Recuperação e purificação do antígeno 503 de Leishmania i. chagasi expresso em E. coli e remoção de endotoxina utilizando adsorção em leito expandido

The growing interest and applications of biotechnology products have increased the development of new processes for recovery and purification of proteins. The expanded bed adsorption (EBA) has emerged as a promising technique for this purpose. It combines into one operation the steps of clarification, concentration and purification of the target molecule. Hence, the method reduces the time and the cost of operation. In this context, this thesis aim was to evaluate the recovery and purification of 503 antigen of Leishmania i. chagasi expressed in E. coli M15 and endotoxin removal by EBA. In the first step of this study, batch experiments were carried out using two experimental designs to define the optimal adsorption and elution conditions of 503 antigen onto Streamline chelating resin. For adsorption assays, using expanded bed, it was used a column of 2.6 cm in diameter by 30.0 cm in height coupled to a peristaltic pump. In the second step of study, the removal of endotoxin during antigen recovery process was evaluated employing the non-ionic surfactant Triton X-114 in the washing step ALE. In the third step, we sought developing a mathematical model able to predict the 503 antigen breakthrough curves in expanded mode. The experimental design results to adsorption showed the pH 8.0 and the NaCl concentration of 2.4 M as the optimum adsorption condition. In the second design, the only significant factor for elution was the concentration of imidazole, which was taken at 600 mM. The adsorption isotherm of the 503 antigen showed a good fit to the Langmuir model (R = 0.98) and values for qmax (maximum adsorption capacity) and Kd (equilibrium constant) estimated were 1.95 mg/g and 0.34 mg/mL, respectively. Purification tests directly from unclarified feedstock showed a recovery of 59.2% of the target protein and a purification factor of 6.0. The addition of the non-ionic surfactant Triton X-114 to the washing step of EBA led to high levels (> 99%) of LPS removal initially present in the samples for all conditions tested. The mathematical model obtained to describe the 503 antigen breakthrough curves in Streamline Chelanting resin in expanded mode showed a good fit for both parameter estimation and validation steps. The validated model was used to optimize the efficiencies, achieving maximum values of the process and of the column efficiencies of 89.2% and 75.9%, respectively. Therefore, EBA is an efficient alternative for the recovery of the target protein and removal of endotoxin from an E. coli unclarified feedstock in just one step.

Estudo do tratamento sequencial (adsorção e eletro-oxidação) para remediação de efluente sintético contaminado com BTX

This paper proposed the study of the treatment of a synthetic wastewater contaminated with BTX by electro-oxidation batch with the anode of Ti/PbO2, and the adsorption of BTX using expanded perlite as adsorbent material, and to evaluate the best operating conditions both methods in order to perform a sequential treatment (adsorption and electro-oxidation) and achieve greater efficiency in the removal of the compounds. The operating conditions were measured: temperature, current density and applied amount of the adsorbent material, by UV-VIS analysis and Demand Chemical oxygen demand (COD). According to the experimental results, the electro-oxidative treatment was efficient in the degradation of the compounds BTX (benzene, toluene and xylenes) in synthetic sewage due to the electrochemical properties of the anode of Ti/PbO2. The applied current density and temperature promoted increased efficiency of COD removal, reaching obtain percentages greater than 70%. In the adsorption process, the temperature increase was not a factor in the removal of organic matter, while the increase in the amount of adsorbent material led to an increase in the percentage removal, obtaining 66.30% using 2 g of adsorbent. The selected operating conditions of both treatments performed separately take into account the removal efficiency of organic matter, and the low energy consumption and operating costs, so the sequential treatment were satisfactory reaching 87.26% of COD removal using adsorption as a pretreatment. Quantification of BTX through the analysis of gas chromatography at the end of the treatments also confirmed the removal efficiency of organic compounds, giving outstanding advantages to sequential treatment.

