Desenvolvimento de uma unidade laboratorial para quantificação de BTX como poluentes atmosféricos, usando microextração em fase sólida

This dissertation aims the development of an experimental device to determine quantitatively the content of benzene, toluene and xylenes (BTX) in the atmosphere. BTX are extremely volatile solvents, and therefore play an important role in atmospheric chemistry, being precursors in the tropospheric ozone formation. In this work a BTX new standard gas was produced in nitrogen for stagnant systems. The aim of this dissertation is to develop a new method, simple and cheaper, to quantify and monitor BTX in air using solid phase microextraction/ gas chromatography/mass spectrometry (SPME/CG/MS). The features of the calibration method proposed are presented in this dissertation. SPME sampling was carried out under non-equilibrium conditions using a Carboxen/PDMS fiber exposed for 10 min standard gas mixtures. It is observed that the main parameters that affect the extraction process are sampling time and concentration. The results of the BTX multicomponent system studied have shown a linear and a nonlinear range. In the non-linear range, it is remarkable the effect of competition by selective adsorption with the following affinity order p-xylene > toluene > benzene. This behavior represents a limitation of the method, however being in accordance with the literature. Furthermore, this behavior does not prevent the application of the technique out of the non-linear region to quantify the BTX contents in the atmosphere.

Montagem e operação de um secador pneumático tipo flash

In this work, a pneumatic dryer has been designed and assembled in laboratory scale in order to study and evaluate configurations more efficient for application in drying of important materials of Northeast region in Brazil. The equipment was tested with drying of corn and rice grains, in conditions of temperature and air velocity at 80 oC and 35 m/s, respectively. For this type of dryer, it is recommended to work at temperatures above 200 °C and air velocity with higher dynamic pressure. However, even under operating conditions below what it is recommended, the results obtained with the pneumatic dryer were satisfactory. In addition, experiments of drying were performed by using a cabinet dryer (batch dryer) under the same conditions used in the pneumatic dryer. Flash one curves for the corn were fitted satisfactorily by applying of the Lewis model, while a better agreement was found for rice by using the Page model. The data obtained with both drying processes allowed to compare the performance between pneumatic and batch dryers. In respect to drying rate, the pneumatic dryer presented a similar performance to the batch dryer during processing with corn and a superior performance to the last one during processing with rice. Therefore, it was possible to verify that the pneumatic dryer assembled in this preliminar study can be applied for different materials and under different operating conditions

Degradação do fungicida tiofanato metílico pelo processo foto-Fenton em reatores anular e solar

Effluents from pesticide industries have great difficulty to decontaminate the environment and, moreover, are characterized by high organic charge and toxicity. The research group Center for Chemical Systems Engineering (CESQ) at the Department of Chemical Engineering of Polytechnical School of University of São Paulo and Department of Chemical Engineering, Federal University of Rio Grande do Norte have been applying the Advanced Oxidation Processes (AOP's) for the degradation of various types of pollutants. These processes are based on the generation of hydroxyl radicals, highly reactive substances. Thus, this dissertation aims to explore this process, since it has been proven to be quite effective in removing organic charge. Therefore, it was decided by photo-Fenton process applied to the degradation of the fungicide Thiophanate methyl in aqueous system using annular reactor (with lamp Philips HPLN 125W) and solar. The samples were collected during the experiment and analyzed for dissolved organic carbon (TOC) using a Shimadzu TOC (Shimadzu 5050A e VCP). The Doehlert experimental design has been used to evaluate the influence of ultraviolet radiation, the concentrations of methyl thiophanate (C12H14N4O4S2), hydrogen peroxide (H2O2) and iron ions (Fe2+), among these parameters, was considered the best experimental conditions, [Fe2+] = 0.6 mmol/L and [H2O2] = 0.038 mol/L in EXP 5 experiment and in SOL 5 experiment, obtaining a percentage of TOC removal of 60% in the annular reactor and 75% in the solar reactor

