Extração de ferro da cera de carnaúba utilizando sistemas microemulsionados

The constant search for biodegradable materials for applications in several fields shows that carnauba wax can be a viable alternative in the manufacturing of biolubricants. Carnauba wax is the unique among the natural waxes to have a combination of properties of great importance. In previous studies it was verified the presence of metals in wax composition that can harm the oxidative stability of lubricants. Considering these factors, it was decided to develop a research to evaluate iron removal from carnauba wax, using microemulsion systems (Me) and perform the optimization of parameters, such as: extraction pH, temperature, extraction time, among others. Iron concentration was determined by atomic absorption and, to perform this analysis, sample digestion in microwave oven was used, showing that this process was very efficient. It was performed some analysis in order to characterize the wax sample, such as: attenuated total reflectance infrared spectroscopy (ATR-IR), thermogravimetry (TG), differential scanning calorimetry (DSC), energy dispersive X-ray fluorescence (EDXRF), scanning electron microscopy (SEM) and melting point (FP). The microemulsion systems were composed by: coconut oil as surfactant, n-butanol as cosurfactant, kerosene and/or heptanes as oil phase, distilled water as water phase. The pH chosen for this study was 4.5 and the metal extraction was performed in finite experiments. To evaluate Me extraction it was performed a factorial design for systems with heptane and kerosene as oil phase, also investigating the influence of temperature time and wax/Me ratio, that showed an statistically significant answer for iron extraction at 95% confidence level. The best result was obtained at 60°C, 10 hours contact time and 1: 10 wax/Me ratio, in both systems with kerosene and heptanes as oil phase. The best extraction occurred with kerosene as oil phase, with 54% iron removal

Extração do corante reactive blue 19 utilizando tensoativo não iônico

The generation of effluent from the finishing process in textile industry is a serious environmental problem and turned into an object of study in several scientific papers. Contamination with dyes and the presences of substances that are toxic to the environment characterize this difficult treatment effluent. Several processes have already been evaluated to remove and even degrade such pollutants are examples: coagulation-flocculation, biological treatment and advanced oxidative processes, but not yet sufficient to enable the recovery of dye or at least of the recovery agent. An alternative to this problem is the cloud point extraction that involves the application of nonionic surfactants at temperatures above the cloud point, making the water a weak solvent to the surfactant, providing the agglomeration of those molecules around the dyes molecules by affinity with the organic phase. After that, the formation of two phases occurred: the diluted one, poor in dye and surfactant, and the other one, coacervate, with higher concentrations of dye and surfactants than the other one. The later use of the coacervate as a dye and surfactant recycle shows the technical and economic viability of this process. In this paper, the cloud point extraction is used to remove the dye Reactive Blue from the water, using nonionic surfactant nonyl phenol with 9,5 etoxilations. The aim is to solubilize the dye molecules in surfactant, varying the concentration and temperature to study its effects. Evaluating the dye concentration in dilute phase after extraction, it is possible to analyze thermodynamic variables, build Langmuir isotherms, determine the behavior of the coacervate volume for a surfactant concentration and temperature, the distribution coefficient and the dye removal efficiency. The concentration of surfactant proved itself to be crucial to the success of the treatment. The results of removal efficiency reached values of 91,38%, 90,69%, 89,58%, 87,22% and 84,18% to temperatures of 65,0, 67,5, 70,0, 72,5 and 75,0°C, respectively, showing that the cloud point extraction is an efficient alternative for the treatment of wastewater containing Reactive Blue

Estudo dos parâmetros de extração de fenol de efluentes aquosos por um tensoativo não iônico

