pasta. The greater acceptance of product quality was good and the pasta with 20% flour, 10% followed by the full product, 10% and 20% flaxseed characterized the average quality of the criterion of loss analysis of solids, together with mass full commercial testing. In assessing the estimated cost of production, the two products more technologically feasible and acceptable (20% whole and 10% flaxseed) were evaluated in high temperature processes. With total cost of R $ 4,872.5 / 1,000 kg and R $ 5,354.9 / 1,000 kg respectively, the difference was related to the addition of lower inputs and higher added value in the market, flour and flaxseed meal. The comparative analysis of cases was confirmed the reduction in production time (10h), more uniform product to the drying process at high temperature compared to conventional

Recuperação e purificação de quitosanases usando adsorção em leito expandido com streamline DEAE com modelagem e simulação usando redes neurais

Expanded Bed Adsorption (EBA) is an integrative process that combines concepts of chromatography and fluidization of solids. The many parameters involved and their synergistic effects complicate the optimization of the process. Fortunately, some mathematical tools have been developed in order to guide the investigation of the EBA system. In this work the application of experimental design, phenomenological modeling and artificial neural networks (ANN) in understanding chitosanases adsorption on ion exchange resin Streamline® DEAE have been investigated. The strain Paenibacillus ehimensis NRRL B-23118 was used for chitosanase production. EBA experiments were carried out using a column of 2.6 cm inner diameter with 30.0 cm in height that was coupled to a peristaltic pump. At the bottom of the column there was a distributor of glass beads having a height of 3.0 cm. Assays for residence time distribution (RTD) revelead a high degree of mixing, however, the Richardson-Zaki coefficients showed that the column was on the threshold of stability. Isotherm models fitted the adsorption equilibrium data in the presence of lyotropic salts. The results of experiment design indicated that the ionic strength and superficial velocity are important to the recovery and purity of chitosanases. The molecular mass of the two chitosanases were approximately 23 kDa and 52 kDa as estimated by SDS-PAGE. The phenomenological modeling was aimed to describe the operations in batch and column chromatography. The simulations were performed in Microsoft Visual Studio. The kinetic rate constant model set to kinetic curves efficiently under conditions of initial enzyme activity 0.232, 0.142 e 0.079 UA/mL. The simulated breakthrough curves showed some differences with experimental data, especially regarding the slope. Sensitivity tests of the model on the surface velocity, axial dispersion and initial concentration showed agreement with the literature. The neural network was constructed in MATLAB and Neural Network Toolbox. The cross-validation was used to improve the ability of generalization. The parameters of ANN were improved to obtain the settings 6-6 (enzyme activity) and 9-6 (total protein), as well as tansig transfer function and Levenberg-Marquardt training algorithm. The neural Carlos Eduardo de Araújo Padilha dezembro/2013 9 networks simulations, including all the steps of cycle, showed good agreement with experimental data, with a correlation coefficient of approximately 0.974. The effects of input variables on profiles of the stages of loading, washing and elution were consistent with the literature

Dinâmica de Sedimentação de Lodo em Lagoas de Estabilização

Stabilization ponds are an effective sewage treatment alternative for the climatic conditions prevailing in Brazil. In the present work, a primary facultative pond was studied, in the city of Natal, Rio Grande do Norte, Northeast Brazil. The aim of this study was to evaluate the sedimentation dynamics in the facultative pond. The pond was divided in three section or zones along its length starting from the inlet end namely A1, A2 and A3. The research was accomplished in three phases. In the first the mapping of the sludge layer was done, sludge core samples were also collected for analysis for total, fixed and volatile solids and the depth of the sludge layer was determined using a portable echo sounder. In the second solids sedimentation rates were measured using traps placed in the inlet and outlet zones and in the third phase resuspension sludge was evaluate using a tracer. The amount accumulated sludge since the start operation was 13.583 m3. The sedimentation constant averages changed between 0.93 to 2.94 and 3.90 to 5.80 for the depths of 0.5 and 1.0 m respectively. The relationship between volatile and fixed solids (SV/SF) increased along the pond. The removal efficiencies were 52.12%, 36.09%, and 37.50% for BOD, COD and SS, respectively. The sludge accumulation model proposed had a good adjustment with 0.17 m3/hab.year rate. The results presented here demonstrated that the wind had a direct influence on the sedimentation of solids in this pond affecting the efficiency and sludge accumulation