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

Diagnóstico regional do processo de queijo coalho comercializado em Natal/RN

Coalho cheese is a typical product of the Northeastern Brazil, which is consumed both raw and cooked. The present work aimed to study the characteristics of artisanal and industrial processes in the production of coalho cheese sold in Natal / RN in order to evaluate its quality and consumer s profile. Four artisanal cheeses plants were monitored and a questionnaire was sent to different cheese industries. Besides this, eight cheese samples (four artisanal and four industrial) were evaluated in regard to the microbiological quality, physical-chemical and sensory attributes. The sensory acceptance was evaluated by using 108 non-trained panelists by using the hedonic scale. The consumer s profile survey was applied to 400 consumers of coalho cheese. The lack of hygiene control was detected at the artisanal cheese production, which uses raw milk as its raw material. Research has shown that the industrialized cheeses are made from pasteurized milk provided by their own production or by a third party, as observed in cheese making dairies. In general, the results indicate variation in the manufacturing process of coalho cheese, which results in the lack of product standardization. Regarding the physical-chemical analysis, most artisanal and industrial samples presented moisture content between 36 and 40 %, classified as medium moisture cheese, which is the only parameter that showed no significant difference (p>0.05). However, the water activity (Aw), pH and acidity results differed significantly. All artisanal samples showed coliform contamination at 35 °C, which confirms the poor hygienic conditions. In regard to coliforms at 45 °C, 75 % of artisanal coalho cheese samples had value higher than 103 MPN / g, a value above the lawful limits determined by RDC nº 12. Fifty percent of industrial coalho cheese samples showed coagulase-positive Staphylococcus values above the limit allowed by the RDC nº 12, indicating poor handling. The sensory evaluation revealed that the taste was the only parameter that showed significant difference, and this difference was only between two industrial brands. The consumer s survey showed that the coalho cheese flavor is the most important reason for buying this kind of cheese. Although coalho cheese is mainly bought in supermarkets, open street markets and country shops are still important selling points. It is concluded that there is no coalho cheese standardization in the RN state, which leads to variations in physical-chemical and sensory attributes. Moreover, it is necessary greater hygiene control in the production and handling procedures of coalho cheese.

Efeito do ácido lático sobre as características microbiológicas, físico-químicas e sensoriais na carne do sol

The dried beef is a food traditionally eaten by Northeastern and has an extensive trade in the city of Natal-RN. It is usually produced in an empirical manner, without any standardization in production. Characterized as partially dehydrated meat product, so that the activity of water present is not sufficient to prevent microbial growth, degradation or the production of microbial toxins. The guarantee that the market dried beef is to provide a quality product hygienic, microbiological, physicochemical and sensory stable and adequate for the safety and consumer satisfaction, which has been increasingly attracted to food with natural preservatives. Thus, the meat industries are replacing the current seasonings and natural preservatives for similar, with it without affecting the shelf life of products. Lactic acid has been used to meet these requirements. In this sense, this study aimed to evaluate the effect of lactic acid on the physico-chemical, microbiological and sensory, besides knowing the consumer profile of dried meat of the City of Natal / RN. The results demonstrated that the use of lactic acid in concentrations of 1% and 2% during the processing of dried meat, had statistically significant effect (p < 0.05) on the physico-chemical (pH and water activity) and consequently reduced the microbial count does not alter the taste of the new product developed. Regarding the results on the consumer profile, it was found that the majority of respondents (71.75%) did not observe the presence of the stamp of the Federal Inspection Service (SIF) to buy this meat food that 81.55% of consumers check the hygiene conditions of the site and handlers, however, a large proportion of respondents not concerned with the guarantee of origin of typical regional products featuring a hazard to food safety for consumers of the city of Natal-RN

Inferência do ponto de orvalho em amostras de gás natural processado

This dissertation aims to assess the representativeness of the manual chilled mirror analyzer (model II Chanscope 13-1200-CN-2) used for the determination of condensed hydrocarbons of natural gas compared to the indirect methods, based on thermodynamic models equation of state. Additionally, it has been implemented in this study a model for calculating the dew point of natural gas. The proposed model is a modification of the equation of state of Peng-Robinson admits that the groups contribution as a strategy to calculate the binary interaction parameters kij (T) temperature dependence. Experimental data of the work of Brown et al. (2007) were used to compare the responses of the dew point of natural gas with thermodynamic models contained in the UniSim process simulator and the methodology implemented in this study. Then two natural gas compositions were studied, the first being a standard gas mixture gravimetrically synthesized and, second, a mixture of processed natural gas. These experimental data were also compared with the results presented by UniSim process simulator and the thermodynamic model implemented. However, data from the manual analysis results indicated significant differences in temperature, these differences were attributed to the formation of dew point of water, as we observed the appearance of moisture on the mirror surface cooling equipment