Environmental sustainability has become one of the topics of greatest interest in industry, mainly due to effluent generation. Phenols are found in many industries effluents, these industries might be refineries, coal processing, pharmaceutical, plastics, paints and paper and pulp industries. Because phenolic compounds are toxic to humans and aquatic organisms, Federal Resolution CONAMA No. 430 of 13.05.2011 limits the maximum content of phenols, in 0.5 mg.L-1, for release in freshwater bodies. In the effluents treatment, the liquid-liquid extraction process is the most economical for the phenol recovery, because consumes little energy, but in most cases implements an organic solvent, and the use of it can cause some environmental problems due to the high toxicity of this compound. Because of this, exists a need for new methodologies, which aims to replace these solvents for biodegradable ones. Some literature studies demonstrate the feasibility of phenolic compounds removing from aqueous effluents, by biodegradable solvents. In this extraction kind called "Cloud Point Extraction" is used a nonionic surfactant as extracting agent of phenolic compounds. In order to optimize the phenol extraction process, this paper studies the mathematical modeling and optimization of extraction parameters and investigates the effect of the independent variables in the process. A 32 full factorial design has been done with operating temperature and surfactant concentration as independent variables and, parameters extraction: Volumetric fraction of coacervate phase, surfactant and residual concentration of phenol in dilute phase after separation phase and phenol extraction efficiency, as dependent variables. To achieve the objectives presented before, the work was carried out in five steps: (i) selection of some literature data, (ii) use of Box-Behnken model to find out mathematical models that describes the process of phenol extraction, (iii) Data analysis were performed using STATISTICA 7.0 and the analysis of variance was used to assess the model significance and prediction (iv) models optimization using the response surface method (v) Mathematical models validation using additional measures, from samples different from the ones used to construct the model. The results showed that the mathematical models found are able to calculate the effect of the surfactant concentration and the operating temperature in each extraction parameter studied, respecting the boundaries used. The models optimization allowed the achievement of consistent and applicable results in a simple and quick way leading to high efficiency in process operation.

Extração enzimática de óleo e produção in situ de biodiesel a partir da Moringa oleífera Lam

With the growth and development of modern society, arises the need to search for new raw materials and new technologies which present the "clean" characteristic, and do not harm the environment, but can join the energy needs of industry and transportation. The Moringa oleifera Lam, plant originating from India, and currently present in the Brazilian Northeast, presents itself as a multi-purpose plant, can be used as a coagulant in water treatment, as a natural remedy and as a feedstock for biodiesel production. In this work, Moringa has been used as a raw material for studies on the extraction and subsequently in the synthesis of biodiesel. Studies have been conducted on various techniques of Moringa oil extraction (solvents, mechanical pressing and enzymatic), being specially developed an experimental design for the aqueous extraction with the aid of the enzyme Neutrase© 0.8 L, with the aim of analyzing the influence variable pH (5.5-7.5), temperature (45-55°C), time (16-24 hours) and amount of catalyst (2-5%) on the extraction yield. In relation to study of the synthesis of biodiesel was initially carried out a conventional transesterification (50°C, KOH as a catalyst, methanol and 60 minutes reaction). Next, a study was conducted using the technique of in situ transesterification by using an experimental design variables as temperature (30-60°C), catalyst amount (2-5%), and molar ratio oil / ethanol (1:420-1:600). The extraction technique that achieved the highest extraction yield (35%) was the one that used hexane as a solvent. The extraction using 32% ethanol obtained by mechanical pressing and extraction reached 25% yield. For the enzymatic extraction, the experimental design indicated that the extraction yield was most affected by the effect of the combination of temperature and time. The maximum yield obtained in this extraction was 16%. After the step of obtaining the oil was accomplished the synthesis of biodiesel by the conventional method and the in situ technique. The method of conventional transesterification was obtained a content of 100% and esters by in situ technique was also obtained in 100% in the experimental point 7, with a molar ratio oil / alcohol 1:420, Temperature 60°C in 5% weight KOH with the reaction time of 1.5 h. By the experimental design, it was found that the variable that most influenced the ester content was late the percentage of catalyst. By physico-chemical analysis it was observed that the biodiesel produced by the in situ method fell within the rules of the ANP, therefore this technique feasible, because does not require the preliminary stage of oil extraction and achieves high levels of esters