Potencialidade do tratamento eletroquímico oxidativo associado à adsorção para remediação de corantes têxteis

This study aimed to evaluate the potential of oxidative electrochemical treatment coupled with adsorption process using expanded perlite as adsorbent in the removal of textile dyes, Red Remazol and Novacron Blue on synthetic effluent. Dyes and perlite were characterized by thermogravimetry techniques (TG), Differential Scanning Calorimetry (DSC), Spectroscopy infrared (IR), Scanning Electron Microscopy (SEM), X-ray diffraction (XRD) and X-ray fluorescence (XRF) techniques. Electrochemical treatments used as anodes, Ti/Pt and Pb/PbO2 under different conditions: 60 minutes, current density 20, 40 e 60 mAcm-2, pH 1, 4.5 e 8 and temperature variation 20, 40 e 60 ºC. In the case of adsorption tests, contact time of 30 minutes for the Remazol Red dye and 20 minutes for Novacron Blue were established, while pH 1, 4.5 e 8, 500 mg adsorbent and temperature variation 20, 40 e 60 ºC were used for both treatments. The results indicated that both treatments, electroxidation/adsorption and the adsorption/electroxidation, were effective for removing color from synthetic solutions. The consumption of electricity allowed to evaluate the applicability of the electrochemical process, providing very acceptable values, which allowed us to estimate the cost. Total organic carbon (TOC) and Gas Chromatography linked mass spectrometer (GC-MS) analyzes were performed, showing that the better combination for removing organic matter is by Pb/PbO2 and perlite. Meanwhile, GC-MS indicated that the by-products formed are benzoic acid, phthalic acid, thiocarbamic acid, benzene, chlorobenzene, phenol-2-ethyl and naphthalene when Remazol Red was degraded. Conversely, aniline, phthalic acid, 1, 6 - dimethylnaphthalene, naphthalene and ion hidroxobenzenosulfonat was detected when Novacron Blue was studied. Analyses obtained through atomic absorption spectrometry showed that there was release of lead in the electrochemical oxidation of analyzes that were performed with the anode Pb/PbO2, but these values are reduced by subjecting the effluent to adsorption analysis. According to these results, sequential techniques electroxidation/adsorption and adsorption/electroxidation are to treat solutions containing dyes.

Potencialidade do tratamento eletroquímico oxidativo associado à adsorção para remediação de corantes têxteis

This study aimed to evaluate the potential of oxidative electrochemical treatment coupled with adsorption process using expanded perlite as adsorbent in the removal of textile dyes, Red Remazol and Novacron Blue on synthetic effluent. Dyes and perlite were characterized by thermogravimetry techniques (TG), Differential Scanning Calorimetry (DSC), Spectroscopy infrared (IR), Scanning Electron Microscopy (SEM), X-ray diffraction (XRD) and X-ray fluorescence (XRF) techniques. Electrochemical treatments used as anodes, Ti/Pt and Pb/PbO2 under different conditions: 60 minutes, current density 20, 40 e 60 mAcm-2, pH 1, 4.5 e 8 and temperature variation 20, 40 e 60 ºC. In the case of adsorption tests, contact time of 30 minutes for the Remazol Red dye and 20 minutes for Novacron Blue were established, while pH 1, 4.5 e 8, 500 mg adsorbent and temperature variation 20, 40 e 60 ºC were used for both treatments. The results indicated that both treatments, electroxidation/adsorption and the adsorption/electroxidation, were effective for removing color from synthetic solutions. The consumption of electricity allowed to evaluate the applicability of the electrochemical process, providing very acceptable values, which allowed us to estimate the cost. Total organic carbon (TOC) and Gas Chromatography linked mass spectrometer (GC-MS) analyzes were performed, showing that the better combination for removing organic matter is by Pb/PbO2 and perlite. Meanwhile, GC-MS indicated that the by-products formed are benzoic acid, phthalic acid, thiocarbamic acid, benzene, chlorobenzene, phenol-2-ethyl and naphthalene when Remazol Red was degraded. Conversely, aniline, phthalic acid, 1, 6 - dimethylnaphthalene, naphthalene and ion hidroxobenzenosulfonat was detected when Novacron Blue was studied. Analyses obtained through atomic absorption spectrometry showed that there was release of lead in the electrochemical oxidation of analyzes that were performed with the anode Pb/PbO2, but these values are reduced by subjecting the effluent to adsorption analysis. According to these results, sequential techniques electroxidation/adsorption and adsorption/electroxidation are to treat solutions containing dyes.