Modelagem e simulação da deposição de parafinas em escoamento turbulento

The flow assurance has become one of the topics of greatest interest in the oil industry, mainly due to production and transportation of oil in regions with extreme temperature and pressure. In these operations the wax deposition is a commonly problem in flow of paraffinic oils, causing the rising costs of the process, due to increased energy cost of pumping, decreased production, increased pressure on the line and risk of blockage of the pipeline. In order to describe the behavior of the wax deposition phenomena in turbulent flow of paraffinic oils, under different operations conditions, in this work we developed a simulator with easy interface. For that we divided de work in four steps: (i) properties estimation (physical, thermals, of transport and thermodynamics) of n-alkanes and paraffinic mixtures by using correlations; (ii) obtainment of the solubility curve and determination the wax appearance temperature, by calculating the solid-liquid equilibrium of parafinnic systems; (iii) modelling wax deposition process, comprising momentum, mass and heat transfer; (iv) development of graphic interface in MATLAB® environment for to allow the understanding of simulation in different flow conditions as well as understand the matter of the variables (inlet temperature, external temperature, wax appearance temperature, oil composition, and time) on the behavior of the deposition process. The results showed that the simulator developed, called DepoSim, is able to calculate the profile of temperature, thickness of the deposit, and the amount of wax deposited in a simple and fast way, and also with consistent results and applicable to the operation

Flotação por ar dissolvido para os minerais quartzo e feldspato utilizando coletores catiônicos

The pegmatite rocks in Rio Grande do Norte are responsible for much of the production of industrial minerals like quartz and feldspar. Quartz and feldspar are minerals from pegmatite which may occur in pockets with metric to centimetric dimensions or as millimetric to sub millimetric intergrowths. The correct physical liberation of the mineral of interest, in case of intergrowths, requires an appropriate particle size, acquired by size reduction operations. The method for treating mineral which has a high efficiency fines particles recovery is flotation. The main purpose of the present study is to evaluate the recovery of quartz and potassium feldspar using cationic diamine and quaternary ammonium salt as collectors by means of dissolved air flotation DAF. The tests were performed based on a central composite design 24, by which the influence of process variables was statistically verified: concentration of the quaternary ammonium salt and diamine collectors, pH and conditioning time. The efficiency of flotation was calculated from the removal of turbidity of the solution. Results of maximum flotation efficiency (60%) were found in the level curves, plotted in conditions of low concentrations of collectors (1,0 x 10-5 mol.L-1). These high flotation efficiencies were obtained when operating at pH 4 to 8 with conditioning time ranging from 3 to 5 minutes. Thus, the results showed that the process variables have played important roles in the dissolved air flotation process concerning the flotability of the minerals.

Modelagem da transferência de massa na remoção do óleo da água produzida por flotação em coluna com uso de tensoativos de origem vegetal

The treatment of oil produced water and its implications are continually under investigation and several questions are related to this subject. In the Northeast Region Brazil, the onshore reservoirs are, in its majority, mature oil fields with high production of water. As this oil produced water has high levels of oil, it cannot be directly discarded into the environment because it represents a risk for contamination of soil, water, and groundwater, or even may cause harm to living bodies. Currently, polyelectrolytes that promote the coalescence of the oil droplets are used to remove the dispersed oil phase, enhancing the effectiveness of the flotation process. The non-biodegradability and high cost of polyelectrolytes are limiting factors for its application. On this context, it is necessary to develop studies for the search of more environmentally friendly products to apply in the flotation process. In this work it is proposed the modeling of the flotation process, in a glass column, using surfactants derived from vegetal oils to replace the polyelectrolytes, as well as to obtain a model that represents the experimental data. In addition, it was made a comparative study between the models described in the literature and the one developed in this research. The obtained results showed that the developed model presented high correlation coefficients when fitting the experimental data (R2 > 0.98), thus proving its efficiency in modeling the experimental data.

Aplicação de microemulsão na recuperação de petróleo de reservatórios carbonáticos