Extração, caracterização e avaliação bioativa do extrato de Rumex acetosa

Studies show the great influence of free radicals and other oxidants as responsible for aging and degenerative diseases. On the other hand, the natural phenolic compounds has shown great as antioxidants to inhibit lipid peroxidation and lipoxygenase in vitro. Among these, is highlighted trans-resveratrol ( 3,5,4 `- trihydroxystilbene ) phenolic compound , characterized as a polyphenol stilbene class. The vegetables popularly known as "Azedinha" (Rumex Acetosa) has trans-resveratrol in its composition and from this, the present work aimed to study on the supercritical extraction and conventional extraction (Soxhlet and sequential) in roots of Rumex Acetosa, evaluating the efficiency of extractive processes, antioxidant activity, total phenolic content and quantification of trans-resveratrol contained in the extracts. Extractions using supercritical CO2 as solvent, addition of co-solvent (ethanol) and were conducted by the dynamic method in a fixed bed extractor. The trial met a 23 factorial design with three replications at the central point, with the variable reply process yield and concentration of trans-resveratrol and pressure as independent variables, temperature and concentration of co-solvent (% v/v). Yields ( mass of dry extract / mass of raw material used ) obtained from the supercritical extraction ranged from 0,8 to 7,63 % , and the best result was obtained at 250 bar and 90 °C using the co-solvent 15% ethanol (% v/v). The value was calculated for YCER a flow rate of 1,0 ± 0,17 g/min resulting in 0,0469 CO2 ( g solute / g solvent ). The results of the mass yield varied between conventional extractions 0,78 % ( hexane) and 9,97 % (ethanol). The statistical model generated from the data of the concentration of trans-resveratrol performed as meaningful and predictive for a 95% confidence. GC analysis on HPLC (High Performance Liquid Chromatography), transresveratrol was quantified in all extracts and concentration values ranged between 0,0033 and 0,42 ( mg / g extract) for supercritical extracts and between 0,449 and 17,046 (mg / g extract) to conventional extractions and therefore, the Soxhlet extraction with ethanol for more selective trans-resveratrol than the supercritical fluid. Evaluation of antioxidant (radical method to sequester 2,2- diphenyl-1- picryl - hydrazyl - DPPH) the supercritical extracts resulted in EC50 values (concentration effective to neutralize 50% of free radicals) of between 7,89 and 18,43 mg/mL , while resulting in a Soxhlet extraction with EC50 values in the range of 6,05 and 7,39 mg/mL. As for quantification of the phenolic compounds (Method Spectrophotometer Folin-Ciocalteau) the supercritical extracts resulted in values between 85,3 and 194,79 mg GAE / g extract, whereas values derived from the Soxhlet extract resulted in values between 178,5 and 237,8 mg GAE / g extract. The high antioxidant activity can not be attributed solely to the presence of phenolic compounds, but the presence of other antioxidants in the existing Rumex acetosa

Extração, caracterização e aplicação do corante de urucum (Bixa orellana L.) no tingimento de fibras naturais

The increasing demand for natural dyes in place of synthetic ones is justified by the non-toxicity or low toxicity of the former. The synthetic dyes are associated with diseases like cancer as well as when released in the environment takes longer to degrade and the intermediates could be still more toxic. The Annatto (Bixa Orellana L.) is a carotenoid and one of the more important natural dyes used in the food industry. In the form of dye, it represents nearly 70% of the world natural dye production and 90% in Brazil. In the present work, annatto seeds were used of the species peruana paulista, which had nearly 2.1% of bixin. The process of dye extraction with ethyl alcohol showed 4% of dye in the form of powder with particle diameter of 28mm. The extraction process did not alter the chemical composition of the dye, which was confirmed by the electronic spectrum of absorption. Dyeings were carried out with different mordents to study the total colour difference as well as the wash fastness properties and friction fastness properties under wet and dry conditions. The samples treated with copper sulphate showed colour difference but at the same time showed better fastness results. The samples treated with resin (no formaldehyde) did not alter the colour significantly still better the fastness properties. From the results, it could be stated that the resin could be an alternative for heavy metallic mordents

Extração de metais pesados de efluentes da indústria do petróleo utilizando derivados de óleos vegetais como extratantes