Catalisadores bifuncionais à base de silicoaluminofosfato e fosfatos de nióbio para emprego em reações de hidroisomerização e hidrocraqueamento do n-hexadecano

Lubricants and cutting middle distillates typically have large amounts of n-paraffins to increase its freezing point and fluidity. Accordingly, the removal of n-paraffins of long chain lubricants oils and diesel is essential to get a product with good cold flow properties. The development of new catalysts, which exhibit thermal stability and catalytic activity for the hydroisomerization reaction is still a challenge. Thus, silicoaluminophosphates (SAPO) were synthesized by different routes. Have been used also post-synthesis treatment for obtaining hybrid structures and others synthesis have been carried out with mesoporous template (soft and hard-template). Therefore, SAPO have been impregnated with H2PtCl6 solution by the incipient wetness method. Then assessments of catalytic activities in hydroisomerization and hydrocracking reactions of hexadecane have been held. Besides SAPO, niobium phosphate - NbP - were also impregnated with platinum and evaluated in the same reaction. After impregnation, these catalysts have been characterized by X-ray diffraction (XRD), nitrogen adsorption, infrared spectroscopy with adsorbed pyridine (IV-PY), scanning electron microscopy (SEM) and resonance nuclear magnetic 29Si (29Si-NMR). The characterization results by XRD have shown that it has been possible to obtain mesoporous SAPOs. However, for the syntheses with soft template there was collapse of the structure after removal of the organic template. Even so, these catalysts have been actives. It was possible to obtain hybrid materials through the synthesis of SAPO-11 made with hard templates and by means of post-synthesis treatments samples of SAPO-11. Moreover, NbP has shown characteristic XRD of amorphous materials, with high acidity and were active in the conversion of hexadecane.

Catalisadores bifuncionais à base de silicoaluminofosfato e fosfatos de nióbio para emprego em reações de hidroisomerização e hidrocraqueamento do n-hexadecano

Lubricants and cutting middle distillates typically have large amounts of n-paraffins to increase its freezing point and fluidity. Accordingly, the removal of n-paraffins of long chain lubricants oils and diesel is essential to get a product with good cold flow properties. The development of new catalysts, which exhibit thermal stability and catalytic activity for the hydroisomerization reaction is still a challenge. Thus, silicoaluminophosphates (SAPO) were synthesized by different routes. Have been used also post-synthesis treatment for obtaining hybrid structures and others synthesis have been carried out with mesoporous template (soft and hard-template). Therefore, SAPO have been impregnated with H2PtCl6 solution by the incipient wetness method. Then assessments of catalytic activities in hydroisomerization and hydrocracking reactions of hexadecane have been held. Besides SAPO, niobium phosphate - NbP - were also impregnated with platinum and evaluated in the same reaction. After impregnation, these catalysts have been characterized by X-ray diffraction (XRD), nitrogen adsorption, infrared spectroscopy with adsorbed pyridine (IV-PY), scanning electron microscopy (SEM) and resonance nuclear magnetic 29Si (29Si-NMR). The characterization results by XRD have shown that it has been possible to obtain mesoporous SAPOs. However, for the syntheses with soft template there was collapse of the structure after removal of the organic template. Even so, these catalysts have been actives. It was possible to obtain hybrid materials through the synthesis of SAPO-11 made with hard templates and by means of post-synthesis treatments samples of SAPO-11. Moreover, NbP has shown characteristic XRD of amorphous materials, with high acidity and were active in the conversion of hexadecane.

Vermiculitas tratadas quimicamente na obtenção de sólidos microporosos como precursores para híbridos inorgânico-orgânicos com aplicações adsortivas

ALVES, Ana paula Melo. Vermiculitas tratadas quimicamente na obtenção de sólidos microporosos como precursores para híbridos inorgânico-orgânicos com aplicações adsortivas. 2009. 124 f. Tese (Doutorado em Quimica) - Centro de Ciências Exatas e da Natureza, Universidade Federal da Paraíba, João Pessoa, PB, 2009.

Desenvolvimento e caracterização de filtros cerâmicos para aplicações a altas temperaturas

Ceramic filters are cellular structures that can be produced by various techniques, among which we highlight the replication method, or method of polymeric sponge. This method consists of impregnating polymeric foam with ceramic slurry, followed by heat treatment, where will occur decomposition of organic material and the sinter of the ceramic material, resulting in a ceramic whose structure is a replica of the impregnated sponge. Ceramic filters have specific properties that make this type of material very versatile, used in various technological applications such as filters for molten metals and burners, make these materials attractive candidates for high temperature applications. In this work we studied the systems Al2O3-LZSA ceramic filters processed in the laboratory, and commercial Al2O3-SiC ceramics filters, both obtained by the replica method, this work proposes the thermal and mechanical characterization. The sponge used in the processing of filters made in the laboratory was characterized by thermogravimetric analysis. The ceramic filters were characterized by compressive strength, flexural strength at high temperatures, thermal shock, permeability and physical characterization (density and porosity) and microstructural (MEV and X-rays). From the results obtained, the analysis was made of the mechanical behavior of these materials, comparing the model proposed by Gibson and Ashby model and modified the effective area and the tension adjusted, where the modified model adapted itself better to the experimental results, representing better the mechanical behavior of ceramic filters obtained by the replica method

