Determinação de CD, PB, e TL em água produzida por HR-CS GF AAS após extração em ponto nuvem

Produced water is a major problem associated with the crude oil extraction activity. The monitoring of the levels of metals in the waste is constant and requires the use of sensitive analytical techniques. However, the determination of trace elements can often require a pre-concentration step. The objective of this study was to develop a simple and rapid analytical method for the extraction and pre-concentration based on extraction phenomenon cloud point for the determination of Cd, Pb and Tl in produced water samples by spectrometry of high resolution Absorption source continues and atomization graphite furnace. The Box Behnken design was used to obtain the optimal condition of extraction of analytes. The factors were evaluated: concentration of complexing agent (o,o-dietilditilfosfato ammonium, DDTP), the concentration of hydrochloric acid and concentration of surfactant (Triton X -114). The optimal condition obtained through extraction was: 0,6% m v-1 DDTP, HCl 0,3 mol L-1 and 0,2% m v-1 of Triton X - 114 for Pb; 0,7% m v-1 DDTP, HCl 0,8 mol L-1 and 0,2% m v-1 Triton X-114 for Cd. For Tl was evidenced that best extraction condition occurs with no DDTP, the extraction conditions were HCl 1,0 mol L-1 e 1,0% m v-1 de Triton X - 114. The limits of detection for the proposed method were 0,005 µg L-1 , 0,03 µg L-1 and 0,09 µg L-1 to Cd, Pb and Tl, Respectively. Enrichment factors Were greater than 10 times. The method was applied to the water produced in the Potiguar basin, and addition and recovery tests were performed, and values were between 81% and 120%. The precision was expressed with relative standard deviation (RSD) is less than 5%

Desenvolvimento de metodologia de extração e pré-concentração utilizando sistema microemulsionado para determinação de Cd, Co, Cu, Ni, Pb e Tl em águas naturais e produzidas por HR-CS AAS

The determination and monitoring of metallic contaminants in water is a task that must be continuous, leading to the importance of the development, modification and optimization of analytical methodologies capab le of determining the various metal contaminants in natural environments, because, in many cases, the ava ilable instrumentation does not provide enough sensibility for the determination of trace values . In this study, a method of extraction and pre- concentration using a microemulsion system with in the Winsor II equilibrium was tested and optimized for the determination of Co, Cd, P b, Tl, Cu and Ni through the technique of high- resolution atomic absorption spectrometry using a continuum source (HR-CS AAS). The optimization of the temperature program for the graphite furnace (HR-CS AAS GF) was performed through the pyrolysis and atomization curves for the analytes Cd, Pb, Co and Tl with and without the use of different chemical modifiers. Cu and Ni we re analyzed by flame atomization (HR-CS F AAS) after pre-concentr ation, having the sample introduction system optimized for the realization of discrete sampling. Salinity and pH levels were also analyzed as influencing factors in the efficiency of the extraction. As final numbers, 6 g L -1 of Na (as NaCl) and 1% of HNO 3 (v/v) were defined. For the determination of the optimum extraction point, a centroid-simplex statistical plan was a pplied, having chosen as the optimum points of extraction for all of the analytes, the follo wing proportions: 70% aqueous phase, 10% oil phase and 20% co-surfactant/surfactant (C/S = 4). After extraction, the metals were determined and the merit figures obtained for the proposed method were: LOD 0,09, 0,01, 0,06, 0,05, 0,6 and 1,5 μg L -1 for Pb, Cd, Tl, Co, Cu and Ni, re spectively. Line ar ranges of ,1- 2,0 μg L -1 for Pb, 0,01-2,0 μg L -1 for Cd, 1,0 - 20 μg L -1 for Tl, 0,1-5,0 μg L -1 for Co, 2-200 μg L -1 and for Cu e Ni 5-200 μg L -1 were obtained. The enrichment factors obtained ranged between 6 and 19. Recovery testing with the certified sample show ed recovery values (n = 3, certified values) after extraction of 105 and 101, 100 and 104% for Pb, Cd, Cu and Ni respectively. Samples of sweet waters of lake Jiqui, saline water from Potengi river and water produced from the oil industry (PETROBRAS) were spiked and the recovery (n = 3) for the analytes were between 80 and 112% confirming th at the proposed method can be used in the extraction. The proposed method enabled the sepa ration of metals from complex matrices, and with good pre-concentration factor, consistent with the MPV (allowed limits) compared to CONAMA Resolution No. 357/2005 which regulat es the quality of fresh surface water, brackish and saline water in Brazil.