Viabilidade técnica de uma rota não convencional para a produção de leite de cabra em pó em cooperativas do Rio Grande do Norte

Nowadays, Brazil has both the greatest goat herd and the greatest goat milk production of South America. The state of Rio Grande do Norte, located in northeast of Brazil, has an average year production of three thousand cubic meters of goat milk in natura. Part of this milk production is homemade and it comes from small farms, which unite in rural cooperatives created to encourage the production and implementation of industrial processes for preservation and processing of milk. Results presented by literature and obtained from preliminary essays in this thesis show that non conventional dryer of spouted bed with inert particles is able to produce powder milk from in natura milk (cattle or goat), with the same quality of spray dryer, however, operating at low cost. The method of drying in spouted bed consists of injecting milk emulsion on the bed of inert particles gushed by hot air. This emulsion covers the particles with a thin film, which dries and is reduced to powder during the circulation of inerts inside the bed. The powder is dragged by exhaustion air and separated in the cyclone. The friction among particles resulted from the particles circulation, encourages high taxes of shear in the thin film of emulsion, breaking the cohesive forces and making this process possible. Studying the drying process and the powder goat milk production in one unit of spouted bed with inert particles, seeing the development of a low cost technological route for powder milk production is the aim of this thesis. The powder milk produced by this route must attend the local demand of food industries which need an intermediate product to be used as a food ingredient (ice-cream, milk candy). In order to reach this aim, this thesis approaches the aspects related to physical, thermodynamics and physic-chemicals characteristics of goat milk, whose complete data are still inexistent in the literature. The properties of materials are of great importance to the project of any process which involves the operations of transportation of movement, heat and mass quantity, such as the dryers which operate in fluid dynamically active regime, like the spouted bed. It was obtained new data related to the goat milk properties in function of concentration of solids and temperature. It is also important to mention the study developed about the kinetic of solids retention in the bed of inert particles during the drying of goat milk. It was found more adequate processes conditions to the proposed technological route to be implemented in small and micro-industries, with simplifications in the system of milk injection as well as in the form of operation of the dryer. Important data were obtained for a posterior stage of this research which involves the v modeling, simulation, control and optimization of the process. The results obtained in this thesis, in relation to process performance as well as to the quality of produced powder milk validate the proposal of using the spouted bed dryer in the production of powder goat milk

Caracterização do conteúdo de fossas e tanques sépticos na cidade de Natal

Only 32% of the population of Natal is attended by sewage, while the remaining population use pits and septic tanks. The characterization of the contents of septic tanks and pits contributes to the performance of such system and may guide the decision on treatment of these contents. The main of this research is to characterize the contents of interior residential pits and septic tanks in the greater Natal, with the following specific goals: to develop and manufacture a sampler capable of collecting a representative sample of the entire column (the surface scum, the clarified liquid and sludge bottom); to compare the contents of the tanks with the pits; to compare the contents of the septage from vacuum trucks; to relate the composition content with socioeconomic characteristics of households; to compare the content in both chambers of the septic tanks in series; to assess the situation of the content before and six months after the cleanness; and ultimately propose a pilot scale plant for treatment of septage. Once the sampler was developed, samples were collected within 14 septic tanks and 10 pits in many districts of Natal. Medians of the 24 systems were obtained: temperature, pH, conductivity, oil and grease, total solids, total suspended solids and sediments of 28.0 °C, 6.95; 882 mS/cm, 75.2 mg/L; 10,169 mg/L, 6,509 mg/L and 175 mL/L respectively; 111.0 mgN/L for ammonia, 130.5 mgN/ L for organic nitrogen, 0.2 mgN/L for nitrite, 0.4 mg/L for nitrate; 8935 mgO2/L for COD, 29.2 mgP/L for total phosphorus, thermotolerant coliforms from 9.95 E +06 CFU/100mL helminth eggs and 9.2 eggs/L with a maximum concentration of 688 eggs/L and minimum of 0 eggs/L. Medians of organic nitrogen and TKN were significantly different between groups of tanks and pits. The systems with cleanness gap from 11 and 20 years presented the higher concentrations for most variables. The effluent from the toilets and bathrooms participate more effectively in contributing fractions of solids, alkalinity, nitrogen, COD, total phosphorus, thermotolerant coliforms and helminth eggs. The systems used by socioeconomics class with income from R$ 3,700.00 to R$ 7,600.00, presented higher concentrations for COD, nitrogen, solids and helminth eggs. The first of the two chambers had always presented higher concentrations over the second compartment. The analysis of variance for most variables, showed that the values of septic tanks, pits and septage from vacuum trucks belong to the same group. In the samples taken after cleanness, the median of pH and temperature increased, while alkalinity, COD, organic nitrogen, total phosphorus, ammonia and helminth eggs decreased. The oils and greases and thermotolerant coliforms had slightly varied due to the continuous release of sewage into the systems that maintained their steady state concentrations.