The study of a promising alternative for the treatment of produced water from the oil industry envisaging its reuse was the focus of this work. Millions of liters of water are generated per day, containing heavy metals in low concentrations (< 0,15 mg/L for Pb, <0,04 mg/L for Cd, <0,04 mg/L for Ni). The technology applied to extract these metals from aqueous phase was the solvent extraction and the extratants used were vegetable oils originated from coconut oil. They can be used in natural form or as derivatives, known as MAC - Mixture of Carboxílics Acids. The determination of the heavy metal con¬centrations in a complex matrix was made by using the atomic absorption spectrometry technique (AAS). On the bench tests using synthetics aqueous solutions containing metals, vegetable oils showed no power to extract the metals studied. The extractant MAC was selective for the Pb> Cd> Ni, in the concentration of 8% in the same organic phase. In this condition, the lower efficiency of extraction obtained was 92% for the Pb, 69% for the Cd, in the range of pH ranging from 6 to 8. An experimental planning was conducted for continuous tests. The device used was called MDIF Misturador-Decantador à Inversão de Fases and the aqueous phase was produced water from Pólo Indutrial de Guamaré/RN . No correlation between the studied variables (concentration of metal, concentration of extratant and agitation in the mixing chamer) could be obtained, because of possible factors which occurred as: variation in the composition of the studied sample, phenomena of precipitation and complexation of metals in the reservoir of feed, solubility of extratant

Extração supercrítica do óleo de linhaça: construção do extrator, estudo de parâmetros de processo, avaliação química e antioxidante do produto

The aim of the present study was to extract vegetable oil from brown linseed (Linum usitatissimum L.), determine fatty acid levels, the antioxidant capacity of the extracted oil and perform a rapid economic assessment of the SFE process in the manufacture of oil. The experiments were conducted in a test bench extractor capable of operating with carbon dioxide and co-solvents, obeying 23 factorial planning with central point in triplicate, and having process yield as response variable and pressure, temperature and percentage of cosolvent as independent variables. The yield (mass of extracted oil/mass of raw material used) ranged from 2.2% to 28.8%, with the best results obtained at 250 bar and 50ºC, using 5% (v/v) ethanol co-solvent. The influence of the variables on extraction kinetics and on the composition of the linseed oil obtained was investigated. The extraction kinetic curves obtained were based on different mathematical models available in the literature. The Martínez et al. (2003) model and the Simple Single Plate (SSP) model discussed by Gaspar et al. (2003) represented the experimental data with the lowest mean square errors (MSE). A manufacturing cost of US$17.85/kgoil was estimated for the production of linseed oil using TECANALYSIS software and the Rosa and Meireles method (2005). To establish comparisons with SFE, conventional extraction tests were conducted with a Soxhlet device using petroleum ether. These tests obtained mean yields of 35.2% for an extraction time of 5h. All the oil samples were sterilized and characterized in terms of their composition in fatty acids (FA) using gas chromatography. The main fatty acids detected were: palmitic (C16:0), stearic (C18:0), oleic (C18:1), linoleic (C18:2n-6) and α-linolenic (C18:3n-3). The FA contents obtained with Soxhlet dif ered from those obtained with SFE, with higher percentages of saturated and monounsaturated FA with the Soxhlet technique using petroleum ether. With respect to α-linolenic content (main component of linseed oil) in the samples, SFE performed better than Soxhlet extraction, obtaining percentages between 51.18% and 52.71%, whereas with Soxhlet extraction it was 47.84%. The antioxidant activity of the oil was assessed in the β-carotene/linoleic acid system. The percentages of inhibition of the oxidative process reached 22.11% for the SFE oil, but only 6.09% for commercial oil (cold pressing), suggesting that the SFE technique better preserves the phenolic compounds present in the seed, which are likely responsible for the antioxidant nature of the oil. In vitro tests with the sample displaying the best antioxidant response were conducted in rat liver homogenate to investigate the inhibition of spontaneous lipid peroxidation or autooxidation of biological tissue. Linseed oil proved to be more efficient than fish oil (used as standard) in decreasing lipid peroxidation in the liver tissue of Wistar rats, yielding similar results to those obtained with the use of BHT (synthetic antioxidant). Inhibitory capacity may be explained by the presence of phenolic compounds with antioxidant activity in the linseed oil. The results obtained indicate the need for more detailed studies, given the importance of linseed oil as one of the greatest sources of ω3 among vegetable oils

