Síntese e caracterização de ferrita ni-zn pelo método dos precursores poliméricos calcinada por energia de microondas

Magnetic ceramics have been widely investigated, especially with respect to intrinsic and extrinsic characteristics of these materials. Among the magnetic ceramic materials of technological interest, there are the ferrites. On the other hand, the thermal treatment of ceramic materials by microwave energy has offered various advantages such as: optimization of production processes, high heat control, low consumption of time and energy among others. In this work were synthesized powders of Ni-Zn ferrite with compositions Ni1- xZnxFe2O4 (0.25 ≤ x ≤ 0.75 mols) by the polymeric precursor route in two heat treatment conditions, conventional oven and microwave energy at 500, 650, 800 and 950°C and its structural, and morphological imaging. The materials were characterized by thermal analysis (TG/ DSC), X-ray diffraction (XRD), absorption spectroscopy in the infrared (FTIR), scanning electron microscopy (SEM), X-ray spectroscopy and energy dispersive (EDS) and vibrating sample magnetometry (VSM). The results of X-ray diffraction confirmed the formation of ferrite with spinel-type cubic structure. The extrinsic characteristics of the powders obtained by microwave calcination and influence significantly the magnetic behavior of ferrites, showing particles ferrimagnéticas characterized as soft magnetic materials (soft), is of great technological interest. The results obtained led the potential application of microwave energy for calcining powders of Ni-Zn ferrite

Síntese e caracterização de ferrita ni-zn pelo método dos precursores poliméricos calcinada por energia de microondas

Magnetic ceramics have been widely investigated, especially with respect to intrinsic and extrinsic characteristics of these materials. Among the magnetic ceramic materials of technological interest, there are the ferrites. On the other hand, the thermal treatment of ceramic materials by microwave energy has offered various advantages such as: optimization of production processes, high heat control, low consumption of time and energy among others. In this work were synthesized powders of Ni-Zn ferrite with compositions Ni1- xZnxFe2O4 (0.25 ≤ x ≤ 0.75 mols) by the polymeric precursor route in two heat treatment conditions, conventional oven and microwave energy at 500, 650, 800 and 950°C and its structural, and morphological imaging. The materials were characterized by thermal analysis (TG/ DSC), X-ray diffraction (XRD), absorption spectroscopy in the infrared (FTIR), scanning electron microscopy (SEM), X-ray spectroscopy and energy dispersive (EDS) and vibrating sample magnetometry (VSM). The results of X-ray diffraction confirmed the formation of ferrite with spinel-type cubic structure. The extrinsic characteristics of the powders obtained by microwave calcination and influence significantly the magnetic behavior of ferrites, showing particles ferrimagnéticas characterized as soft magnetic materials (soft), is of great technological interest. The results obtained led the potential application of microwave energy for calcining powders of Ni-Zn ferrite

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)

Avaliação de metodologia de preparo de amostra de petróleo por digestão ácida auxiliada por microondas para determinação de metais por ICP-OES

This project describes a methodology optimization that would allow for a more efficient microwave assisted digestion process for petroleum samples. With the possible chance to vary various factors at once to see if any one factor was significant enough in the answers, experimental planning was used. Microwave assisted digestion allows, through the application of potency, an increasing number of collisions between the HNO3 and H2O2 molecules, favoring sample opening for complex matrixes. For this, a 24 factorial experimental planning was used, varying potency, time and the volumes for HNO3 65% and H2O2 30%. To achieve the desired answers, several elements were monitored (C, Cu, Cr, Fe, Ni, Zn and V) through Inductively coupled plasma atomic emission spectroscopy (ICP-OES). With this initial study it was noticed that the HNO3 was not a significant factor for any of the statistical studies for any of the analytes and the other 3 factors and their interactions showed statistical significance. A Box Behnken experimental planning was used taking in consideration 3 factors: H2O2 volume, time (min) and Potency (W), Nitric Acid kept at 4mL for a mass of 0,1g of petroleum. The results were extremely satisfying showing higher efficiency in the digestion process and taking in a responsibility between the answers for each analyte and the carbon monitoring was achieved in the following conditions: 7mL of H2O2, 700 Watts of potency and a reaction time of 7 minutes with 4mL de HNO3 for a mass of 0,1g of petroleum. The optimized digestion process was applied to four different petroleum samples and the analytes determined by ICP-OES

Desenvolvimento de uma metodologia para caracterização de amostras de sedimento: Rio Jundiaí RN