Adição de nanopartículas de Ti em matriz de Fe através da deposição por magnetron sputtering

Microalloyed steels constitute a specific class of steel with low amount of carbon and microalloying elements such as Vanadium (V), Niobium (Nb) and Titanium (Ti). The development and application of microalloyed steels and steels in general are limited to the handling of powders with particles of submicron or nanometer dimensions. Therefore, this work presents an alternative in order to construction of microalloyed steels utilizing the deposition by magnetron sputtering technique as a microalloying element addiction in which Ti nanoparticles are dispersed in an iron matrix. The advantage of that technique in relation to the conventional metallurgical processes is the possibility of uniformly disperse the microalloying elements in the iron matrix. It was carried out deposition of Ti onto Fe powder in high CH4, H2, Ar plasma atmosphere, with two deposition times. After the deposition, the iron powder with nanoparticles of Ti dispersed distributed, were compacted and sintered at 1120 ° C in resistive furnace. Characterization techniques utilized in the samples of powder before and after deposition of Ti were Granulometry, Scanning Electron Microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX) and X-ray diffraction (DRX). In the case of sintered samples, it was carried out characterization by SEM and Vickers Microhardness assays. The results show which the deposition technique by magnetron sputtering is practicable in the dispersion of particles in iron matrix. The EDX microanalysis detected higher percentages of Ti when the deposition were carried out with the inert gas and when the deposition process was carried out with reactive gas. The presence of titanium in iron matrix was also evidenced by the results of X-ray diffraction peaks that showed shifts in the network matrix. Given these results it can be said that the technique of magnetron sputtering deposition is feasible in the dispersion of nanoparticles of iron matrix in Ti.

Determinação do perfil térmico em amostras de aço AISI M35 imersas em plasma

The heat transfer between plasma and a solid occurs mostly due the radiation and the collision of the particles on the material surface, heating the material from the surface to the bulk. The thermal gradient inside the sample depends of the rate of particles collisions and thermal conductivity of the solid. In order to study that effect, samples of AISI M35 steel, with 9,5 mm X 3,0 mm (diameter X thickness) were quenched in resistive furnace and tempereds in plasma using the plane configuration and hollow cathode, working with pressures of 4 and 10 mbar respectively. Analyzing the samples microstructure and measuring the hardness along the transversal profile, it was possible to associate the tempered temperature evaluating indirectly the thermal profile. This relation was obtained by microstructural analyzes and through the hardness curve x tempered sample temperature in resistive furnace, using temperatures of 500, 550, 600, 650 and 700°C. The microstructural characterization of the samples was obtained by the scanning electron microscopy, optic microscopy and X-ray diffraction. It was verified that all samples treated in plasma presented a superficial layer, denominated affected shelling zone, wich was not present in the samples treated in resistive furnace. Moreover, the samples that presented larger thermal gradient were treated in hollow cathode with pressure of 4 mbar

Tratamento de materiais contaminados com bifenilas policloradas (PCBS) via extração convencional e fluído supercrítico

