Síntese, caracterização e cinética da decomposição térmica dos materiais cerâmicos PrMO3 (M = Ni ou Co)

In this work have been studied the preparation, characterization and kinetic study of decomposition of the polymerizing agent used in the synthesis under non-isothermal condition ceramics PrMO3 of general formula (M = Co and Ni). These materials were obtained starting from the respective metal nitrates, as a cations source, and making use of gelatin as polymerizing agent. The powders were calcined at temperatures of 500°C, 700°C and 900°C and characterized by X-ray Diffraction (XRD), Thermogravimetric Analysis (TG / DTG/ DTA), Infrared Spectroscopy (FTIR), Temperature Programmed Reduction (TPR) and Scanning Electron Microscopy (SEM). The perovskite phase was detected in all the X-rays patterns. In the infrared spectroscopy observed the oxide formation as the calcination temperature increases with the appearance of the band metal - oxygen. The images of SEM revealed uniform distribution for the PrCoO3 and particles agglomerated as consequence of particle size for PrNiO3. From the data of thermal analysis, the kinetics of decomposition of organic matter was employed using the kinetics methods called Model Free Kinetics and Flynn and Wall, in the heating ratios 10, 20 and 30° C.min-1 between room temperature and 700°C. Finally, been obtained the values of activation energy for the region of greatest decomposition of organic matter in samples that were determined by the degree of conversion (α)

Síntese de nanopartículas de magnetita via decomposição térmica em meio não-aquoso

This work aims at obtaining nanoparticles of iron oxide, the magnetite one (Fe3O4), via synthesis by thermal decomposition through polyol. Thus, two routes were evaluated: a simple decomposition route assisted by reflux and a hydrothermal route both without synthetic air atmosphere using a synthesis temperature of 260ºC. In this work observed the influence of the observe of surfactants which are generally applied in the synthesis of iron oxide nanoparticles decreasing cluster areas. Further, was observed pure magnetite phase without secondary phases generally found in the iron oxide synthesis, a better control of crystallite size, morphology, crystal structure and magnetic behavior. Finally, the introduction of hydroxyl groups on the nanoparticles surface was analyzed besides its employment in the polymer production with OH radicals. The obtained materials were characterized by XRD, DLS, VSM, TEM, TG and DSC analyses. The results for the magnetite obtainment with a particle size greater than 5 nm and smaller than 11 nm, well defined morphology and good magnetic properties with superparamagnetic behavior. The reflux synthesis was more efficient in the deposition of the hydroxyl groups on the nanoparticles surface

Atenuação de ruídos coerentes utilizando decomposição em modos empíricos

The seismic processing technique has the main objective to provide adequate picture of geological structures from subsurface of sedimentary basins. Among the key steps of this process is the enhancement of seismic reflections by filtering unwanted signals, called seismic noise, the improvement of signals of interest and the application of imaging procedures. The seismic noise may appear random or coherent. This dissertation will present a technique to attenuate coherent noise, such as ground roll and multiple reflections, based on Empirical Mode Decomposition method. This method will be applied to decompose the seismic trace into Intrinsic Mode Functions. These functions have the properties of being symmetric, with local mean equals zero and the same number of zero-crossing and extremes. The developed technique was tested on synthetic and real data, and the results were considered encouraging

Produção, acúmulo e decomposição da serrapilhadeira e repartição da precipitação pluviométrica por espécies da caatinga

This study aimed to establish patterns of dynamics of litter and redistribution of rainfall of Caatinga vegetation. Sampling was done monthly for twenty three months in four areas: degraded, successional primary stage, secondary stage and late stage. We installed 72 collectors of 1.0 mx 1.0 m, with nylon fabric background in three areas. Litter deposited was fractionated into leaves, twigs, reproductive structures and miscellaneous, dried and weighed. To assess the stock of accumulated litter we used metal frame with dimensions of 0.5 mx 0.5 m, thrown randomly and collected monthly, taken to the laboratory for oven drying and weighed. To evaluate the decomposition, 40g of litter were placed in nylon bags (litterbags) mesh 1 mm ², dimensions 20.0 x 20.0 cm, being distributed on the soil surface and removed monthly, cleaned, dried and weighed. To evaluate the contribution of rainfall we used interceptometers installed 1.0 m above the ground surface, distributed under the canopy of six species of the caatinga, which evaluated the stemflow through collecting system installed around the stems of these species. The deposition of litter in the primary stage was 2.631,26 kg ha-1; 3.144,89 kg ha-1 in the secondary stage; 3.144,89 kg ha-1 in the late stage. The fraction of leaves was the largest contributor to the formation of litter in three stages. The degraded area showed greater accumulation of litter and decomposition has been sluggish during the dry period. We conclude that occurred greater litterfall in later stages. The late successional stage showed faster decomposition of litter, the evidence that is a better use of litter in nutrient cycling processes and incorporation of organic matter to the soil. The time required to decompose 50 % of the litter in the later stages of succession was lower indicating greater speed of release and reuse of nutrients by the vegetation. The specie jurema preta with less leaf area and consists of leaflets, showed greater internal precipitation in rain events of greater magnitude. The stemflow was not influenced by DAP and basal area. The water lost by trapping represented the largest proportion of total rainfall in all species studied

