Radiação gama e atmosfera modificada passiva na qualidade de goiabas 'Pedro Sato'

O objetivo deste trabalho foi avaliar o efeito da irradiação gama associada à atmosfera modificada passiva na qualidade pós-colheita de goiabas 'Pedro Sato', verificando suas características físico-químicas. Foram utilizadas goiabas provenientes da região de Vista Alegre do Alto-SP,Brasil. Após a colheita, as goiabas foram imediatamente transportadas ao Laboratório de Frutas e Hortaliças, pertencente ao Departamento de Gestão e Tecnologia Agroindustrial, da Faculdade de Ciências Agronômicas - UNESP - Câmpus de Botucatu-SP, onde foram armazenadas a 10ºC e 90-95%UR, em câmara frigorífica, por 28 dias. Os tratamentos foram: controle 1 (sem embalagem e sem irradiação); controle 2 (embalagem de poliestireno (PS) + polietileno de baixa densidade (PEBD) e sem irradiação); tratamento 1 (PS+PEBD e 0,2kGy); tratamento 2 (PS+PEBD e 0,6kGy), e tratamento 3 (PS+PEBD e 1,0kGy). As análises realizadas foram: firmeza, sólidos solúveis (SS), acidez titulável (AT) e índice de maturação. Foi utilizado o delineamento inteiramente casualizado, com esquema fatorial 5 x 5 (tratamento x tempo). Concluiu-se que as altas doses de irradiação promoveram efeito negativo nas características físico-químicas da goiaba 'Pedro Sato', e que apenas a menor dose utilizada (0,2kGy) associada à atmosfera modificada conservou frutos com maior qualidade e aceitabilidade, indicado por maiores índice de maturação e teor de sólidos solúveis obtidos.

Síntese e caracterização do carbeto de molibdênio nanoestruturado para fins catalíticos na reação de oxidação parcial do metano

The nanostructures materials are characterized to have particle size smaller than 100 nm and could reach 1 nm. Due to the extremely reduced dimensions of the grains, the properties of these materials are significantly modified relatively when compared with the conventional materials. In the present work was accomplished a study and characterization of the molybdenum carbide, seeking obtain it with particles size in the nanometers order and evaluate its potential as catalyst in the reaction of partial methane oxidation. The method used for obtaining the molybdenum carbide was starting from the precursor ammonium heptamolybdate of that was developed in split into two oven, in reactor of fixed bed, with at a heating rate of 5ºC/min, in a flow of methane and hydrogen whose flow was of 15L/h with 5% of methane for all of the samples. The studied temperatures were 350, 500, 600, 650, 660, 675 and 700ºC and were conducted for 0, 60, 120 and 180 minutes, and the percent amount and the crystallite size of the intermediate phases were determined by the Rietveld refinement method. The carbide obtained at 660ºC for 3 hours of reaction showed the best results, 24 nm. Certain the best synthesis condition, a passivating study was accomplished, in these conditions, to verify the stability of the carbide when exposed to the air. The molybdenum carbide was characterized by SEM, TEM, elemental analysis, ICP-AES, TG in atmosphere of hydrogen and TPR. Through the elemental analysis and ICP-AES the presence carbon load was verified. TG in atmosphere of hydrogen proved that is necessary the passivating of the molybdenum carbide, because occur oxidation in room temperature. The catalytic test was accomplished in the plant of Fischer-Tropsch of CTGAS, that is composed of a reactor of fixed bed. Already the catalytic test showed that the carbide presents activity for partial oxidation, but the operational conditions should be adjusted to improve the conversion

Desenvolvimento de uma unidade laboratorial para quantificação de BTX como poluentes atmosféricos, usando microextração em fase sólida

This dissertation aims the development of an experimental device to determine quantitatively the content of benzene, toluene and xylenes (BTX) in the atmosphere. BTX are extremely volatile solvents, and therefore play an important role in atmospheric chemistry, being precursors in the tropospheric ozone formation. In this work a BTX new standard gas was produced in nitrogen for stagnant systems. The aim of this dissertation is to develop a new method, simple and cheaper, to quantify and monitor BTX in air using solid phase microextraction/ gas chromatography/mass spectrometry (SPME/CG/MS). The features of the calibration method proposed are presented in this dissertation. SPME sampling was carried out under non-equilibrium conditions using a Carboxen/PDMS fiber exposed for 10 min standard gas mixtures. It is observed that the main parameters that affect the extraction process are sampling time and concentration. The results of the BTX multicomponent system studied have shown a linear and a nonlinear range. In the non-linear range, it is remarkable the effect of competition by selective adsorption with the following affinity order p-xylene > toluene > benzene. This behavior represents a limitation of the method, however being in accordance with the literature. Furthermore, this behavior does not prevent the application of the technique out of the non-linear region to quantify the BTX contents in the atmosphere.