Nitrificação de efluentes de reatores anaeróbicos em filtros submersos aerados

Although the good performance in organic matter and suspended solids removal, the anaerobic reactors are unable to remove ammonia nitrogen from sewage, which makes indispensable to include a step of post-treatment for removal of ammonia or nitrate as necessary. This paper presents the performance of a new variant technology, where the nitrification unit, preceded by anaerobic units, is a submerged aerated biological filter, without continuous sludge discharge in their daily operation. The oxygenation system is very simple and inexpensive, consisting of perforated hoses and compressors. The anaerobic reactors are a septic tank with two chambers followed (8.82 m³) and two parallel anaerobic filters (36 m³ each) filled with ceramic bricks and conics plastic parts. Both followed aerated filters were filled with cut corrugated conduit. The study evaluated the behavior of the system with constant domestic sewage flow (10 m³/d) and different aeration conditions, are these: stage 01, when applied air flow of 0.01 m³ air/min in both aerated filter; stage 02, remained in the initial air flow rate in the second aerated filter and increased at the first to 0.05 m³ air/min; at last, at last, in stage 03, the air flow rate of first aerated filter was 0.10 m³ air/min and on the second remained at 0.01 m³ air/min. The filter FA1 received load of 0.41 kg COD/m³.d, 0.37 kg COD/m³.d and 0.26 kg COD/m³.d on phases 01, 02 and 03, respectively. The FA2 received loads of 0.25 kg COD/m³.d, 0.18 kg COD/m³.d and 0.14 kg COD/m³.d on phases 01, 02 and 03, respectively. During stage 01, were found the following results: 98% removals of BODtotal and 92% of CODtotal, with effluent presenting 9 mg/L of BODtotal final average and 53 mg/L of CODtotal average; suspended solids removals of 93%, with a mean concentration of 10 mg/L in the final effluent; 47% reduction of ammonia of FA2 to FAN 's, presenting average of 28 mg NNH3/ L of ammonia in the effluent with; the dissolved oxygen levels always remained around 2.0 mg/L. During stage 02, were found removals of 97% and 95% to BODtotal and suspended solids, respectively, with average final concentrations of 8 and 7 mg/L, respectively; was removed 60% of ammonia, whose final concentration was 16.3 mg NNH3/ L, and nitrate was increased to a final average concentration of 16.55 mg N-NO3/L. Finally, the stage 03 provided 6 mg/L of DBOtotal (98% removal) and 23 mg/L of CODtotal (95% removal) of final effluent concentrations average. At this stage was identified the higher ammonia oxidation (86%), with final effluent showing average concentration of 6.1 mg N-NH3/L, reaching a minimum of 1.70 mg N-NH3/L. In some moments, during stage 03, there was a moderate denitrification process in the last aerated filter. The average turbidity in the effluent showed around 1.5 NTU, proving the good biomass physical stability. Therefore, the results demonstrate the submerged biological filters potential, filled with high void ratio material (98%), and aerated with hoses and compressor adoption, in the carbonaceous and nitrogenous matter oxidation, also generating an effluent with low concentration of solids