Adsorção de cobre e cromo utilizando fibra de sisal visando o tratamento da água produzida pela indústria petrolífera

Currently, the oil industry is the biggest cause of environmental pollution. The objective was to reduce the concentration of copper and chromium in the water produced by the oil industry. It was used as adsorbent natural sisal fiber Agave sp treated with nitric acid and sodium hydroxide. All vegetable fibers have physical and morphological properties that enablies the adsorption of pollutants. The basic composition of sisal is cellulose, hemicellulose and lignin. The features are typically found in the characterization of vegetable fibers, except the surface area that was practically zero. In the first stage of adsorption, it was evaluated the effect of temperature and time skeeking to optimize the execution of the factorial design. The results showed that the most feasible fiber was the one treated with acid in five hours (30°C). The second phase was a factorial design, using acid and five hours, this time was it determined in the first phase. The tests were conducted following the experimental design and the results were analyzed by statistical methods in order to optimize the main parameters that influence the process: pH, concentration (mol / L) and fiber mass/ metal solution volume. The volume / mass ratio factor showed significant interference in the adsorption process of chromium and copper. The results obtained after optimization showed that the highest percentages of extraction (98%) were obtained on the following operating conditions: pH: 5-6, Concentration: 100 ppm and mass/ volume: 1 gram of fiber/50mL solution. The results showed that the adsorption process was efficient to remove chromium and copper using sisal fibers, however, requiring further studies to optimize the process.

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

Reforma a seco de metano com catalisadores Ni/MCM-41 sintetizados a partir de fontes alternativas de sílica

The production of synthesis gas has received renewed attention due to demand for renewable energies to reduce the emissions of gases responsible for enhanced greenhouse effect. This work was carried out in order to synthesize, characterize and evaluate the implementation of nickel catalysts on MCM-41 in dry reforming reactions of methane. The mesoporous molecular sieves were synthesized using as silica sources the tetraethyl orthosilicate (TEOS) and residual glass powder (PV). The sieves were impregnated with 10% nickel to obtain the metallic catalysts (Ni/MCM-41). These materials were calcined and characterized by Thermogravimetric Analysis (TG), Infrared spectroscopy (FTIR), X-ray Diffraction (XRD), Temperature-Programmed Reduction (TPR) and N2 Adsorption/Desorption isotherms (BET/BJH). The catalytic properties of the samples were evaluated in methane dry reforming with CO2 in order to produce synthesis gas to be used in the petrochemical industry. The materials characterized showed hexagonal structure characteristic of mesoporous material MCM-41 type, being maintained after impregnation with nickel. The samples presented variations in the specific surface area, average volume and diameter of pores based on the type of interaction between the nickel and the mesoporous support. The result of the the catalytic tests showed conversions about 91% CO2, 86% CH4, yelds about 85% CO and 81% H2 to Ni/MCM-41_TEOS_C, and conversions about 87% CO2, 82% CH4, yelds about 70% CO and 59% H2 to Ni/MCM-41_PV_C. The similar performance confirms that the TEOS can be replaced by a less noble materials

Extração de metais (K, Mg, Ba, Ca, Cr, Mn, Li, Fe) de água produzida utilizando sistema microemulsionado