The study of sediment in water bodies presents great environmental importance, because of its ability to adsorb the pollutants, they may facilitate the understanding of the history of the current quality of the water system. Depending on how it is done the collection, analysis can show both a recent contamination as old. The detailed characterization of the sediment may reveal details that can understand how each type of pollutant interacts with the material given its composition. In this work it has developed a systematic methodology to characterize samples of sediment, with the aim to understand how a series of metal is distributed in different size fractions of the sediment. This study was conducted in five samples of sediment (P1, P2, P3a, P3B and P3c) collected in Jundiaí river, one of the most important tributaries of the river Potengi in the region of Macaíba, RN. The characterization was made with the samples previously sieved into meshes with different granulometries (+8#, -8+16#, -16+65# - 65+100#,-100+200#,-200+250# and -250#), using the following techniques: Analysis of specific surface area by BET method, determining the levels of organic matter (OM%) and humidity through the gravimetry and Analysis Thermogravimetric (TG), Infrared Spectroscopy in a Fourier transform (FTIR ), Analysis of X ray diffraction (XRD), analysis of heavy metals by optical emission spectrometry with the Argon Plasma (ICP-OES). The analyzed elements were Al, Cd, Cr, Cu, Fe, Mn, Ni, Zn and P. In addition to the techniques of characterization above, was also made the rebuilding of the samples P1, P2 and P3B in relation to the levels of organic matter and concentration of heavy metals. Then, the results of the recomposed samples were compared with those obtained in crude samples, showing great consistency. The gravimetry, used in determining the levels of organic matter, was not considered an appropriate method because the clay minerals present in the sediment samples analyzed fall apart in the same range of temperature (550-600 0C) used in roasting (600 0C). The results also showed the trend of organic matter and heavy metals to focus on the thin fractions, although the largest concentrations of metals are in intermediate fractions

Avaliação de metodologia de preparo de amostra de petróleo por digestão ácida auxiliada por microondas para determinação de metais por ICP-OES

This project describes a methodology optimization that would allow for a more efficient microwave assisted digestion process for petroleum samples. With the possible chance to vary various factors at once to see if any one factor was significant enough in the answers, experimental planning was used. Microwave assisted digestion allows, through the application of potency, an increasing number of collisions between the HNO3 and H2O2 molecules, favoring sample opening for complex matrixes. For this, a 24 factorial experimental planning was used, varying potency, time and the volumes for HNO3 65% and H2O2 30%. To achieve the desired answers, several elements were monitored (C, Cu, Cr, Fe, Ni, Zn and V) through Inductively coupled plasma atomic emission spectroscopy (ICP-OES). With this initial study it was noticed that the HNO3 was not a significant factor for any of the statistical studies for any of the analytes and the other 3 factors and their interactions showed statistical significance. A Box Behnken experimental planning was used taking in consideration 3 factors: H2O2 volume, time (min) and Potency (W), Nitric Acid kept at 4mL for a mass of 0,1g of petroleum. The results were extremely satisfying showing higher efficiency in the digestion process and taking in a responsibility between the answers for each analyte and the carbon monitoring was achieved in the following conditions: 7mL of H2O2, 700 Watts of potency and a reaction time of 7 minutes with 4mL de HNO3 for a mass of 0,1g of petroleum. The optimized digestion process was applied to four different petroleum samples and the analytes determined by ICP-OES

Determinação de Ba, Cd, Cr, Cu, Ni, Pb, Sn e Zn em Tainha (Mugil brasiliensis) nos estuários potiguares

Heavy metals can cause problems of human poisoning by ingestion of contaminated food, and the environment, a negative impact on the aquatic fauna and flora. And for the presence of these metals have been used for aquatic animals biomonitoramento environment. This research was done in order to assess the environmental impact of industrial and domestic sewage dumped in estuaries potiguares, from measures of heavy metals in mullet. The methods used for these determinations are those in the literature for analysis of food and water. Collections were 20 samples of mullet in several municipality of the state of Rio Grande do Norte, from the estuaries potiguares. Were analyzed the content of humidity, ash and heavy metals. The data were subjected to two methods of exploratory analysis: analysis of the main components (PCA), which provided a multivariate interpretation, showing that the samples are grouped according to similarities in the levels of metals and analysis of hierarchical groupings (HCA), producing similar results. These tests have proved useful for the treatment of the data producing information that would hardly viewed directly in the matrix of data. The analysis of the results shows the high levels of metallic species in samples Mugil brasiliensis collected in Estuaries /Potengi, Piranhas/Açu, Guaraíra / Papeba / Arês and Curimataú