Determinantes locais da decomposição foliar e de raízes finais em um ecossistema semiárido do nordeste brasileiro

The decomposition process exercises an extensive control over the carbon cycle, affecting its availability and nutrient cycling in terrestrial ecosystems. The understanding of leaf decomposition patterns above the soil and fine roots decomposition below the soil is necessary and essential to identify and quantify more accurately the flow of energy and matter in forest systems. There is still a lack of studies and a large gap in the knowledge about what environmental variables act as local determinants over decomposition drivers. The knowledge about the decomposition process is still immature for Brazilian semiarid region. The aim of this study was to analyze the decomposition process (on leaves and fine roots) of a mixture of three native species for 12 months in a semiarid ecosystem in Northeast Brazil. We also examined whether the rate of decomposition can be explained by local environmental factors, specifically plant species richness, plant density and biomass, soil macro-arthropods species richness and abundance, amount of litterfall and fine root stock. Thirty sampling points were randomly distributed within an area of 2000 m x 500 m. To determine the decomposition rate, the litterbag technique was used and the data analysis were made with multiple regressions. There was a high degradation of dead organic matter along the experiment. Above ground plant biomass was the only environmental local factor significantly related to leaf decomposition. The density of vegetation and litter production were positively and negatively related to decay rates of fine roots, respectively. The results suggest that Caatinga spatial heterogeneity may exert strong influences over the decomposition process, taking into account the action of environmental factors related to organic matter exposure of and the consequent action of solar radiation as the decomposition process main controller in this region

Efeitos individuais e interativos da diversidade de detritos, contexto e variabilidade ambiental sobre a magnitude e estabilidade do processo de decomposição

Studies on the effects of changes in biodiversity and ecosystem functioning have been a central theme in ecology over the past two decades. Several studies have showed that the diversity of plant debris differently affects the decomposition process in aquatic and terrestrial environments, but we know very about the effects of detritus diversity on decomposition under fluctuating environmental conditions. We tested whether and how the environmental contexts, as well as the dynamic of their alternation, influence the effects of detritus diversity on the decomposition process. We performed a field experiment where we manipulate the litter diversity of 8 species of terrestrial plants decomposing (litterbags) in single and in mixture containing the eight species together in three different environmental contexts: the terrestrial environment (T), aquatic (A) and interface (I) - experimental treatment that simulates variation in flooding regime. We measured the rate of decomposition through the loss of mass of the community and each individual detritus in monocultures and mixtures. Species richness and environmental variability had no effects on the magnitude and stability of the decomposition process. However, there were significant diversity effects on the decomposition of an individual alien species, F. benjamina. Environmental context had significant effects on the magnitude and variability of decomposition. Detritus decomposition was faster and more variable on aquatic, interface and terrestrial conditions, respectively. Our results demonstrate that the diversity of plant detritus has minor effects to the decomposition across disparate environmental conditions and suggest that it is necessary to consider the potential of other abiotic factors in affect the magnitude and variability of the decomposition processes

