Síntese e caracterização de tensoativos e estudo de equilíbrio de fase dos sistemas CnH2n+2/H2O/CnH2n+1COONa/But-OH

The growing utilization of surfactants in several different areas of industry has led to an increase on the studies involving solutions containing this type of molecules. Due to its amphiphilic nature, its molecule presents one polar part and one nonpolar end, which easily interacts with other molecules, being able to modify the media properties. When the concentration in which its monomers are saturated, the airliquid system interface is reached, causing a decrease in interfacial tension. The surfactants from pure fatty acids containing C8, C12 and C16 carbonic chains were synthesized in an alcoholic media using sodium hydroxide. They were characterized via thermal analysis (DTA and DTG) and via infrared spectroscopy, with the intention of observing their purity. Physical and chemical properties such as superficial tension, critical micelle concentration (c.m.c), surfactant excess on surface and Gibbs free energy of micellization were determined in order to understand the behaviour of these molecules with an aqueous media. Pseudo-ternary phase diagrams were obtained aiming to limit the Windsor equilibria conditions so it could be possible to understand how the surfactants carbonic chain size contributes to the microemulsion region. Solutions with known concentrations were prepared to study how the surfactants can influence the dynamic light scattering spectroscopy (DLS) and how the diffusion coefficient is influenced when the media concentration is altered. The results showed the variation on the chain size of the studied surfactant lipophilic part allows the conception of surfactants with similar interfacial properties, but dependent on the size of the lipophilic part of the surfactant. This variation causes the surfactant to have less tendency of microemulsionate oil in water. Another observed result is that the n-alcanes molecule size promoted a decrease on the microemulsion region on the obtained phase diagrams

Sistema microemulsionado: caracterização e aplicação na indústria de petróleo

Alkyl polyethoxylates are surfactants widely used in vastly different fields, from oil exploitation to pharmaceutical applications. One of the most interesting characteristics of these surfactants is their ability to form micellar systems with specific geometry, the so-called wormlike micelle. In this work, microemulsions with three distinct compositions (C/T = 40 %, 30 % and 25 %) was used with contain UNITOL / butanol / water / xylene, cosurfactant / surfactante (C/S) ratio equal to 0,5. The microemulsion was characterized by dynamic light scattering (DLS), capillary viscometry, torque rheometry and surface tensiometry experiments carried out with systems based on xylene, water, butanol (cosurfactant) and nonaethyleneglycolmonododecyl ether (surfactant), with fixed surfactant:cosurfactant:oil composition (with and without oil phase) and varying the overall concentration of the microemulsion. The results showed that a transition from wormlike micelles to nanodrops was characterized by maximum relative viscosity (depending on how relative viscosity was defined), which was connected to maximum effective diameter, determined by DLS. Surface tension suggested that adsorption at the air water interface had a Langmuir character and that the limiting value of the surfactant surface excess was independent of the presence of cosurfactant and xylene. The results of the solubilization of oil sludge and oil recovery with the microemulsion: C/S = 40%, 30% and 25% proved to be quite effective in solubilization of oil sludge, with the percentage of solubilization (%solubilization) as high as 92.37% and enhanced oil recovery rates up to 90.22% for the point with the highest concentration of active material (surfactant), that is, 40%.

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

Síntese enzimática de ésteres de açúcar: surfactantes e polímeros como novos materiais ambientalmente seguros