The produced water is a byproduct formed due to production of petroleum and carries with it a high amount of contaminants such as oil particles in suspension, organic compounds and metals. Thus, these latter pollutants are very difficult to treat because of its high solubility in water. The objective of this work is to use and evaluate a microemulsioned system to remove metals ( K , Mg , Ba , Ca , Cr , Mn , Li , Fe ) of synthetic produced water. For the extraction of metals, it was used a pseudoternary diagram containing the following phases: synthetic produced water as the aqueous phase (AP), hexane as organic phase (OP), and a cosurfactant/surfactant ratio equal to four (C/S = 4) as the third phase, where the OCS (saponified coconut oil) was used as surfactant and n-butanol as cosurfactant. The synthetic produced water was prepared in a bench scale and the region of interest in the diagram for the removal of metals was determined by experimental design called. Ten points located in the phase Winsor II were selected in an area with a large amount of water and small amounts of reagents. The samples were analyzed in atomic absorption spectrometer, and the results were evaluated through a statistical assesment, allowing the efficiency analysis of the effects and their interactions. The results showed percentages of extraction above 90% for the metals manganese, iron, chromium, calcium, barium and magnesium, and around 45% for metals lithium and potassium. The optimal point for the simultaneous removal of metals was calculated using statistical artifact multiple response function (MR). This calculation showed that the point of greatest extraction of metals occurs was the J point, with the composition [72% AP, 9% OP, 19% C/S], obtaining a global extraction percentage about 80%. Considering the aspects analyzed, the microemulsioned system has shown itself to be an effective alternative in the extraction of metals on synthetic produced water remediation

Nitretação a plasma: fundamentos e aplicações

A nitretação é uma técnica de tratamento de superfície utilizada para endurecer superfícies de metais, principalmente de aços. O uso do plasma para auxiliar esta técnica vem crescendo nos últimos anos. Pelo fato desta técnica utilizar o plasma como fonte energética e este possuir uma vasta aplicação em outras técnicas para processamento de materiais, enobrece ainda mais a leitura do presente livro. Ele apresenta uma revisão da descarga elétrica em gases levando o leitor a refletir, multidisciplinarmente, sobre possibilidades de aplicação da mesma. Apresenta a técnica de nitretação iônica sob o aspecto histórico, científico, tecnológico, operacional e econômico e, finalmente, faz uma revisão das novas técnicas de endurecimento superficial assim como as técnicas convencionais de nitretação

Diagnóstico ecotoxicológico dos efluentes lançados no complexo estuarino do Jundiaí/Potengi, Natal/RN

Untreated effluents that reach surface water affect the aquatic life and humans. This study aimed to evaluate the wastewater s toxicity (municipal, industrial and shrimp pond effluents) released in the Estuarine Complex of Jundiaí- Potengi, Natal/RN, through chronic quantitative e qualitative toxicity tests using the test organism Mysidopsis Juniae, CRUSTACEA, MYSIDACEA (Silva, 1979). For this, a new methodology for viewing chronic effects on organisms of M. juniae was used (only renewal), based on another existing methodology to another testorganism very similar to M. Juniae, the M. Bahia (daily renewal).Toxicity tests 7 days duration were used for detecting effects on the survival and fecundity in M. juniae. Lethal Concentration 50% (LC50%) was determined by the Trimmed Spearman-Karber; Inhibition Concentration 50% (IC50%) in fecundity was determined by Linear Interpolation. ANOVA (One Way) tests (p = 0.05) were used to determinate the No Observed Effect Concentration (NOEC) and Low Observed Effect Concentration (LOEC). Effluents flows were measured and the toxic load of the effluents was estimated. Multivariate analysis - Principal Component Analysis (PCA) and Correspondence Analysis (CA) - identified the physic-chemical parameters better explain the patterns of toxicity found in survival and fecundity of M. juniae. We verified the feasibility of applying the only renewal system in chronic tests with M. Juniae. Most efluentes proved toxic on the survival and fecundity of M. Juniae, except for some shrimp pond effluents. The most toxic effluent was ETE Lagoa Aerada (LC50, 6.24%; IC50, 4.82%), ETE Quintas (LC50, 5.85%), Giselda Trigueiro Hospital (LC50, 2.05%), CLAN (LC50, 2.14%) and COTEMINAS (LC50, IC50 and 38.51%, 6.94%). The greatest toxic load was originated from ETE inefficient high flow effluents, textile effluents and CLAN. The organic load was related to the toxic effects of wastewater and hospital effluents in survival of M. Juniae, as well as heavy metals, total residual chlorine and phenols. In industrial effluents was found relationship between toxicity and organic load, phenols, oils and greases and benzene. The effects on fertility were related, in turn, with chlorine and heavy metals. Toxicity tests using other organisms of different trophic levels, as well as analysis of sediment toxicity are recommended to confirm the patterns found with M. Juniae. However, the results indicate the necessity for implementation and improvement of sewage treatment systems affluent to the Potengi s estuary

Haemulidae, modelo cariotípico de estase evolutiva

Conselho Nacional de Desenvolvimento Científico e Tecnológico