Análise estatística de padrões sísmicos: decomposição em multiescala

O processamento de registros sísmicos é uma tarefa muito importante dentro da Geofísica e que representa um desafio permanente na exploração de petróleo. Embora esses sinais forneçam uma imagem adequada da estrutura geológica do subsolo, eles são contaminados por ruídos e, o ground roll é a componente principal. Este fato exige um esforço grande para o desenvolvimento de metodologias para filtragem, Dentro desse contexto, este trabalho tem como objetivo apresentar um método de remoção do ruído ground roll fazendo uso de ferramentas da Física Estatística. No método, a Análise em Ondeletas é combinada com a Transformada de Karhunen-Loève para a remoção em uma região bem localizada. O processo de filtragem começa com a Decomposição em Multiescala. Essa técnica permite uma representação em tempo-escala fazendo uso das ondeletas discretas implementadas a filtros de reconstrução perfeita. O padrão sísmico original fica representado em multipadrões: um por escala. Assim, pode-se atenuar o ground roll como uma operação cirúrgica em cada escala, somente na região onde sua presença é forte, permitindo preservar o máximo de informações relevantes. A atenuação é realizada pela definição de um fator de atenuação Af. Sua escolha é feita pelo comportamento dos modos de energia da Transformada de Karhunen-Loève. O ponto correspondendo a um mínimo de energia do primeiro modo é identificado como um fator de atenuação ótimo

Síntese e Caracterização de Titanatos de Cobalto e Níquel, dopados com Praseodímio, obtidos a partir da decomposição de Nitrilotriacetatos

In recent years, studies about the physicochemical properties of mixed oxides, call attention of the scientific community, properties like as piezoelectricity, photoluminescence, or applications as catalysts, arise in these compounds, when their chemical compositions are modified, in this context some routes are employed in the synthesis of these materials, among which can be cited these methods: ceramic, combustion, co-precipitation, Pechini or polymeric precursor method, hydrothermal, sol-gel; these routes are divided into traditional routes or chemical routes. In this work were synthesized oxides with variable composition, from the thermal decomposition of titanium, cobalt, nickel and praseodymium nitrilotriacetates. The nitrilotriacetates were characterized by IR Spectroscopy (FTIR), Thermogravimetric (TG/ DTG) and Differential Scanning Calorimetry (DSC), while oxides have been characterized by X-ray diffraction (XRD), Spectrofluorimetry and IR Spectroscopy (FTIR). From FTIR data, it was demonstrated that the displacement of the band corresponding to the carboxylate group (νCOOH) at 1712 cm-1, present in nitrilotriacetic acid (H3NTA), for 1680-1545 cm-1, these stretches are characteristics of coordinated nitrilotriacetates, By thermal analysis (TG/DTG /DSC), it was suggested, that in an oxidizing atmosphere (air) oxides are obtained at lower temperatures than in an inert atmosphere N2(g). By results from X-ray Diffraction (XRD), it was determinated that the oxides are crystalline and the predominant phases obtained are summarized titanate phases rutile and ilmenite. By fluorimetry was observed that the intensity of emission bands are directly proportional to the concentration of ions Ni2+, Co2+ and Pr3+, and IR spectroscopy (FTIR) from oxides, demonstrated the disappearance of characteristic bands by nitrilotriacetates, determining the complete decomposition of the nitrilotriacetates in oxides

Síntese, caracterização e cinética da decomposição térmica dos materiais cerâmicos PrMO3 (M = Ni ou Co)

In this work have been studied the preparation, characterization and kinetic study of decomposition of the polymerizing agent used in the synthesis under non-isothermal condition ceramics PrMO3 of general formula (M = Co and Ni). These materials were obtained starting from the respective metal nitrates, as a cations source, and making use of gelatin as polymerizing agent. The powders were calcined at temperatures of 500°C, 700°C and 900°C and characterized by X-ray Diffraction (XRD), Thermogravimetric Analysis (TG / DTG/ DTA), Infrared Spectroscopy (FTIR), Temperature Programmed Reduction (TPR) and Scanning Electron Microscopy (SEM). The perovskite phase was detected in all the X-rays patterns. In the infrared spectroscopy observed the oxide formation as the calcination temperature increases with the appearance of the band metal - oxygen. The images of SEM revealed uniform distribution for the PrCoO3 and particles agglomerated as consequence of particle size for PrNiO3. From the data of thermal analysis, the kinetics of decomposition of organic matter was employed using the kinetics methods called Model Free Kinetics and Flynn and Wall, in the heating ratios 10, 20 and 30° C.min-1 between room temperature and 700°C. Finally, been obtained the values of activation energy for the region of greatest decomposition of organic matter in samples that were determined by the degree of conversion (α)

Síntese de nanopartículas de magnetita via decomposição térmica em meio não-aquoso