Estudo da influência de tensoativos em sistemas microemulsionados na extração de gálio e alumínio

Gallium is an important material used in the electronic industry whose demand in the world market is increasing in view of its potential applications. A selective technique is required to allow for the production of the metal, separated from aluminium. Due to the fact that microemulsions constitute an attractive alternative to metal extraction procedures, microemulsified systems have been employed as gallium-selective extraction agents. Two surfactants have been synthesized: sodium 12-N,N-diethylamino-9,10-dihydroxyestearate (AMINE) and saponified coconut oil (SCO), both produced from raw materials readily available in Northeastern Brazil. Also, the commercial extraction agent KELEX-100, conventionally used with the same purpose, has been used in this work for comparison. The optimization of the extraction process with microemulsions was carried out by investigating the influence of some parameters, namely the type of cosurfactant, the cosurfactant/surfactant (C/S) ratio, the pH and concentration of metals in the aqueous phase. Pseudoternary diagrams, which are representative of the microemulsified systems under study, have been constructed in order to establish the boundaries of the regions where the several Winsor systems are formed. An experimental planning methodology (Scheffé Net) has been used to optimize the extraction. The extraction percentage values were as high as 100% for gallium and 99.99% for aluminium for the system with KELEX-100; 96.6% for gallium and 98.8% for aluminium for the system containing AMINE; and 88% for gallium and 85% for aluminium for the system with SCO. The microemulsified system chosen for presenting the best results in gallium extraction was composed by SCO/isoamyl alcohol/kerosene/Bayer licquor with a C/S ratio of 28 and pH of the original aqueous phase of 6.0. The selectivity that has not been observed in the extraction stage was accomplished in the reextraction process using HCl. For the KELEX-100 system, gallium was reextracted at 100% with 6M HCl and aluminium was reextracted at 100% with 0.8M HCl. For the AMINE system, the reextraction percentages were also 100% for both metals, using 6M HCl for gallium and 0.5M HCl for aluminium. On the other hand, the reextraction percentages for the system with SCO were as high as 84% for gallium and 92% for aluminium, with HCl in the same concentrations as those used in the AMINE system. Finally, an optimized system was applied in the gallium extraction process employing a reciprocating perforated-plates extractor. As a result, the metal content was extracted at a recovery rate of 95% for gallium and 97% for aluminium

Efeitos do ultrassom terapêutico sobre parâmetros morfométricos e clínicos e método de extração de metaloproteinases em sujeitos com úlceras venosas

Venous wounds cause physical, psychological and financial problems that impact the quality of life of patients. Treatment alternatives are investigated in order to reduce healthcare costs and improve quality of life of people affected by this problem. Physical resources, such as therapeutic ultrasound (US), are being considered in the treatment of ulcers as a potential healing agent. This study aimed to investigate the application of US as a treatment for venous ulcers. Subjects were divided into two groups: US group, where treatment consisted of 5 sessions of pulsed US (3 MHz, 1W/cm²) associated with compression and kinesiotherapy; and sham group, where individuals went through the same procedures, but with sham US therapy. Subjects were evaluated for wound size by planimetry and digital photography, visual analogue scale for pain, quality of life by the questionnaires SF- 36 and VEINES-QoL/Sym and enzymatic activity of metalloproteinases 2 and 9 by zymography. It was observed mean reduction in wound area of 41.58±53.8% for the US group and 63.47±37.2% for the placebo group, maintenance of quality of life scores in the US group and significant improvement (p<0.05) in the placebo group by VEINES questionnaire. It was observed decreased perception of pain in the placebo group. Sample feasibility for analysis of the protein activity of metalloproteinases 2 and 9 by zymography collected by swab method was also confirmed. Our data did not give us evidence to support the theory that the US accelerates healing of venous ulcers in a short-term analysis. However, we observed that standard care associated with compression therapy and kinesiotherapy were able to significantly shorten the progression of chronic venous ulcers