The decontamination of the materials has been subject of some studies. One of the factors that it increases the pollution is the lack of responsibility in the discarding of toxic trash, as for example the presence of PCB (Polychlorinated Biphenyls) in the environment. In the Brazilian regulations, the material contaminated with PCB in concentrations higher than 50 ppm must be stored in special places or destroyed, usually by incineration in plasma furnace with dual steps. Due to high cost of the procedure, new methodologies of PCBs removal has been studied. The objective of this study was to develop an experimental methodology and analytical methodology for quantification of removal of PCBs through out the processes of extractions using supercritical fluid and Soxhlet method, also technical efficiency of the two processes of extraction, in the treatment of contaminated materials with PCBs. The materials studied were soils and wood, both were simulated contamination with concentration of 6.000, 33.000 and 60.000 mg of PCB/ kg of materials. Soxhlet extractions were performed using 100 ml of hexane, and temperature of 180 ºC. Extractions by fluid supercritical were performed at conditions of 200 bar, 70°C, and supercritical CO2 flow-rate of 3 g/min for 1-3 hours. The extracts obtained were quantified using Gas chromatography-mass spectrometry (GC/MS). The conventional extractions were made according to factorial experimental planning technique 22, with aim of study the influence of two variables of process extraction for the Soxhlet method: contaminant concentration and extraction time for obtain a maximum removal of PCB in the materials. The extractions for Soxhlet method were efficient for extraction of PCBs in soil and wood in both solvent studied (hexane and ethanol). In the experimental extraction in soils, the better efficient of removal of PCBs using ethanol as solvent was 81.3% than 95% for the extraction using hexane as solvent, for equal time of extraction. The results of the extraction with wood showed statistically it that there is not difference between the extractions in both solvent studied. The supercritical fluid extraction in the conditions studied showed better efficiency in the extraction of PCBs in the wood matrix than in soil, for two hours extractions the obtain percentual of 43.9 ± 0.5 % for the total of PCBs extracted in the soils against 95.1 ± 0,5% for the total of PCBs extracted in the wood. The results demonstrated that the extractions were satisfactory for both technical studied

Efeito da adição de WC e Co na sinterização e propriedades mecânicas da alumina

Composites based on alumina (Al2O3), tungsten carbide (WC) and cobalt (Co) exhibit specific properties such as low density, high oxidation resistance, high melting point and high chemical inertia. That composite shows to be a promising material for application in various fields of engineering. In this work, the mechanical properties of the composite (Al2O3 – WC – Co), particularly density and hardness, were evaluated according to the effects of the variables of powder processing parameters, green compact and sintered. Powder composites with the composition of 80 wt% Al2O3, 18 wt% WC and 2 wt% Co were processed by high energy ball milling in a planetary mill for 50 hours as well as mixed by manual mixing in a glass vessel with the same proportion. Samples were collected (2, 10, 20, 30, 40 and 50 hours) during the milling process. Then, the powders were compacted in a cylindrical die with 5 mm in diameter in a uniaxial press with pressures of 200 and 400 MPa. The sintering was in two stages: first, the solid phase sintering was performed at 1126 and 1300 °C for 1 hour with a heating rate of 10 °C/min in a resistive furnace under argon atmosphere for green samples compacted in 200 and 400 MPa; the second sintering was performed on dilatometer in solid phase at 1300 °C for green sample compacted in 200 MPa, another sintering also was performed on dilatometer, this time in liquid phase at 1550 °C for green samples compacted in 200 and 400 MPa, with the same parameters used in resistive furnace. The raw materials were characterized by X – ray diffraction (XRD), X – ray fluorescence (XRF), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS) and laser particlemeter. The sintered samples were subjected to microhardness testing. The results showed that high energy milling achieved to the objectives regarding the particle size and the dispersion of composite phases. However, the hardness did not achieve to significant results, this is an indication that the composite has low fracture toughness.