This work aims at obtaining nanoparticles of iron oxide, the magnetite one (Fe3O4), via synthesis by thermal decomposition through polyol. Thus, two routes were evaluated: a simple decomposition route assisted by reflux and a hydrothermal route both without synthetic air atmosphere using a synthesis temperature of 260ºC. In this work observed the influence of the observe of surfactants which are generally applied in the synthesis of iron oxide nanoparticles decreasing cluster areas. Further, was observed pure magnetite phase without secondary phases generally found in the iron oxide synthesis, a better control of crystallite size, morphology, crystal structure and magnetic behavior. Finally, the introduction of hydroxyl groups on the nanoparticles surface was analyzed besides its employment in the polymer production with OH radicals. The obtained materials were characterized by XRD, DLS, VSM, TEM, TG and DSC analyses. The results for the magnetite obtainment with a particle size greater than 5 nm and smaller than 11 nm, well defined morphology and good magnetic properties with superparamagnetic behavior. The reflux synthesis was more efficient in the deposition of the hydroxyl groups on the nanoparticles surface

Atenuação de ruídos coerentes utilizando decomposição em modos empíricos

The seismic processing technique has the main objective to provide adequate picture of geological structures from subsurface of sedimentary basins. Among the key steps of this process is the enhancement of seismic reflections by filtering unwanted signals, called seismic noise, the improvement of signals of interest and the application of imaging procedures. The seismic noise may appear random or coherent. This dissertation will present a technique to attenuate coherent noise, such as ground roll and multiple reflections, based on Empirical Mode Decomposition method. This method will be applied to decompose the seismic trace into Intrinsic Mode Functions. These functions have the properties of being symmetric, with local mean equals zero and the same number of zero-crossing and extremes. The developed technique was tested on synthetic and real data, and the results were considered encouraging

Avaliação da ecotoxicidade de percolados em áreas de disposição de resíduos na região metropolitana de Natal/RN

Leachates are effluent produced by decomposition of solid waste, they have complex composition and can be highly toxic. Therefore such percolated liquid should be collected and treated properly to avoid environmental contamination of soil and of water bodies. The objective of this study was to evaluate the toxicity through ecotoxicological tests with Ceriodaphnia dubia (Cladocera - Crustacea) of percolated liquids generated in two different systems of municipal solid waste (MSW) disposal in the city of Natal/ RN: A Sanitary Landfill in the Metropolitan Region of Natal/ RN, and in a dump off area. Furthermore, it was evaluated the possible contamination of the underground water of the dump off area. Two monthly samples were taken at four points between the months of May/2009 and January/2010. The Point "A" corresponds to the end of the pond leachate treatment in ASRMN; The Point "B" corresponds to a containment pond at the dump. The Point "C" is an area near one of the cells of the dump off area where the leachate outcrops; The Point "D" stands for an underground water well at the area. The last point, called "E" was sampled only once and corresponds to the slurry produced by temporary accumulation of solid waste in the open area of the dump. The ecotoxicological tests, acute and chronic, followed the ABNT 13373/2005 rules, with some modifications. The samples were characterized by measuring the pH number, the dissolved oxygen (DO), the salinity, BOD5, COD, Cd, Cu, Pb, Cr, Fe, Mg, Ni, and Zn. At Point A, the average number of EC50-48h ranged between 1.0% and 2.77% (v/v), showing a high toxicity of the leachate to C.dubia in all months. To this point, positive correlations were found between the EC50- 48 with precipitation. Negative correlations were found between the EC50- 48h with salinity. At point B there was no response of the acute exposure of organisms to the test samples. At point C the EC50-48h ranged from 17.68% to 35.36% in just two months of the five ones analyzed, not correlated meaning. Point D, the EC50-48h level ranged between 12.31% and 71.27%, showed a negative correlation with, only, precipitation. Although it was observed toxicity of underground water in the Landfill Area, there was no evidence of water contamination by leachate, however, due to the toxic character of this water, additional tests should be conducted to confirm the quality of water that is used for human supply. At point E there was no acute toxicity. These results support the dangers of inappropriate disposal of MSW to water bodies due to the high toxicity of the leachate produced highlighting the necessity of places of safe confinement and a treatment system more effective to it

Síntese, estudo cinético e análise microestrutural do sistema cério-níquel obtido pelo método pechini