Sugar esters are substances which possess surfactant, antifungical and bactericidal actions and can be obtained through two renewable sources of raw materials: sugars and vegetable oils. Their excellent biodegradability, allied to lhe fact that they are non toxic, insipid, inodorous, biocompatible, no-ionic, digestible and because they can resist to adverse conditions of temperature, pH and salinity, explain lhe crescent use of these substances in several sections of lhe industry. The objective of this thesis was to synthesize and characterize surfactants and polymers containing sugar branched in their structures, through enzymatic transesterification of vinyl esters and sugars, using alkaline protease from Bacillus subtilis as catalyst, in organic medium (DMF).Three types of sugars were used: L-arabinose, D-glucose and sucrose and two types of vinyl esters: vinyl laurate and vinyl adipate. Aiming to reach high conversions from substrates to products for a possible future large scale industrial production, a serie of variables was optimized, through Design of Experiments (DOE), using Response Surface Methodology (RSM).The investigated variables were: (1) enzyme concentration; (2) molar reason of substrates; (3) water/solvent rale; (4) temperature and (5) time. We obtained six distinct sugar esters: 5-0-lauroyl L-arabinose, 6-0-lauroyl D-glucose, 1'-O-lauroyl sucrose, 5-0-vinyladipoyl L-arabinose, 6-0-vinyladipoyl D-glucose and 1 '-O-vinyladipoyl sucrose, being lhe last three polymerizable. The progress of lhe reaction was monitored by HPLC analysis, through lhe decrease of sugar concentration in comparison to lhe blank. Qualitative analysis by TLC confirmed lhe formation of lhe products. In lhe purification step, two methodologies were adopted: (1) chromatographic column and (2) extraction with hot acetone. The acylation position and lhe chemical structure were determined by 13C-RMN. The polymerization of lhe three vinyl sugar esters was possible, through chemical catalysis, using H2O2 and K2S2O8 as initiators, at 60°C, for 24 hours. IR spectra of lhe monomers and respective polymers were compared revealing lhe disappearance of lhe vinyl group in lhe polymer spectra. The molar weights of lhe polymers were determined by GPC and presented lhe following results: poly (5-0-vinyladipoyl L-arabinose): Mw = 7.2 X 104; PD = 2.48; poly (6-0-vinyladipoyl D-glucose): Mw = 2.7 X 103; PD = 1.75 and poly (1'-O-vinyladipoyl sucrose): Mw = 4.2 X 104; PD = 6.57. The six sugar esters were submitted to superficial tension tests for determination of the critical micelle concentrations (CMC), which varied from 122 to 167 ppm. Finally, a study of applicability of these sugar esters, as lubricants for completion fluids of petroleum wells was' accomplished through comparative analysis of lhe efficiency of these sugar esters, in relation to three commercial lubricants. The products synthesized in this thesis presented equivalent or superior action to lhe tested commercial products

Análise in vitro da atividade antifúngica e de toxicidade da anfotericina B pré-aquecida

The aim of this work was to evaluate how an aqueous micellar system containing Amphotericin B (AmB) and sodium deoxycholate (DOC) can be rebuilt after heating treatment. Also a review of the literature about the new physicochemical and biological properties of this new system was carried out. Afterwards, heated (AmB-DOC-H) and unheated (AmB-DOC) micelles were subsequently diluted at four different concentrations (50mg.L-1, 5mg.L-1, 0.5mg.L-1 and 0.05mg.L-1) to perform the physicochemical study and, then, the pharmacotoxicity assay, in which two cell models were used for the in vitro experiments, Red Blood Cells (RBC) from human donors and Candida parapisilosis (Cp). While potassium (K+) and hemoglobin leakage from RBC were the used parameters to evaluate the acute and chronic toxicity, respectively, the efficacy of AmB-DOC and AmB-DOC-H were assessed by K+ leakage and cell survival rate from Cp. The spectral study revealed a slight change on the aggregate peak from 327nm to 323nm for AmB-DOC-H compared to AmB-DOC. Concerning the toxicity, although AmB-DOC and AmB-DOC-H presented different behavior for hemoglobin leakage, AmB-DOC produced higher leakage than AmB-DOC-H at high concentrations (from 5mg.L-1) with values tending to zero. However, concerning K+ leakage, both AmB-DOC and AmB-DOC-H, showed similar profile for both cell models, RBC and Cp (p<0,05). AmB-DOC-H and AmB-DOC also revealed similar profile of activity against Cp with equivalent survival rate. In short, the AmB-DOC-H showed much less toxicity than AmB-DOC, but remained as active as the late one against fungal cell. Therefore, the results highlight the importance of this new procedure as a simple, inexpensive and safe alternative to produce a new kind of micelle system for treatment of systemic fungal infections

A oficina como método de desenvolvimento de projeto do produto aplicado à atividade jangadeira de Ponta Negra Natal-RN

The jangadas (brazilian fishing rafts) are rudimentary artisanal vessels intrinsic to the Northeast of Brazil. The fishery with jangadas is highly representative in the State of Rio Grande do Norte, and source of income for many families in addition to being a strong cultural icon. Is still alive despite the difficulties, bringing the history and customs of the fishermen and their people. However, is in process of extinction due to factors such as the low profitability of the activity, tourism and urbanization. From the understanding of activity involving their context and circumstances, based on identified problems regarding the conditions of use of jangadas as the unpredictability, the risk of accidents, poor working conditions, hygiene and housing, this dissertation aims to: analyzing the design of the jangada on the beach of Ponta Negra and its relationship with the activity in relation to health, safety, productivity and environment, and from such assessments, together with the results achieved during the workshops of the project, proposing a cart to move the raft, adapted to the local fisherman activity studied. To perform analysis of jangadeira activity, we used a methodology based on ergonomic work analysis - AET (WISNER, 1987; GUÈRIN, 2001; VIDAL, 2008, SALDANHA, 2004 and Carvalho, 2005). For data collection were used observational and interaction methods as a conversational action, verbalizations, photographs and video. It is emphasized that the search for solutions appropriate to the jangadeira activity was possible through the collaboration of several people, not just an informational level and understanding during the work activity, but effectively contributing to the making decisions