Efeito da adição de WC e Co na sinterização e propriedades mecânicas da alumina

Composites based on alumina (Al2O3), tungsten carbide (WC) and cobalt (Co) exhibit specific properties such as low density, high oxidation resistance, high melting point and high chemical inertia. That composite shows to be a promising material for application in various fields of engineering. In this work, the mechanical properties of the composite (Al2O3 – WC – Co), particularly density and hardness, were evaluated according to the effects of the variables of powder processing parameters, green compact and sintered. Powder composites with the composition of 80 wt% Al2O3, 18 wt% WC and 2 wt% Co were processed by high energy ball milling in a planetary mill for 50 hours as well as mixed by manual mixing in a glass vessel with the same proportion. Samples were collected (2, 10, 20, 30, 40 and 50 hours) during the milling process. Then, the powders were compacted in a cylindrical die with 5 mm in diameter in a uniaxial press with pressures of 200 and 400 MPa. The sintering was in two stages: first, the solid phase sintering was performed at 1126 and 1300 °C for 1 hour with a heating rate of 10 °C/min in a resistive furnace under argon atmosphere for green samples compacted in 200 and 400 MPa; the second sintering was performed on dilatometer in solid phase at 1300 °C for green sample compacted in 200 MPa, another sintering also was performed on dilatometer, this time in liquid phase at 1550 °C for green samples compacted in 200 and 400 MPa, with the same parameters used in resistive furnace. The raw materials were characterized by X – ray diffraction (XRD), X – ray fluorescence (XRF), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS) and laser particlemeter. The sintered samples were subjected to microhardness testing. The results showed that high energy milling achieved to the objectives regarding the particle size and the dispersion of composite phases. However, the hardness did not achieve to significant results, this is an indication that the composite has low fracture toughness.

Adição de nanopartículas de Ti em matriz de Fe através da deposição por magnetron sputtering

Microalloyed steels constitute a specific class of steel with low amount of carbon and microalloying elements such as Vanadium (V), Niobium (Nb) and Titanium (Ti). The development and application of microalloyed steels and steels in general are limited to the handling of powders with particles of submicron or nanometer dimensions. Therefore, this work presents an alternative in order to construction of microalloyed steels utilizing the deposition by magnetron sputtering technique as a microalloying element addiction in which Ti nanoparticles are dispersed in an iron matrix. The advantage of that technique in relation to the conventional metallurgical processes is the possibility of uniformly disperse the microalloying elements in the iron matrix. It was carried out deposition of Ti onto Fe powder in high CH4, H2, Ar plasma atmosphere, with two deposition times. After the deposition, the iron powder with nanoparticles of Ti dispersed distributed, were compacted and sintered at 1120 ° C in resistive furnace. Characterization techniques utilized in the samples of powder before and after deposition of Ti were Granulometry, Scanning Electron Microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX) and X-ray diffraction (DRX). In the case of sintered samples, it was carried out characterization by SEM and Vickers Microhardness assays. The results show which the deposition technique by magnetron sputtering is practicable in the dispersion of particles in iron matrix. The EDX microanalysis detected higher percentages of Ti when the deposition were carried out with the inert gas and when the deposition process was carried out with reactive gas. The presence of titanium in iron matrix was also evidenced by the results of X-ray diffraction peaks that showed shifts in the network matrix. Given these results it can be said that the technique of magnetron sputtering deposition is feasible in the dispersion of nanoparticles of iron matrix in Ti.

Determinação do perfil térmico em amostras de aço AISI M35 imersas em plasma

The heat transfer between plasma and a solid occurs mostly due the radiation and the collision of the particles on the material surface, heating the material from the surface to the bulk. The thermal gradient inside the sample depends of the rate of particles collisions and thermal conductivity of the solid. In order to study that effect, samples of AISI M35 steel, with 9,5 mm X 3,0 mm (diameter X thickness) were quenched in resistive furnace and tempereds in plasma using the plane configuration and hollow cathode, working with pressures of 4 and 10 mbar respectively. Analyzing the samples microstructure and measuring the hardness along the transversal profile, it was possible to associate the tempered temperature evaluating indirectly the thermal profile. This relation was obtained by microstructural analyzes and through the hardness curve x tempered sample temperature in resistive furnace, using temperatures of 500, 550, 600, 650 and 700°C. The microstructural characterization of the samples was obtained by the scanning electron microscopy, optic microscopy and X-ray diffraction. It was verified that all samples treated in plasma presented a superficial layer, denominated affected shelling zone, wich was not present in the samples treated in resistive furnace. Moreover, the samples that presented larger thermal gradient were treated in hollow cathode with pressure of 4 mbar