Uso de técnicas de Geoprocessamento e Sensoriamento Remoto no levantamento e integração de dados necessários a gestão ambiental dos campos de extração de óleo e gás do Canto do Amaro e Alto da Pedra no município de Mossoró - RN

The objective of this work is to identify, to chart and to explain the evolution of the soil occupation and the envirionment vulnerability of the areas of Canto do Amaro and Alto da Pedra, in the city of Mossoró-RN, having as base analyzes it multiweather of images of orbital remote sensors, the accomplishment of extensive integrated works of field to a Geographic Information System (GIS). With the use of inserted techniques of it analyzes space inserted in a (GIS), and related with the interpretation and analyzes of products that comes from the Remote Sensoriamento (RS.), make possible resulted significant to reach the objectives of this works. Having as support for the management of the information, the data set gotten of the most varied sources and stored in digital environment, it comes to constitute the geographic data base of this research. The previous knowledge of the spectral behavior of the natural or artificial targets, and the use of algorithms of Processing of Digital images (DIP), it facilitates the interpretation task sufficiently and searchs of new information on the spectral level. Use as background these data, was generated a varied thematic cartography was: Maps of Geology, Geomorfológicals Units soils, Vegetation and Use and Occupation of the soil. The crossing in environment SIG, of the above-mentioned maps, generated the maps of Natural and Vulnerability envirionmental of the petroliferous fields of I Canto do Amaro and Alto da Pedra-RN, working in an ambient centered in the management of waters and solid residuos, as well as the analysis of the spatial data, making possible then a more complex analysis of the studied area

Comparação entre metodologias de extração de HPAs em água utilizando um planejamento fatorial com quantificação no CG/EM

PAHs (Polycyclic Aromatic Hydrocarbons) are a group of organic substances which receive considerable attention because of the carcinogenic and mutagenic properties of some of them. It is therefore important to determine the PAHs in different environmental matrices. Several studies have shown the use of gas chromatography coupled to mass spectrometry as a technique for quantification of PAHs by presenting excellent detection limits. This study aimed to develop an analytical methodology for the determination of 16 PAHs listed by the USEPA, test two methods for extraction of PAHs in water from a 23 factorial design, quantify them through the analytical technique coupled to gas chromatography mass spectrometry (GC/MS) using the method developed, and finally apply the results in chemometrics. The sample was synthesized and subjected to tests of the 23 factorial design, which has the factors: the type of extraction technique (ultrasound and digester), the ratio solvent / sample (1:1 and 1:3) and the type of solvent (dichloromethane / hexane and acetone / dichloromethane). The responses of eight combinations of the factorial design were obtained from the quantification by external calibration in GC/MS. The quantification method was developed from an optimized adaptation of the USEPA Method 8270. We used the full scan mode as a way of acquiring the mass spectra of 16 PAHs. The time in which the samples were subjected to ultrasound was fixed at 10 min and held an investigation to establish the conditions of power and time in the digester. We had the best response in the investigation of the digester power of 100 watts and the time of six minutes. The factorial design of liquid-liquid extraction showed that the most representative factors were: the use of the digester as extraction technique, the ratio solvent / sample 1:1 and the use of a 1:1 mixture of dichloromethane / hexane as a solvent more suitable. These results showed that the 1:1 mixture of dichloromethane / hexane is an excellent mixture to recover the extraction of PAHs an aqueous sample using the microwave digester. The optimization of the method of separation, identification and quantification of PAHs in the GC/MS was valid for 16 PAHs present in each chromatogram of the samples

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)

Extração e análise da fração lipídica da microalga monoraphidium sp., síntese e caracterização do seu biodiesel