Novas alternativas de remoção de enxofre do óleo diesel utilizando tensoativos e microemulsões

The diesel combustion form sulfur oxides that can be discharged into the atmosphere as particulates and primary pollutants, SO2and SO3, causing great damage to the environment and to human health. These products can be transformed into acids in the combustion chamber, causing damage to the engines. The worldwide concern with a clean and healthy environment has led to more restrictive laws and regulations regulating the emission levels of pollutants in the air, establishing sulfur levels increasingly low on fuels. The conventional methods for sulfur removal from diesel are expensive and do not produce a zero-level sulfur fuel. This work aims to develop new methods of removing sulfur from commercial diesel using surfactants and microemulsion systems. Its main purpose is to create new technologies and add economic viability to the process. First, a preliminary study using as extracting agent a Winsor I microemulsion system with dodecyl ammonium chloride (DDACl) and nonyl phenol ethoxylated (RNX95) as surfactant was performed to choose the surfactant. The RNX95 was chosen to be used as surfactant in microemulsioned systems for adsorbent surface modification and as an extracting agent in liquid-liquid extraction. Vermiculite was evaluated as adsorbent. The microemulsion systems applied for vermiculite surface modification were composed by RNX95 (surfactant), n-butanol (cosurfactant), n-hexane (oil phase), and different aqueous phases, including: distilled water (aqueous phase),20ppm CaCl2solution, and 1500ppm CaCl2solution. Batch and column adsorption tests were carried out to estimate the ability of vermiculite to adsorb sulfur from diesel. It was used in the experiments a commercial diesel fuel with 1,233ppm initial sulfur concentration. The batch experiments were performed according to a factorial design (23). Two experimental sets were accomplished: the first one applying 1:2 vermiculite to diesel ratio and the second one using 1:5 vermiculite to diesel ratio. It was evaluated the effects of temperature (25°C and 60°C), concentration of CaCl2in the aqueous phase (20ppm and 1500ppm), and vermiculite granule size (65 and 100 mesh). The experimental response was the ability of vermiculite to adsorb sulfur. The best results for both 1:5 and 1:2 ratios were obtained using 60°C, 1500ppm CaCl2solution, and 65 mesh. The best adsorption capacities for 1:5 ratio and for 1:2 ratio were 4.24 mg sulfur/g adsorbent and 2.87 mg sulfur/g adsorbent, respectively. It was verified that the most significant factor was the concentration of the CaCl2 solution. Liquid-liquid extraction experiments were performed in two and six steps using the same surfactant to diesel ratio. It was obtained 46.8% sulfur removal in two-step experiment and 73.15% in six-step one. An alternative study, for comparison purposes, was made using bentonite and diatomite asadsorbents. The batch experiments were done using microemulsion systems with the same aqueous phases evaluated in vermiculite study and also 20ppm and 1500 ppm BaCl2 solutions. For bentonite, the best adsorption capacity was 7.53mg sulfur/g adsorbent with distilled water as aqueous phase of the microemulsion system and for diatomite the best result was 17.04 mg sulfur/g adsorbent using a 20ppm CaCl2solution. The accomplishment of this study allowed us to conclude that, among the alternatives tested, the adsorption process using adsorbents modified by microemulsion systems was considered the best process for sulfur removal from diesel fuel. The optimization and scale upof the process constitutes a viable alternative to achieve the needs of the market