Oportunidades de melhoria ergonômica das exigências físicas da atividade jangadeira em Ponta Negra Natal-RN

The fishing is an activity with rafts marked by unpredictability, poor tools, physical stress, awkward postures, risk of accidents and incidents, which contribute to insecurity in the context of activity. This study aimed to contribute to reducing of physical effort and the biomechanical impacts in jangadeiro activity of artisanal fishing using jangadas on the beach of Ponta Negra, Natal-RN. To achieve this purpose the methodology of the Work Ergonomic Analysis - WEA became a reference using techniques such as observational and interactional observation notes, photographs, videos, action conversational and listening verbalizations. The resulting activity in health jangadeiro, discussed in this research were: static postural assessment, flexibility of movement of shoulder flexion-extension, flexibility of the hamstrings and lower back, grip and musculoskeletal pain. It was found from observations, interactions and activity analysis, that in carrying out fishing rafts are frequent awkward postures associated with demand for power and many are already feeling the jangadeiros reflections of years of life dedicated to this work. These have already adopted some measures to manage the activity, such as job rotation during the expedition of capture. Therefore, there is a need to expand these measures of activity management, as well as design and capabilities of the raft, seeking positive changes in the activity and consequently the quality of life jangadeiro

Desenvolvimento de sistemas a base de tensoativos para recuperação avançada de petróleo

Petroleum is a complex combination of various classes of hydrocarbons, with paraffinic, naphtenic and aromatic compounds being those more commonly found in its composition. The recent changes in the world scenario, the large reserves of heavy oils and also the lack of new discoveries of large petroleum fields are indications that, in the near future, the oil recovery by conventional methods will be limited. In order to increase the efficiency of the extraction process, enhanced recovery methods are cited in applications where conventional techniques have proven to be little effective. The injection of surfactant solutions as an enhanced recovery method is advantageous in that surfactants are able to reduce the interfacial tensions between water and oil, thus augmenting the displacement efficiency and, as a consequence, increasing the recovery factor. This work aims to investigate the effects of some parameters that influence the surfactant behavior in solution, namely the type of surfactant, the critical micelle concentration (CMC) and the surface and interface tensions between fluids. Seawater solutions containing the surfactants PAN, PHN and PJN have been prepared for presenting lower interfacial tensions with petroleum and higher stability under increasing temperature and salinity. They were examined in an experimental apparatus designed to assess the recovery factor. Botucatu (Brazil) sandstone plug samples were submitted to assay steps comprising saturation with seawater and petroleum, conventional recovery with seawater and enhanced recovery with surfactant solutions. The plugs had porosity between 29.6 and 32.0%, with average effective permeability to water of 83 mD. The PJN surfactant, at a concentration 1000% above CMC in water, had a higher recovery factor, causing the original oil in place to be recovered by an extra 20.97%, after conventional recovery with seawater

Formação de particulas submicrometricas de pmma por cristalização termica de solução polimérica

Polymer particles in the nanometer range are of fundamental interest today, especially when used as carrier systems in the controlled release of drugs, cosmetics and nutraceuticals, as well as in coating materials with magnetic properties. The main objective of the present study concerns the production of submicron particles of poly (methyl methacrylate) (PMMA) by crystallization of a polymer solution by thermally controlled cooling. In this work, PMMA solutions in ethanol and 1-propanol were prepared at different concentrations (1% to 5% by weight) and crystallized at different cooling rates (0.2 to 0.8 ° C / min) controlled linearly. Analysis of particle size distribution (DLS / CILAS) and scanning electron microscopy (SEM) were performed in order to evaluate the morphological characteristics of the produced particles. The results demonstrated that it is possible to obtain submicron polymer perfectly spherical particles using the technique discussed in this study. It was also observed that, depending on the cooling rate and the concentration of the polymer solution, it is possible to achieve high yield in the formation of submicron particles. In addition, preliminary tests were performed in order to verify the ability of this technique to form particulated carrier material with magnetic properties. The results showed that the developed technique can be an interesting alternative to obtain polymer particles with magnetic properties