The cultivation of microalgae biomass in order to produce biodiesel arises as an extremely promising aspect, in that the microalgae culture includes short cycle of reproduction, smaller areas for planting and residual biomass rich in protein content. The present dissertation evaluates the performance and features, through spectrometry in the region of infrared with transformed Fourier (FTIR) and spectrometry in the region of UVvisible (UV-Vis), of the extracted lipid material (LM) using different techniques of cell wall disruption (mechanical agitation at low and at high spin and agitation associated with cavitation). The technique of gas chromatography (GC) brought to light the success of alkaline transesterification in the conversion of oil into methyl monoesters (MME), which was also analyzed by spectroscopic techniques (FTIR, proton magnetic resonance (1H NMR) and carbon (13C NMR). Through thermogravimetric analysis (TGA) were analyzed the lipid material (LM), biodiesel and the microalgae biomass. The method which provided the best results concerning the efficiency in extraction of the LP of Monoraphidium sp. (12,51%) was by mechanical agitation at high spin (14 000 rpm), for 2 hours being the ideal time, as shown by the t test. The spectroscopic techniques (1H NMR, 13C NMR and FTIR) confirmed that the structure of methyl monoesters and the chromatographic data (CG) revealed a high content of saturated fatty acid esters (about 70%) being the major constituent eicosanoic acid (33,7%), which justifies the high thermal stability of microalgae biodiesel. The TGA also ratified the conversion rate (96%) of LM into MME, pointing out the quantitative results compatible with the values obtained through GC (about 98%) and confirmed the efficiency of the extraction methods used, showing that may be a good technique to confirm the extraction of these materials. The content of LM microalgae obtained (12,51%) indicates good potential for using such material as a raw material for biodiesel production, when compared to oil content which can be obtained from traditional oil for this use, since the productivity of microalgae per hectare is much larger and requires an extremely reduced period to renew its cultivation

Eficiência de extração de cobre e níquel utilizando sistemas microemulsionados bifásicos e trifásicos

The environmental impact due to the improper disposal of metal-bearing industrial effluents imposes the need of wastewater treatment, since heavy metals are nonbiodegradable and hazardous substances that may cause undesirable effects to humans and the environment. The use of microemulsion systems for the extraction of metal ions from wastewaters is effective when it occurs in a Winsor II (WII) domain, where a microemulsion phase is in equilibrium with an aqueous phase in excess. However, the microemulsion phase formed in this system has a higher amount of active matter when compared to a WIII system (microemulsion in equilibrium with aqueous and oil phases both in excess). This was the reason to develop a comparative study to evaluate the efficiency of two-phases and three-phases microemulsion systems (WII and WIII) in the extraction of Cu+2 and Ni+2 from aqueous solutions. The systems were composed by: saponified coconut oil (SCO) as surfactant, n-Butanol as cosurfactant, kerosene as oil phase, and synthetic solutions of CuSO4.5H2O and NiSO4.6H2O, with 2 wt.% NaCl, as aqueous phase. Pseudoternary phase diagrams were obtained and the systems were characterized by using surface tension measurements, particle size determination and scanning electron microscopy (SEM). The concentrations of metal ions before and after extraction were determined by atomic absorption spectrometry. The extraction study of Cu+2 and Ni+2 in the WIII domain contributed to a better understanding of microemulsion extraction, elucidating the various behaviors presented in the literature for these systems. Furthermore, since WIII systems presented high extraction efficiencies, similar to the ones presented by Winsor II systems, they represented an economic and technological advantage in heavy metal extraction due to a small amount of surfactant and cosurfactant used in the process and also due to the formation of a reduced volume of aqueous phase, with high concentration of metal. Considering the reextraction process, it was observed that WIII system is more effective because it is performed in the oil phase, unlike reextraction in WII, which is performed in the aqueous phase. The presence of the metalsurfactant complex in the oil phase makes possible to regenerate only the surfactant present in the organic phase, and not all the surfactant in the process, as in WII system. This fact allows the reuse of the microemulsion phase in a new extraction process, reducing the costs with surfactant regeneration