Variação da qualidade da água de chuva no início da precipitação

One of the most evident and actual concern, not only in the scientific means, but also of the public knowledge in general, is the lack problem of the potable water, that come increasing more each time, motivated mainly for the po llution of the sources, the bad use of the water and the increase of the population. In such a way, the necessity of looking for new water sources and the development of techniques to use sources minus explored is becoming even more important and urgent. T he rainwater comes being used since a long time like a supplying source, but, due the few knowledge of its characteristics, the generated preconception and the discrimination around its consumption and to the bad use of the technique of collection and stor age, it comes being little used, wasting consequently a significant parcel of this source. Trying to develop the knowing of some characteristics of the rainwater, the present work looks for to define the curve of variation of the quality of the rainwater i n three points with distinct characteristics of the city of Natal -RN, in the course of the precipitation, in some situations of time and space. For describe the curve of variation of the water s quality, some variables must be analyzed, and to be identifie d when they modify themselves in the endurance of rain, showing in which moment the purification of the water is more or less quickly. The pH, the Turbidity and the Electric Conductivity can be related with a big part of the physicist -chemistries variables found in the water and, like its analyses don't spend any material, they have easy access and measurement. The present work analyzes the curves of decline of these three variables, in three points with distinct characteristics in the city of Natal -RN, being these points: one next to the sea, another one in region with great buildings concentration and the last point in a less polluted area. For the studied region, it was during the five first millimeters of rain that occurs the biggest reduction of the exi sting impurities in the atmosphere, mainly between the first and the second millimeter, and after the five first millimeters the values of the variables stabilize. With exception of the University Campus, where initially the rainwater already has very good quality, the values of Turbidity and Electric Conductivity suffer a brusque reduction after the first millimeter of rain

Sobre a natureza dos processos físicos de aquecimento da atmosfera de estrelas do tipo solar

In the present work, we have studied the nature of the physical processes of the coronal heating, considering as basis significant samples of single and binary evolved stars, that have been achieved with the ROSAT satellite. In a total of 191 simple stars were studied, classified in the literature as giants with spectral type F, G and K. The results were compared with those obtained from 106 evolved stars of spectral type F, G and K, which belong to the spectroscopic binary systems. Accurate measurements on rotation and information about binarity were obtained from De Medeiros s catalog. We have analysed the behavior of the coronal activity in function of diverse stellar parameters. With the purpose to better clarify the profile of the stars evolution, the HR diagram was built for the two samples of stars, the single and the binary ones. The evolved traces added in the diagram were obtained from the Toulouse-Geneve code, Nascimento et al. (2000). The stars were segregated in this diagram not only in range of rotational speed but also in range of X-ray flux. Our analysis shows clearly that the single stars and the binary ones have coronal activity controlled by physical process independent on the rotation. Non magnetic processes seem to be strongly influencing the coronal heating. For the binary stars, we have also studied the behavior of the coronal emission as a function of orbital parameters, such as period and eccentricity, in which it was revealed the existence of a discontinuity in the emission of X-rays around an orbital period of 100 days. The study helped to conclude that circular orbits of the binary stars are presented as a necessary property for the existence of a higher level ofX-rays emission, suggesting that the effect of the gravitational tide has an important role in the coronal activity level. When applied the Kolmogorov-Smirnov test (KS test ) for the Vsini and FX parameters to the samples of single and binary stars, we could evidence very relevant aspects for the understanding of the mechanisms inherent to the coronal activity. For the Vsini parameter, the differences between the single stars and the binary ones for rotation over 6.3 km/s were really remarkable. We believe, therefore, that the existence of gravitational tide is, at least, one of the factors that most contribute for this behavior. About the X-rays flux, the KS test showed that the behavior of the single and the binary stars, regarding the coronal activity, comes from the same origin

Processos de aquecimento na alta atmosfera estelar: emissão coronal em raio-x e emissão cromosférica em CaII

In the present work we study the processes of heating in the high stellar atmosphere, with base in an analysis of behavior of the cromospheric and coronal emission for a sample of single stars classified as giant in the literature. The evolutionary status of the stars of the sample was determined from HIPPARCOS satellite trigonometric parallax measurements and from the Toulouse Genéve code. In this study we show the form of behavior of the CaII emission flux in spectral lines H and K F(CaII) and the X-ray emission flux in function of the rotation, number of Rossby Ro and depth in mass of the convective envelope. In this analysis we show that while the cromospheric activity is dominated clearly by a physical process of heating associated with the rotation, like a magnetic field produced by dynamo effect, the coronal activity seems to be influenced for a mechanism independent of the rotation. We show also that the effective role of the depth in massa of the convective envelope on the stellar activity has an important effect in the responsible physical process for the behavior of the activity in the atmosphere of the stars.