The cerium oxide has a high potential for use in removing pollutants after combustion, removal of organic matter in waste water and the fuel-cell technology. The nickel oxide is an attractive material due to its excellent chemical stability and their optical properties, electrical and magnetic. In this work, CeO2-NiO- systems on molars reasons 1:1(I), 1:2(II) e 1:3(III) metal-citric acid were synthesized using the Pechini method. We used techniques of TG / DTG and ATD to monitor the degradation process of organic matter to the formation of the oxide. By thermogravimetric analysis and applying the dynamic method proposed by Coats-Redfern, it was possible to study the reactions of thermal decomposition in order to propose the possible mechanism by which the reaction takes place, as well as the determination of kinetic parameters as activation energy, Ea, pre-exponential factor and parameters of activation. It was observed that both variables exert a significant influence on the formation of complex polymeric precursor. The model that best fitted the experimental data in the dynamic mode was R3, which consists of nuclear growth, which formed the nuclei grow to a continuous reaction interface, it proposes a spherical symmetry (order 2 / 3). The values of enthalpy of activation of the system showed that the reaction in the state of transition is exothermic. The variables of composition, together with the variable temperature of calcination were studied by different techniques such as XRD, IV and SEM. Also a study was conducted microstructure by the Rietveld method, the calculation routine was developed to run the package program FullProf Suite, and analyzed by pseudo-Voigt function. It was found that the molar ratio of variable metal-citric acid in the system CeO2-NiO (I), (II), (III) has strong influence on the microstructural properties, size of crystallites and microstrain network, and can be used to control these properties

Síntese e caracterização de catalisadores nanométricos de LaSrNiO4 para aplicação em dessulfurização de tiofeno

The mixed metal oxides constitute an important class of catalytic materials widely investigated in different fields of applications. Studies of rare earth nickelates have been carried by several researchers in order to investigate the structural stability afforded by oxide formed and the existence of catalytic properties at room temperature. So, this study aims synthesize the nanosized catalyst of nickelate of lanthanum doped with strontium (La(1-x)SrxNiO4-d; x = 0,2 and 0,3), through the Pechini method and your characterization for subsequent application in the desulfurization of thiophene reaction. The precursor solutions were calcined at 300ºC/2h for pyrolysis of polyester and later calcinations occurred at temperatures of 500 - 1000°C. The resulting powders were characterized by thermogravimetric analysis (TG / DTG), surface area for adsorption of N2 by BET method, X-ray diffraction (XRD), scanning electron microscopy (HR_SEM) and spectrometry dispersive energy (EDS). The results of XRD had show that the perovskites obtained consist of two phases (LSN and NiO) and from 700ºC have crystalline structure. The results of SEM evidenced the obtainment of nanometric powders. The results of BET show that the powders have surface area within the range used in catalysis (5-50m2/g). The characterization of active sites was performed by reaction of desulfurization of thiophene at room temperature and 200ºC, the relation F/W equal to 0,7 mol h-1mcat -1. The products of the reaction were separated by gas chromatography and identified by the selective detection PFPD sulfur. All samples had presented conversion above 95%

Desenvolvimento e caracterização de compósitos poli(tereftalato de etileno) reciclado (PET reciclado) com flocos de vidro.

The growing concern with the solid residues management, observed in the last decade, due to its huge amount and impact, has motivated the search for recycling processes, where these residues can be reprocessed to generate new products, enlarging the cycle of materials and energy which are present. Among the polymeric residues, there is poly (ethylene terephthalate) (PET). PET is used in food packaging, preferably in the bottling of carbonated beverages. The reintegration of post-consumer PET in half can be considered a productive action mitigation of environmental impacts caused by these wastes and it is done through the preparation of several different products at the origin, i.e. food packaging, with recycling rates increasing to each year. This work focused on the development and characterization mechanical, thermal, thermo-mechanical, dynamic mechanical thermal and morphology of the pure recycled PET and recycled PET composites with glass flakes in the weight fraction of 5%, 10% and 20% processed in a single screw extruder, using the following analytical techniques: thermogravimetry (TG), differential scanning calorimetry (DSC), tensile, Izod impact, Rockwell hardness, Vicat softening temperature, melt flow rate, burn rate, dynamic mechanical thermal analysis (DMTA) and scanning electron microscopy (SEM). The results of thermal analysis and mechanical properties leading to a positive evaluation, because in the thermograms the addition of glass flakes showed increasing behavior in the initial temperatures of thermal decomposition and melting crystalline, Furthermore was observed growing behavior in the mechanical performance of polymer composites, whose morphological structure was observed by SEM, verifying a good distribution of glass flakes, showing difference orientation in the center and in the surface layer of test body of composites with 10 and 20% of glass flakes. The results of DMTA Tg values of the composites obtained from the peak of tan ä showed little reductions due to poor interfacial adhesion between PET and recycled glass flakes.