Levantamento e avaliação de critérios para a ampliação de escala da produção de biossurfactantes utilizando melaço como substrato

Biosurfactants are amphiphilic molecules synthesized by microorganisms such as bacteria, yeast or filamented fungi cultivated in various carbon sources among sucrose and hydrocarbons. These molecules are composed by a hydrophilic and hydrophobic part. They operate mostly at interfaces of fluids of different polarities. Because of this characteristic, they are potentially employed in numerous industries, such as the textile, medical, cosmetics, food and mainly in the petrochemical ones. Therefore industry has interest in developing new biosurfactant production processes in high scale, in order to become them economically competitive when compared to synthetic biosurfactants. This work aims to evaluate the biosurfactant production applying a non-conventional substrate sugar cane molasses proceeding from the sugar industry thus reducing the production costs. The strain identified as AP029/GLIIA, isolated from oil wells in Rio Grande do Norte state and used in these experiments belongs to the culture collection of Antibiotics Department of UFPE. The fermentation were carried out using different conditions according to a factorial planning 24 with duplicate at center point, in which the studied factors were molasse concentration, nitrate concentration, agitation and aeration ratio. The experiments were performed in a shaker at 38ºC of temperature. Samples were withdrawn in regular periods of time of up to 72 hours of fermentation in order to analyze substrate consumption, cellular concentration, superficial tension, critical micelle dilution (CMD-1 e CMD-2) as well as extracelullar protein production. The results showed a production of 3,480 g/L of biomass, a reduction of 41% on superficial tension, 67% of substrate consumption and 0,2805 g/L of extracellular protein

Influência da adição de carga na marcha em esteira de crianças com paralisia cerebral hemiparética espástica

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior

Criar o próprio jogo didático ou apenas jogar? Efeitos de diferentes estratégias de ensino na motivação e aprendizado de ciências

The use of games as educational tools is common, however the effectiveness of games with educational purposes is still poorly known. In this study we evaluated three different low-cost teaching strategies make and play your own board game, just play an educational science game and make a poster to be exposed in the school regarding: (1) science learning; (2) use of deep learning strategies (DLS); and (3) intrinsic motivation. We tested the hypothesis that, in these three parameters evaluated, scores would be higher in the group that made and play their own game, followed respectively by the group that just played a game and the group that made a poster. The research involved 214 fifth-grade students from six elementary schools in Natal/RN. A group of students made and played their own science board game (N = 68), a second group played a science game (N = 75), and a third group made a poster to be exposed at school (N = 71). Our hypothesis was partly empirically supported, since there was no significant difference in science learning and in the use of DLS between the group that made their own game and the group that just played the game; however, both groups had significantly higher scores in science learning and in use of DLS than the group that made the poster. There was no significant difference in the scores of intrinsic motivation among the three experimental groups. Our results indicate that activities related to non-digital games can provide a favorable context for learning in the school environment. We conclude that the use of games for educational purposes (both making a game and just playing a game) is an efficient and viable alternative to teach science in Brazilian public school

Caracterização e aplicação de sistemas micelares e microemulsionados como inibidores de corrosão

Corrosion is an important phenomenon that frequently occurs in the oil industry, causing surface ablation, such as it happens on the internal surfaces of oil pipes. This work aims to obtain new systems to reduce this specific problem. The surfactants SDS, CTAB, and UNITOL L90 (in micellar and microemulsionated systems) were used as corrosion inhibitors. The systems were obtained using a C/S ratio of 2, butanol as cosorfactant, kerosene as oil phase and, as water phase, NaCl solutions of 0.5M with pH = 2, 4, and 7. Microemulsion regions were found both for direct and inverse micelles. SDS had the higher microemulsion region and the area was not dependent of pH. The study of micellization of these surfactans in the liquid-gas interface was carried out via the determination of CMC from surface tension measurements. Regarding microemulsionated systems, in the case of CTAB, CMC increased when pH was increased, being constant for SDS and UNITOL L90. Concerning micellar systems, increase in pH caused decrease and increase in CMC for SDC and CTAB, respectively. In the case of UNITOL L90, CMC was practically constant, but increased for pH = 4. The microemulsionated systems presented higher CMC values, except for UNITOL L90 L90. The negative values of free energy of micellization indicated that the process of adsorption was spontaneous. The results also indicated that, comparing microemulsionated to systems, adsorption was less spontaneous in the case of SDS and CTAB, while it did not change for UNITOL L90. SAXS experiments indicated that micelle geometry was spherical, existing also as halter and flat micelles, resuting in a better inght on the adsorption at the liquid-solid interface. Efficiency of corrosion inhibition as determined by electrochemical measurements, from corrosion currents calculated from Tafel extrapolation indicuting heat showed surfactants to be efficient even at low concentrations. Equilibrium isotherm data were fitted to the Freundlich model, indicating that surfactant adsorption occurs in the form of multilayers