Uso urbano não potável de água de lagoas do sistema de drenagem de Natal

The detention and infiltration ponds of urban drainage system has function to protect the population from undesirable effects of floods. In general these ponds are not completly used and it potential is wasted. As it are disseminated at different places at cities it can reduce costs with water transport and permit water preservation of best quality. Some it utilities includes use in green areas irrigation, industrial among than cooling towers and boiler, soil compaction, cleaning urban road, pisciculture and fire fighting system. The quality these water is influenced by anauthorized sewage in the drainage system. This study was performed in six detention and infiltration ponds at drainage system of Natal, which aim was to verify the non-portable use these ponds on urban environment. As indirect aim would to incentive the water utilization these ponds as a water source to another uses in urban environment. These ponds represents the characteristics of detention and infiltration of Natal city and consequently of Brazil. As the water quality, the ponds presents following characteristics: three has apparently good quality, other showed intermediate condition and two had water polluted. Were performed twenty sample in each ponds and the following parameters assessed: pH, temperature, dissolved oxygen, turbidity, electrical conductivity, coliform thermotolerant, ammonia, organic nitrogen, TKN, nitrate, total phosphorus and alkalinity, bicarbonate, chloride, total hardness, calcium and magnesium hardness, total solids, TSS, TDS, COD and SAR°. To utilization on pisciculture we recommend use in ponds which presents the best quality. Only one pond presented higher pollutants and it not being appropriated for use in cooling tower. The content of solids suspension restricted the water use in all ponds in boilers. As water use in soil compaction, cleaning urban road and fire fighting system the water from these ponds are not appropriated. However, the recommended limits from literature are to domestic sewage, due to this, the parameters are restrictive to diminish the sanitary risk that could be offered with it utilization. The infiltration velocity of water these assessed ponds restrict a moderato use, however the effects are potentiated only in soil less sandy, which not occur in Natal. It is recommend the unrestricted irrigation utilization in ponds with best quality of water, and a restricted irrigation to ponds with worst quality of water. As load of pollutants, it is recommended a complementary treatment in those ponds whit higher load to diminish sanitary risks. In only one pond was found one helminth eggs and due to the convention formula of results, it was found for all ponds less than 1 helminth/liter eggs.

Degradação catalítica de polietileno de alta densidade sobre a zeólita HZSM

In last years it has talked a lot about the environment and the plastic waste produced and discarded. In last decades, the increasing development of research to obtain fuel from plastic material, by catalytic degradation, it has become a very attractive looking, as these tailings are discarded to millions worldwide. These materials take a long time to degrade themselves by ways said natural and burning it has not demonstrated a viable alternative due to the toxic products produced during combustion. Such products could bring serious consequences to public health and environment. Therefore, the technique of chemical recycling is presented as a suitable alternative, especially since could be obtain fractions of liquid fuels that can be intended to the petrochemical industry. This work aims to propose alternatives to the use of plastic waste in the production of light petrochemical. Zeolites has been widely used in the study of this process due to its peculiar structural properties and its high acidity. In this work was studied the reaction of catalytic degradation of high-density polyethylene (HDPE) in the presence HZSM-12 zeolites with different acid sites concentrations by thermogravimetry and pyrolysis coupled with GC-MS. The samples of the catalysts were mixed with HDPE in the proportion of 50% in mass and submitted to thermogravimetric analyses in several heating rates. The addition of solids with different acid sites concentrations to HDPE, produced a decrease in the temperature of degradation of the polymer proportional the acidity of the catalyst. These qualitative results were complemented by the data of activation energy obtained through the non-isothermal kinetics model proposed by Vyazovkin. The values of Ea when correlated to the data of surface acidity of the catalysts indicated that there is a exponential decrease of the energy of activation in the reaction of catalytic degradation of HDPE, in function of the concentration of acid sites of the materials. These results indicate that the acidity of the catalyst added to the system is one of the most important properties in the reaction of catalytic degradation of polyethylene

Síntese, caracterização e estudo fotofísico de complexos de 4,4- diaminoestilbeno-2,2-dissulfonato com íons lantanídeos