Síntese, sinterização e caracterização de ferritas à base de Ni-Zn

Were synthesized different ferrites NixZn1-xFe2O4 (0,4 ≤ x ≤ 0,6) compositions by using citrate precursor method. Initially, the precursors citrates of iron, nickel and zinc were mixed and homogenized. The stoichiometric compositions were calcined at 350°C without atmosphere control and the calcined powders were pressed in pellets and toroids. The pressed material was sintered from 1100º up to 1200ºC in argon atmosphere. The calcined powders were characterized by XRD, TGA/DTG, FTIR, SEM and vibrating sample magnetometer (VSM). All sintered samples were characterized using XRD, SEM, VSM and measurements of magnetic permeability and loss factor were obtained. It was formed pure ferromagnetic phase at all used temperatures. The Rietveld analyses allowed to calculate the cations level occupation and the crystallite size. The analyses obtained nanometric crystals (12-20 nm) to the calcined powder. By SEM, the sintered samples shows grains sizes from 1 to 10 μm. Sintered densities (ρ) were measured by the Archimedes method and with increasing Zn content, the bulk density decrease. The better magnetization results (105-110 emu/g) were obtained for x=0,6 at all sintering temperatures. The hysteresis shows characteristics of soft magnetic material. Two magnetization processes were considered, superparamagnetism at low temperature and the magnetic domains formation at high temperatures. The sintered toroids presents relative magnetic permeability (μr) from 7 to 32 and loss factor (tanδ) of about 1. The frequency response of toroids range from 0,3 kHz to 0,2 GHz. The composition x=0,5 presents both greater μr and tanδ values and x=0,6 the most broad range of frequency response. Various microstructural factors show influence on the behavior of μr and tanδ, such as: grain size, porosity across grain boundary and inside the grain, grain boundary content and domain walls movement during the process of magnetization at high frequency studies (0,3kKz 0,2 GHz)

Síntese análise das propriedades magnéticas da ferrita de NiMg e características de absorção de radiação

It was synthesized different Ni1-xMgxFe2O4 (0,2 ≤ x ≤ 0,7) compositions by use of citrate precursor method. Initially, the precursory citrates of iron, nickel and magnesium were mixed and homogenized. The stoichiometric compositions were calcined from 350°C to 1200°C at ambient atmosphere or in argon atmosphere. The calcined powders were characterized by XRD, TGA/DTG, FTIR, magnetic measures and reflectivity using the wave guide method. I was observed pure magnetic phase formation between 350°C and 500°C, with formation of ferrite and hematite after 600°C at ambient atmosphere. The calcined powder at argon atmosphere formed pure ferromagnetic phase at 1100°C and 1200°C. The Rietveld analyses calculated the cations level occupation and the crystallite size. The analyses obtained nanometric crystals (11-66 nm), that at 900°C/3h presents micrometric sizes (0,45 - 0,70 Om). The better magnetization results were 54 Am2/Kg for x= 0,2 composition, calcined at 350°C/3h and 30 min, and 55,6 Am2/Kg for x= 0,2 1200°C, calcined in argon. The hysteresis shows characteristics of soft magnetic material. Two magnetization processes were considered, superparamagnetism at low temperature and the magnetic domains formation at high temperatures. The materials presented absorption less or equal the 50 % in ranges specific frequency. As for the 2,0 and 3,0 thickness (in 11,0 - 11,8 GHz), the reflectivity of the x= 0,3, 0,5 and 0,4 compositions, all calcined at 900°C/3h showed agreement with MS and O. Various factors contribute for the final radiation absortion effect, such as, the particle size, the magnetization and the polymer characteristics in the MARE composition. The samples that presented better magnetization does not obtaining high radiation absorption. It is not clear the interrelaction between the magnetization and the radiation absorption in the strip of frequencies studied (8,2 - 12,4 GHz)

Síntese, caracterização e aplicação de MCM-41 funcionalizado com diisopropilamina no processo de adsorção do dióxido de carbono