Caracterização do processo de gelificação de soluções quitosana utilizando reometria e espalhamento dinâmico da luz

Gels consist of soft materials with vast use in several activities, such as in pharmaceutical industry, food science, and coatings/textile applications. In order to obtain these materials, the process of gelification, that can be physical (based on physical interactions) and/or chemical (based on covalent crosslinking), has to be carried out. In this work we used dynamic light scattering (DLS) and rheometry to monitor the covalent gelification of chitosan solutions by glutaraldehyde. Intensity correlation function (ICF) data was obtained from DLS and the exponential stretched Kohrausch-William-Watts function (KWW) was fitted to them. The parameters of the KWW equation, β, Γ and C were evaluated. These methods were effective in clarifying the process of sol-gel transition, with the emergence of non-ergodicity, and determining the range of gelation observed in about 10-20 minutes. The dependence between apparent viscosity on reaction time was used to support the discussion proposed.

Estudo da digestão de sedimento de curtume visando a extração do cromo por microemulsão

Leather tanneries generate effluents with high content of heavy metals, especially chromium, which is used in the mineral tanning process. Microemulsions have been studied in the extraction of heavy metals from aqueous solutions. Considering the problems related with the sediment resulting from the tanning process, due to its high content in chromium, in this work this sediment was characterized and microemulsion systems were applied for chromium removal. The extraction process consists in the removal of heavy metal ions present in an aqueous feeding solution (acid digestion solution) by a microemulsion system. First three different solid sludge digestion methods were evaluated, being chosen the method with higher digestion capacity. For this digestion method, seeking its optimization, was evaluated the influence of granule size, temperature and digestion time. Experimental results showed that the method proposed by USEPA (Method A) was the most efficient one, being obtained 95.77% of sample digestion. Regarding to the evaluated parameters, the best results were achieved at 95°C, 14 Mesh granule size, and 60 minutes digestion time. For chromium removal, three microemulsion extraction methods were evaluated: Method 1, in a Winsor II region, using as aqueous phase the acid digestion solution; Method 2, in a Winsor IV region, being obtained by the addition of the acid digestion solution to a microemulsion phase, whose aqueous phase is distilled water, until the formation of Winsor II system; and Method 3, in a Winsor III region, consisting in the formation of a Winsor III region using as aqueous phase the acid digestion solution, diluted in NaOH 0.01N. Seeking to optimize the extraction process only Method 1 (Systems I, II, and VIII) and Method 2 (System IX) were evaluated, being chosen points inside the interest regions (studied domains) to study the influence of contact time and pH in the extraction percentiles. The studied systems present the following compositions: System I: Surfactant Saponified coconut oil, Cosurfactant 1-Butanol, Oil phase Kerosene, Aqueous phase 2% NaCl solution; System II: Aqueous phase Acid digestion solution with pH adjusted using KOH (pH 3.5); System VIII: Aqueous phase - Acid digestion solution (pH 0.06); and System IX Aqueous phase Distilled water (pH 10.24), the other phases of Systems II, VIII and IX are similar to System I. Method 2 showed to be the more efficient one regarding chromium extraction percentile (up to 96.59% - pH 3.5). Considering that with Method 2 the microemulsion region only appears in the Winsor II region, it was studied Method 3 (System X) for the evaluation and characterization of a triphasic system, seeking to compare with a biphases system. System X is composed by: Surfactant Saponified coconut oil, Cosurfactant 1-Butanol, Oil phase Kerosene, Aqueous phase Acid digestion solution diluted with water and with its pH adjusted using 0.01N NaOH solution. The biphasic and triphasic microemulsion systems were analyzed regarding its viscosity, extraction efficiency and drop effective diameter. The experimental results showed that for viscosity studies the obtained values were low for all studied systems, the diameter of the drop is smaller in the Winsor II region, with 15.5 nm, reaching 46.0 nm in Winsor III region, being this difference attributed to variations in system compositions and micelle geometry. In chromium extraction, these points showed similar results, being achieved 99.76% for Winsor II system and 99.62% for Winsor III system. Winsor III system showed to be more efficient due to the obtaining of a icroemulsion with smaller volume, with the possibility to recover the oil phase in excess, and the use of a smaller proportion of surfactant and cosurfactant (C/S)