This is a work involving fundamental studies of chemistry where the synthesis and structural characterization, as well as a possible future application of these new compounds as luminescent sensors or sunscreen agents, complexes with 4,4 diaminostilbene-2,2-disulfonic (DSD) and trivalent lanthanide ions La3+, Nd3+, Eu3+, Gd3+ and Yb3+, were synthesized in the ratio of 3 mmol: 1 mmol (DSD: lanthanides). The complexes obtained with these ions were present in powder form and were characterized by complexometric titration with EDTA CHN Elemental analysis, molecular absorption spectroscopy in the ultraviolet region, the absorption spectroscopy in the infrared, thermal analysis (TG / DTG), Nuclear Magnetic Resonance - NMR 1H and Luminescence Spectroscopy. The complexometric titration and CHN analysis, confirmed the TG / DTG which suggest that these complexes have the following general chemical formulas: [La2(C14H12S2O6N2)2(H2O)2Cl2].7H2O,[Nd2(C14H12S2O6N2)2(H2O)2Cl2].6H2O,[Eu2(C14 H12S2O6N2)2(H2O)2Cl2].7H2O,[Gd2(C14H12S2O6N2)2(H2O)2Cl2].4H2O e [Yb2(C14H12S2O6N2)2(H2O)2].6H2O. The disappearance of the bands in the infrared spectrum at 2921 cm-1 and 2623 cm-1 and the displacement of the bands in the spectra of the amine complex indicate that the lanthanide ion is coordinated to the oxygen atoms and the sulfonate groups of the nitrogens amines, suggesting the formation of the dimer. The disappearance of the signal and the displacement signal SO3H amines in the 1H NMR spectrum of this complex are also indicative coordination and dimer formation. The Thermogravimetry indicates that the DSD is thermally stable in the range of 40º to 385°C and their complexes with lanthanide ions exhibit weight loss between 4 and 5 stages. The Uv-visible spectra indicated that the DSD and complexes exhibit cis isomers. The analysis of luminescence indicates that the complexes do not exhibit emission in the region of the lanthanides but an intense emission part of the binder. This is related to the triplet states of the ligand, which are in the lowest energy state emitting lanthanide ions, and also the formation of the dimer that suppress the luminescence of ion Eu3+. The formation of dimer was also confirmed by calculating the europium complex structure using the model Hamiltonian PM6 and Sparkle

Avaliação do potencial da fibra e casca de coco maduro, casca de coco verde e cacto pré-tratados visando à produção de etanol