Emissions of CO2 in the atmosphere have increased successively by various mechanisms caused by human action, especially as fossil fuel combustion and industrial chemical processes. This leads to the increase in average temperature in the atmosphere, which we call global warming. The search for new technologies to minimize environmental impacts arising from this phenomenon has been investigated. The capture of CO2 is one of the alternatives that can help reduce emis ions of greenhouse gases. The CO2 can be captured through the process of selective adsorption using adsorbents for this purpose. Were synthesized by hydrothermal method, materials of the type MCM-41 and Al-MCM-41 in the molar ratio Si / Al equal to 50. The synthesis of gels were prepared from a source of silicon, sodium, water and aluminum in the case of Al-MCM-41. The period of synthesis of the materials was 5 days in autoclave at 100°C. After that time materials were filtered, washed and dried in greenhouse at 100 º C for 4 hours and then calcined at 450 º C. Then the calcined material was functionalized with the Di-isopropylamine (DIPA) by the method of wet impregnation. We used 0.5 g of material mesopores to 3.5 mL of DIPA. The materials were functionalized in a closed container for 24 hours, and after this period were dried at brackground temperature for 2 hours. Were subsequently subjected to heat treatment at 250°C for 1 hour. These materials were used for the adsorption of CO2 and were characterized by XRD, FT-IR, BET / BJH, SEM, EDX and TG / DTG. Tests of adsorption of CO2 was carried out under the following conditions: 100 mg of adsorbent, temperature of 75°C under flow of 100 mL/min of CO2 for 2 hours. The desorption of CO2 was carried out by thermogravimetry from ambient temperature to 900ºC under flow of 25 mL min of He and a ratio of 10ºC/min. The difratogramas X-ray for the synthesized samples showed the characteristic peaks of MCM-41, showing that the structure of it was obtained. For samples functionalized there was a decrease of the intensities of these peaks, with a consequent reduction in the structural ordering of the material. However, the structure was preserved mesopores. The adsorption tests showed that the functionalized MCM-41 is presented as a material promising adsorbent, for CO2 capture, with a loss of mass on the desorption CO2 of 7,52%, while that in Al-MCM- 41 functionalized showed no such loss

Estudo termoanalítico da perlita hidrofobizada com óleo de linhaça

In this work, expanded perlite, a mineral clay, consisting of SiO2 and Al2O3 in the proportions of 72.1 and 18.5%, respectively, was used as an adsorbent for oil in its pure expanded form as well as hydrofobized with linseed oil. Thermogravimetry (TG), Derivative Thermogravimetry (DTG) and Differential Thermal Analysis (DTA) were used to study the thermal behavior and quantify the percent adsorption of perlite in differents processes comparing the results with the ones obtained using Gravimetric Analysis. In the process of hydrophobization with linseed oil granulometric fractions > 20, 20-32 and 32-60 mesh were used and adsorption tests with crude oil were performed in triplicate at room temperature. The results obtained by TG/DTG in dynamic atmosphere of air showed mass losses in a single step for the expanded perlite with pure adsorbed oil, indicating that the adsorption of oil was limited and that the particle size did not in this process. Linseed oil has performed well as an agent of hydrophobized perlite (32 to 60 mesh) indicating a maximum percentage of 59.9% and 68.6% the linseed with a fraction range from considering the data obtained by thermogravimetry and Gravimetry, respectively. The adsorption of oil in the expanded perlite and hydrofobized pure perlite with linseed oil did not produce good results, characterizing an increase of 0.5 to 4.6% in pure perlite and 3.3% in hydrofobized perlite with granulometric 32 to 60 mesh

Determinação do teor de cálcio através da termogravimetria, em medicamentos utilizados no tratamento da osteoporose: um estudo comparativo

The present study utilized the thermogravimetry (TG) and optical emission spectroscopy with inductively coupled plasma - ICP / OES to determine the calcium content in tablets of carbonate, citrate and calcium lactate used in the treatment of osteoporosis. The samples were characterized by IR, SEM, TG / DTG, DTA, DSC and XRD. The thermal analysis evaluated the thermal stability and physical-chemical events and showed that the excipients influence the decomposition of active ingredients. The results of thermogravimetry indicated that the decomposition temperature of the active CaCO3 (T = 630.2 °C) is lower compared to that obtained in samples of the tablets (633.4 to 655.2 °C) except for sample AM 2 (Ti = 613.8 oC). In 500.0 °C in the samples of citrate and calcium lactate, as well as their respective active principles had already been formed calcium carbonate. The use of N2 atmosphere resulted in shifting the initial and final temperature related to the decomposition of CaCO3. In the DTA and DSC curves were observed endo and exothermic events for the samples of tablets and active ingredients studied. The infrared spectra identified the main functional groups in all samples of active ingredients, excipients and tablets studied, such as symmetric and asymmetric stretches of the groups OH, CH, C = O. Analysis by X-ray diffraction showed that all samples are crystalline and that the final residue showed peaks indicative of the presence of calcium hydroxide by the reaction of calcium oxide with moisture of the air. Although the samples AM 1, AM 2, AM 3 and AM 6 in their formulations have TiO2 and SiO2 peaks were not observed in X-ray diffractograms of these compounds. The results obtained by TGA to determine the calcium content of the drugs studied were satisfactory when compared with those obtained by ICP-OES. In the AM 1 tablet was obtained the content of 35.37% and 32.62% for TG by ICP-OES, at 6 AM a percentage of 17.77% and 16.82% and for AM 7 results obtained were 8.93% for both techniques, showing that the thermogravimetry can be used to determine the percentage of calcium in tablets. The technique offers speed, economy in the use of samples and procedures eliminating the use of acid reagents in the process of the sample and efficiency results.