The large investment in exploration activities offshore Brazil has generated new findings, generally in carbonate reservoirs, with different wettability conditions usually considered in the sandstone, strongly water-wet. In general, the carbonates reservoirs tend to be oil-wet, it difficult to mobilize of oil these reservoirs. These oils can be mobilized by different methods, or it may reverse the wettability of the surface of the reservoir and facilitate the flow of oil, improving production rates. Thus, the objective of this work was to study the influence of inversion on the wettability of the rock in the production and recovery of petroleum from carbonate reservoirs, using microemulsions. Three systems were chosen with different classes of surfactants: a cationic (C16TAB), an anionic (SDS) and nonionic (Unitol L90). Studies of the influence of salinity on the formation of the microemulsion as well as the characterization of fluids using density and viscosity measurements were also performed. To verify the potential of microemulsion systems in changing the wettability state of the chalk oil-wet to water-wet, contact angle measurements were performed using chalk of neutral-wet as surface material. Overall, with respect to the ionic character of the surfactants tested, the cationic surfactant (C16TAB) had a greater potential for reversal in wettability able to transform the rock wettability neutral to strongly water-wet, when compared with the anionic surfactant (SDS) and nonionic (Unitol L90), which showed similar behavior, improving the wettability of the rock to water. The microemulsions of all surfactants studied were effective in oil recovery, resulting in 76.92% for the system with C16TAB, 67.42% for the SDS and 66.30% for Unitol L90 of residual oil

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

Secagem do resíduo de acerola (Malphigia emarginata D.C.): estudo do processo e avaliação do impacto sobre o produto final

Brazil, one of the largest agricultural producers in the world, has managed in recent years to significantly improve its production. However, in response to this advance in the agro-industrial sector, the generation of agro-industrial residues has also increased. New technological alternatives have to be implemented in order to bring economic and rational use of this material and drying is one of the possible choices. Considering the great importance that bioactive compounds present for food science and technology, this research aims to evaluate the air-drying process of acerola residue in a tray convective drier under controlled temperature (60, 70 e 80ºC), air velocity (4.0, 5.0 e 6.0 m/s) and material width (0.5, 0.62 e 0.75 cm) by applying an experimental planning 23 + 3. Based on that, the impact on physical-chemical characteristics, color, bioactive compounds concentration and antioxidant activity of dried acerola waste was evaluated, having the in natura and freeze dried waste as control groups. Dried acerola residue presented natural pigments, mainly carotenoids (143.68 - 68.29 mg/g) and anthocyanins (290.92 - 90.11 mg/100 g), which explain the red and yellow instrumental color parameters observed. The acerola residue powder is also rich in phenolic compounds (3261.11 -2692.60 mgGAEeq/100g), proanthocyanidins (61.33-58.46 eq/100g), ascorbic acid (389.44 739.29 mg/100 g) and DPPH antioxidant activity (20.91 24.72 μg Trolox eq/g). Results show decreased concentration of phenolic compounds, anthocyanins, carotenoids, proanthocyanidins and ascorbic acid caused by the air-drying process. However, even after the observed drying losses, the acerola residue powder can be considered a high value food ingredient, considering the high bioactive compounds concentration found in the final product, as well as the colorimetric characterization and microbiological stability of the dried powder

Otimização do tempo e temperatura no processamento da gipsita oriunda dos cristalizadores da produção de sal para obter gesso de uso na construção civil

During the process of the salt production, the first the salt crystals formed are disposed of as industrial waste. This waste is formed basically by gypsum, composed of calcium sulfate dihydrate (CaSO4.2H2O), known as carago cru or malacacheta . After be submitted the process of calcination to produce gypsum (CaSO4.0,5H2O), can be made possible its application in cement industry. This work aims to optimize the time and temperature for the process of calcination of the gypsum (carago) for get beta plaster according to the specifications of the norms of civil construction. The experiments involved the chemical and mineralogical characterization of the gypsum (carago) from the crystallizers, and of the plaster that is produced in the salt industry located in Mossoró, through the following techniques: x-ray diffraction (XRD), x-ray fluorescence (FRX), thermogravimetric analysis (TG/DTG) and scanning electron microscopy (SEM) with EDS. For optimization of time and temperature of the process of calcination was used the planning three factorial with levels with response surfaces of compressive mechanical tests and setting time, according norms NBR-13207: Plasters for civil construction and x-ray diffraction of plasters (carago) beta obtained in calcination. The STATISTICA software 7.0 was used for the calculations to relate the experimental data for a statistical model. The process for optimization of calcination of gypsum (carago) occurred in the temperature range from 120° C to 160° C and the time in the range of 90 to 210 minutes in the oven at atmospheric pressure, it was found that with the increase of values of temperature of 160° C and time calcination of 210 minutes to get the results of tests of resistance to compression with values above 10 MPa which conform to the standard required (> 8.40) and that the X-ray diffractograms the predominance of the phase of hemidrato beta, getting a beta plaster of good quality and which is in accordance with the norms in force, giving a by-product of the salt industry employability in civil construction

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.