The present work investigated the potential of different residual lignocellulosic materials generated in rural and urban areas (coconut fibre mature, green coconut shell and mature coconut shell), and vegetable cultivated in inhospitable environments (cactus) aimed at the production of ethanol, being all materials abundant in the Northeast region of Brazil. These materials were submitted to pretreatments with alkaline hydrogen peroxide followed by sodium hydroxide (AHP-SHP), autohydrolysis (AP), hydrothermal catalyzed with sodium hydroxide (HCSHP) and alkali ethanol organosolv (AEOP). These materials pretreated were submitted to enzymatic hydrolysis and strategies of simultaneous saccharification and fermentation (SSF) and saccharification and fermentation semi-simultaneous (SSSF) by Saccharomyces cerevisiae, Zymomonas mobilis and Pichia stipitis. It was also evaluated the presence of inhibitory compounds (hydroxymethylfurfural, furfural, acetic acid, formic acid and levulinic acid) and seawater during the fermentative process. Materials pretreated with AHP-SHP have resulted in delignification of the materials in a range between 54 and 71%, containing between 51.80 and 54.91% of cellulose, between 17.65 and 28.36% of hemicellulose, between 7.99 and 10.12% of lignin. Enzymatic hydrolysis resulted in the conversions in glucose between 68 and 76%. Conversion yields in ethanol using SSF and SSSF for coconut fibre mature pretreated ranged from 0.40 and 0.43 g/g, 0.43 and 0.45 g/g, respectively. Materials pretreated by AP showed yields of solids between 42.92 and 92.74%, containing between 30.65 and 51.61% of cellulose, 21.34 and 41.28% of lignin. Enzymatic hydrolysis resulted in glucose conversions between 84.10 and 92.52%. Proceeds from conversion into ethanol using green coconut shell pretreated, in strategy SSF and SSSF, were between 0.43 and 0.45 g/g. Coconut fibre mature pretreated by HCSHP presented solids yields between 21.64 and 60.52%, with increased in cellulose between 28.40 and 131.20%, reduction of hemicellulose between 43.22 and 69.04% and reduction in lignin between 8.27 and 89.13%. Enzymatic hydrolysis resulted in the conversion in glucose of 90.72%. Ethanol yields using the SSF and SSSF were 0.43 and 0.46 g/g, respectively. Materials pretreated by AEOP showed solid reductions between 10.75 and 43.18%, cellulose increase up to 121.67%, hemicellulose reduction up to 77.09% and lignin reduced up to 78.22%. Enzymatic hydrolysis resulted in the conversion of glucose between 77.54 and 84.27%. Yields conversion into ethanol using the SSF and SSSF with cactus pretreated ranged from 0.41 and 0.44 g/g, 0.43 and 0.46 g/g, respectively. Fermentations carried out in bioreactors resulted in yields and ethanol production form 0.42 and 0.46 g/g and 7.62 and 12.42 g/L, respectively. The inhibitory compounds showed negative synergistic effects in fermentations performed by P. stipitis, Z. mobilis and S. cerevisiae. Formic acid and acetic acid showed most significant effects among the inhibitory compounds, followed by hydroxymethylfurfural, furfural and levulinic acid. Fermentations carried out in culture medium diluted with seawater showed promising results, especially for S. cerevisiae (0.50 g/g) and Z. mobilis (0.49 g/g). The different results obtained in this study indicate that lignocellulosic materials, pretreatments, fermentative processes strategies and the microorganisms studied deserve attention because they are promising and capable of being used in the context of biorefinery, aiming the ethanol production.

Influência dos parâmetros de processo na deposição de nitreto de titânio por plasma em gaiola catódica

Titanium nitride films were grown on glass using the Cathodic Cage Plasma Deposition technique in order to verify the influence of process parameters in optical and structural properties of the films. The plasma atmosphere used was a mixture of Ar, N2 and H2, setting the Ar and N2 gas flows at 4 and 3 sccm, respectively and H2 gas flow varied from 0, 1 to 2 sccm. The deposition process was monitored by Optical Emission Spectroscopy (OES) to investigate the influence of the active species in plasma. It was observed that increasing the H2 gas flow into the plasma the luminescent intensities associated to the species changed. In this case, the luminescence of N2 (391,4nm) species was not proportional to the increasing of the H2 gas into the reactor. Other parameters investigated were diameter and number of holes in the cage. The analysis by Grazing Incidence X-Ray Diffraction (GIXRD) confirmed that the obtained films are composed by TiN and they may have variations in the nitrogen amount into the crystal and in the crystallite size. The optical microscopy images provided information about the homogeneity of the films. The atomic force microscopy (AFM) results revealed some microstructural characteristics and surface roughness. The thickness was measured by ellipsometry. The optical properties such as transmittance and reflectance (they were measured by spectrophotometry) are very sensitive to changes in the crystal lattice of the material, chemical composition and film thicknesses. Therefore, such properties are appropriate tools for verification of this process control. In general, films obtained at 0 sccm of H2 gas flow present a higher transmittance. It can be attributed to the smaller crystalline size due to a higher amount of nitrogen in the TiN lattice. The films obtained at 1 and 2 sccm of H2 gas flow have a golden appearance and XRD pattern showed peaks characteristics of TiN with higher intensity and smaller FWHM (Full Width at Half Maximum) parameter. It suggests that the hydrogen presence in the plasma makes the films more stoichiometric and becomes it more crystalline. It was observed that with higher number of holes in the lid of the cage, close to the region between the lid and the sample and the smaller diameter of the hole, the deposited film is thicker, which is justified by the most probability of plasma species reach effectively the sample and it promotes the growth of the film