Hidróxidos duplos lamelares de magnésio e alumínio modificados com carbonato e p123 para adsorção de dióxido de carbono

Muitos mecanismos provocados pela ação humana vêm gerando um aumento na queima de combustíveis fósseis e processos químicos (produtos orgânicos, carvão, madeira, óleo diesel, gasolina e outros derivados de petróleo) e, consequentemente, há um aumento na emissão de CO2 na atmosfera. Uma das alternativas para a captura desse poluente é o processo de adsorção, o qual pode ajudar na redução do CO2. As hidrotalcitas ou hidróxidos duplos lamelares (HDL s) estão dentre esses materiais estudados, já que apresentam alta estabilidade e uma boa porosidade, tornando-se assim um promissor adsorvente de gases poluentes. Os HDL s formam um grupo de argilas do tipo aniônico que consiste em camadas positivamente carregadas de óxido de metal (ou hidróxido de metal) com intercamadas de ânions. Foi constatado que ânions que possuem duas cargas negativas, estabilizam muito mais que ânions monovalentes, sendo o carbonato o mais estável dos ânions divalentes. Neste trabalho, foi proposta uma modificação na síntese direta através da co-precipitação a pH constante utilizando sais de cátions divalentes (Mg2+) e trivalentes (Al3+) reportados na literatura. Durante a síntese dos HDL s retirou-se o carbonato, bem como, utilizou-se um copolímero como um template para o alargamento das lamelas. As amostras foram caracterizadas utilizando as técnicas de DRX, TG/DTG, FTIR, MEV/EDX, MET e adsorção e dessorção de N2. Os dados obtidos indicam que a estrutura, mesmo após a modificação, apresentou resultados condizentes com os encontrados na literatura. Dentre as várias aplicações dos HDL s foi realizado o estudo da adsorção do CO2. A capacidade de adsorção do material foi testada de acordo com o tempo de contato entre o adsorvente e o adsorbato, sendo esperado que os materiais tratados com template apresentassem um maior desempenho

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

Otimização da síntese de nanoferritas de nizn dopada com cobre e cobalto

Different compositions of Ni0,5-xCuxZn0,5Fe2O4 and Ni0,5-xCoxZn0,5Fe2O4 0 ≤ x ≤ 0.3 were synthesized ferrite y the citrate precursor method. The stoichiometric compositions were calcined in air at 350°C and then pressed into pellets and toroids. The pressed samples were sintered at temperatures of 1000, 1050 and 1100°C/3h in air control at the speed of heating and cooling. The calcined powders were characterized by XRD, TGA / DTG, FTIR, SEM and vibrating sample magnetometry (VSM) and the sintered samples by XRD, SEM, MAV, density and measurements of permeability and magnetic losses. There was pure phase formation ferrimagnetism applied at all temperatures except for A-I composition at all sintering temperatures and A-II only at a temperature of 1100°C. Crystallite sizes were obtained by Rietveld analysis, nanometer size from 11 to 20 nm for the calcined powders. For SEM, the sintered samples showed grain size between 1 and 10 micrometers. Bulk density (ρ) of sintered material presented to the Families almost linear behavior with increasing temperature and a tendency to decrease with increasing concentration of copper, different behavior of the B Family, where the increase in temperature decreased the density. The magnetic measurements revealed the powder characteristics of a soft ferrimagnetic material. Two processes of magnetization were considered, the superparamagnetism at low temperatures (350°C) and the formation of magnetic domains at higher temperatures. Obtaining the best parameters for P and B-II magnetic ferrites at high temperatures. The sintered material at 1000°C showed a relative permeability (μ) from 50 to 800 for the A Family and from 10 to 600 for the B Family. The samples sintered at 1100°C, B Family showed a variation from 10 to 1000 and the magnetic loss (tan δ) of A and B Families, around of 1. The frequency response of the toroidal core is in the range of 0.3 kHz. Several factors contribute to the behavior of microstructure considering the quantities μ and tan δ, such as the grain size, inter-and intragranular porosity, amount of grain boundary and the aspects of the dynamics of domain walls at high frequencies.