80 resultados para Águas residuárias : Recuperação
em Universidade Federal do Rio Grande do Norte(UFRN)
Resumo:
The tanning industries are those which transform animal hide or skin into leather. Due to the complexity of the transformation process, greater quantities of chemicals are being used which results in the generation of effluents with residual solids. The chromium in the residual waters generated by tanning tend to be a serious problem to the environment, therefore the recovery of this metal could result in the reduction of manufacturing costs. This metal is usually found in a trivalent form which can be converted into a hexavalent compound under acidic conditions and in the presence of organic matter. The present study was carried out with the objective to recover chromium through an extraction/re-extraction process using micro emulsions. Micro emulsions are transparent and thermodynamically stable system composed of two immiscible liquids, one forming the continuous phase and the other dispersed into micro bubbles, established by an interfacial membrane formed by surface active and co-surface active molecules. The process of recovering the chromium was carried out in two stages. The first, an extraction process, where the chromium was extracted in the micro emulsion phase and the aqueous phase in excess was separated. In the second stage, a concentrated acid was added to the micro emulsion phase rich in chromium in order to obtain a Winsor II system, where the water that formed in the micro emulsion phase separates into a new micro emulsion phase with a higher concentration of chromium, due to the lowering of the hydrophiles as well as the ionisation of the system. During the experimental procedure, a study was initiated with a synthetic solution of chromium sulphate passing onto the effluent. A Morris extractor was used in the extraction process. Tests were carried out according to the plan and the results were analysed by statistical methods in order to optimise the main parameters that influence the process: the total rate of flow (Q), stirring speed (w) and solvent rate (r). The results, after optimization, demonstrated that the best percentuals in relation to the chromium extraction (99 %) were obtained in the following operational conditions: Q= 2,0 l/h, w= 425 rpm and r= 0,375. The re-extraction was carried out at room temperature (28 °C), 40 °C and 50°C using hydrochloric acid (8 and 10 M) and sulphuric acid (8 M) as re-extracting agents. The results obtained demonstrate that the process was efficient enough in relation to the chromium extraction, reaching to re-extraction percentage higher than 95 %.
Resumo:
The present work had as objective to apply an experimental planning aiming at to improve the efficiency of separation of a new type of mixer-settler applied to treat waste water contaminated with oil. An unity in scale of laboratory, was installed in the Post-graduation Program of Chemical Engineering of UFRN. It was constructed in partnership with Petrobras S.A. This called device Misturador-Decantador a Inversão de Fases (MDIF) , possess features of conventional mixer-settler and spray column type. The equipment is composed of three main parts: mixing chamber; chamber of decantation and chamber of separation. The efficiency of separation is evaluated analyzing the oil concentrations in water in the feed and the output of the device. For the analysis one used the gravimetric method of oil and greases analysis (TOG). The system in study is a water of formation emulsified with oil. The used extractant is a mixture of Turpentine spirit hydro-carbons, supplied for Petrobras. It was applied, for otimization of the efficiency of separation of the equipment, an experimental planning of the composite central type, having as factorial portion fractionary factorial planning 2 5-2, with the magnifying of the type star and five replications in the central point. In this work, the following independents variables were studied: contents of oil in the feed of the device; volumetric ratio (O/A); total flowrate ; agitation in the mixing chamber and height of the organic bed. Minimum and maximum limits for the studied variables had been fixed according previous works. The analysis of variance for the equation of the empirical model, revealed statistically significant and useful results for predictions ends. The variance analysis also presented the distribution of the error as a normal distribution and was observed that as the dispersions do not depend on the levels of the factors, the independence assumption can be verified. The variation around the average is explained by 98.98%, or either, equal to the maximum value, being the smoothing of the model in relation to the experimental points of 0,98981. The results present a strong interaction between the variable oil contents in the feed and agitation in the mixing chamber, having great and positive influence in the separation efficiency. Another variable that presented a great positive influence was the height of the organic bed. The best results of separation efficiency had been obtained for high flowrates when associates the high oil concentrations and high agitation. The results of the present work had shown excellent agreement with the results carried out through previous works with the mixer-settler of phase inversion
Resumo:
At the cashew nut processing industry it is often the generation of wastewaters containing high content of toxic organic compounds. The presence of these compounds is due mainly to the so called liquid of the cashew nut (CNSL). CNSL, as it is commercially known in Brazil, is the liquid of the cashew nut. It looks like an oil with dark brown color, viscous and presents a high toxicity index due to the chemical composition, i.e. phenol compounds, such as anacardic acid, cardol, 2-methyl cardol and monophenol (cardanol). These compounds are bio resistant to the conventional treatments. Furthermore, the corresponding wastewaters present high content of TOC (total organic carbon). Therefore due to the high degree of toxicity it is very important to study and develop treatments of these wastewaters before discharge to the environmental. This research aims to decompose these compounds using advanced oxidative processes (AOP) based on the photo-Fenton system. The advantage of this system is the fast and non-selective oxidation promoted by the hydroxyl radicals (●OH), that is under determined conditions can totally convert the organic pollutants to CO2 and H2O. In order to evaluate the decomposition of the organic charge system samples of the real wastewater od a processing cashew nut industry were taken. This industry was located at the country of the state of Rio Grande do Norte. The experiments were carried out with a photochemical annular reactor equipped with UV (ultra violet) lamp. Based on preliminary experiments, a Doehlert experimental design was defined to optimize the concentrations of H2O2 and Fe(II) with a total of 13 runs. The experimental conditions were set to pH equal to 3 and temperature of 30°C. The power of the lamps applied was 80W, 125W and 250W. To evaluate the decomposition rate measures of the TOC were accomplished during 4 hours of experiment. According to the results, the organic removal obtained in terms of TOC was 80% minimum and 95% maximum. Furthermore, it was gotten a minimum time of 49 minutes for the removal of 30% of the initial TOC. Based on the obtained experimental results, the photo-Fenton system presents a very satisfactory performance as a complementary treatment of the wastewater studied
Resumo:
In wastewater treatment, activated sludge systems have been a technology widely applied as secondary treatment. During this step, which has a strong biological aspect, it is necessary to introduce oxygen supply for the maintenance of metabolic activity of the bacteria through the aerators. Aeration devices are responsible for most of the energy consumption in this stage. In this background, the influence of three aeration intensities (atmospheric air flow 3.5, 7.0 and 10.5 L.min-1) and the concentration of dissolved oxygen (DO) on the dimension of activated sludge flocs as well as on the efficiency of organic matter removal were assessed using a traditional activated sludge system which was fed with synthetic domestic wastewater. Samples were taken weekly from the three units that make up the system feed, aeration and storage tank in order to verify the Chemical Oxygen Demand (COD). It was established the process efficiency through a comparison between the initial and final COD. Besides the parameters already mentioned, this monitoring work on activated sludge batch system was also observed by Mixed Liquor Suspend Solids (MLSS), Volatile Suspend Solids (VSS), pH and temperature measures. The results have showed a maximum removal efficiency around 75% in the first aeration sequence and approximately 85% for the second and third one. For the first aeration, the DO concentration remained higher than 3.0 mg.L-1 and a diameter range from 10 to 60 μm was observed. In the second e third sequence, the DO concentration remained higher than 4.0 mg.L-1 with a diameter range of 10 until 200 μm. Although the sequence 1 and 2 have presented similar performances for organic matter removal, the sequence 2 promoted a regular floc size distribution and with lower values of Sludge Volumetric Index (SVI) meaning a better flocculating ability. In addition, the results reaffirmed what the literature has reported: higher DO concentrations produce flocs with greater dimensions
Resumo:
Petroleum Refinery wastewaters (PRW) have hart-to-degrade compounds, such as: phenols, ammonia, cyanides, sulfides, oils and greases and the mono and polynuclear aromatic hydrocarbons: benzene, toluene and xylene (BTX), acenaphthene, nitrobenzene and naphtalene. It is known that the microrganisms activity can be reduced in the presence of certain substances, adversely affecting the biological process of wastewater treatment. This research was instigated due the small number of studies regarding to this specific topic in the avaiable literature. This body of work ims to evaluate the effect of toxic substances on the biodegradability of the organic material found in PRW. Glucose was chosen as the model substrate due to its biodegradable nature. This study was divided into three parts: i) a survey of recalcitants compounds and the removal of phenol by using both biological and photochemical-biological processes; ii) biomass aclimation and iii) evaluation of the inhibitory effect certain compounds have on glucose biodegradation. The phenol degradation experiments were carried out in an activity sludge system and in a photochemical reactor. The results showed the photochemical-biological process to be more effective on phenol degradation, suggesting the superioruty of a combined photochemical-biological treatment when compared with a simple biological process for phenol removal from industry wastewaters. For the acclimation step, was used an activated sludge from industrial wastewaters. A rapid biomass aclimation to a synthetic solution composed of the main inhibitory compouns fpund in a PRW was obtained using the following operation condition: (pH = 7,0; DO ≥ 2,0 mg/L; RS = 20 days e qH = 31,2 and 20,4 hours), The last part was consisted of using respirometry evaluation toxicity effects of selected compounds over oxygen uptake rate to adaptated and non adaptated biomass in the presence of inhibitory compounds. The adaptated sludge showed greater degration capacity, with lower sensibility to toxic effects. The respirometry has proved to be very practical, as the techiniques used were simple and rapid, such as: Chemical Oxygen Demand (COD), Dissolved Oxygen (DO), and Volatile Suspended Solids (VSS). Using the latter it is possible to perform sludge selection to beggingthe process; thus allowing its use for aerobic treatment system`s behacior prediction
Resumo:
The technology of anaerobic reactors for sanitary wastewater treatment has been extensively developed in Brazil, and today it is practically consolidated. They present several advantages, such as low construction and operating costs, and low sludge production, the anaerobic reactors are an attractive alternative to minimize problematic lack of basic sanitation in urban areas, and also of the rural areas. The anaerobic filters have been widely used in Brazil. It produces an effluent with low concentration of organic matter and solids suspended, besides conserving the nutrients, therefore, it is good for use in irrigation, but the practice must be associated with knowledge of the pathogens presence. The main objective of this study was to evaluate the efficiency of anaerobic filters in removal faecal coliforms and helminth eggs, and to verify if the effluent can be used for agricultural purposes, according to the World Organization of Health (WHO, 1989). The protocol used to enumerate helminths eggs was the modified Bailenger method, (Ayres and Mara, 1996) recommended by WHO for evaluation of raw effluent and treated effluent. The membrane filtration method was utilized to determine the concentrations of faecal coliforms. Three different systems of sewer treatment composed by anaerobic filters were analyzed. The results, in a general analysis, showed that all the researched systems reached a larger removal than 93% to helminth eggs, resulting in an effluent with smaller average than 1 egg/L. One of these systems, Sistema RN, reached a larger removal than 99%, confirming the good performance of the anaerobic filters in removal helminths eggs. Even with low concentrations of eggs in the influent, the filters were capable to remove this parameter efficiently. About faecal coliforms, it was observed for all the researched systems an effluent with 106 CFU/100mL. The high concentrations to faecal coliforms in the effluent just allow reuse for restricted irrigation, in agreement with the guidelines of WHO. Although the researched systems have not removed faecal coliforms efficiently, the results indicated a good efficiency of the anaerobic filters in removal helminth eggs
Resumo:
In the urban areas of the cities a larger problem of destiny of effluents of the treatment stations is verified due to the junction of the sewages in great volumes. This way the hidroponic cultive becomes important, for your intensive characteristic, as alternative of reuse. This work presents as objective the improvement of the relation hidric-nutritious of the hidroponic cultive of green forage (FVH) using treaty sewage. The production of forage was with corn (Zea mays L.), using double hybrid AG1051, in the experimental field of the Federal University of Rio Grande do Norte (UFRN), in the city of Natal-RN-Brazil. The treated effluent essentially domestic had origin of anaerobic reactor, type decant-digester of two cameras in series followed by anaerobic filters drowned. The hidroponic experimental system was composed of 08 stonemasons, with limited contours for masonry of drained ceramic brick, measuring each one 2,5 meters in length for 1,0 meter of width, with inclination of 4% (m/m) in the longitudinal sense, leveled carefully, in way to not to allow preferential roads in the flow. These dimensions, the useful area of Isow was of 2 square meters. The stonemasons of cultive were waterproof (found and lateral) with plastic canvas of 200 micres of thickness, in the white color. Controlled the entrance and exit of the effluente in the stonemasons, with cycles of 12,68 minutes, it being water of 1,18 minutes. The treatments were constituted of: T1 - 24 hours/day under it waters with flow of 2 L/min; T2 - 12 hours/day under waters with flow of 4 L/min; T3 - 12 hours/day under waters with flow of 2 L/min; and T4 - 16 hours/day under waters with flow of 3 L/min. There were evaluations of the evapotranspirometric demand, of hidroponic system affluent and effluent seeking to characterize and to monitor physical-chemical parameters as: pH, temperature, Electric Conductivity and Fecal Coliforms. This last one was analyzed to the 11 days after isow (DAS) and to the 14 DAS. The others were analyzed daily. I sow it was accomplished in the dates of February 21, 2007, first experiment, and April 10, 2007, second experiment. The density of Isow was of 2 kg of seeds, germinated before 48 hours, for square meter of stonemason. The statistic delineament was it casual entirely with two repetitions, in two experiments. It was applied Tukey test of average to five percent of probability. The cultivation cycle was of 14 DAS with evapotranspirometric demand maximum, reached by T1, of 67,44 mm/day. The analyzed parameters, as mass of green matter - Kg, productivity-Kg/m2 and reason of production of seed FVH/Kg used in Isow, the best result was presented by T1, obtaining value of up to 19,01 Kg/m2 of cultive. Without significant difference, the T4 presented greats values with 16 hours under cycle of water. The Treatments 2 and 3 with 12 hours under cycle of water, they obtained inferior results to the other Treatments. As treatment system, came efficient in the reduction of the salinity. T1 obtained reduction medium maxim of 62,5%, to the 7 DAS, in the amount of salts that enter in the system in they are absorbed in the cultivation. The cultivation FVH acted reducing the microbiologic load. Significant percentile of reduction they were reached, with up to 90,23% of reduction of Units of Colonies (UFC), constituting, like this, the Hidroponic System as good alternative of treatment of effluents of Reactors of high Efficiency
Resumo:
The improper disposal of nitrogen in receiving water courses causes problems such as toxicity to living beings through the consumption of oxygen to meet the nitrogen demand, eutrophication and nitrate contamination of aquifers. For this reason it is often necessary to be carried out complementary treatment of wastewater to eliminate or reduce the concentration of this compound in the wastewater. The objective of this study is to evaluate the biological removal of nitrogen compounds using submerged aerated and anoxic filters as post-treatment of an anaerobic system, with low cost and innovative technology, which in previous studies has shown high removal efficiency of organic matter and great potential biological nitrogen compounds removal. The simple design with perforated hoses for air distribution and filling with plastic parts proved to be very efficient in relation to organic matter removal and nitrification. The system presented, in the best stage, efficiency in converting ammonia to nitrate by 71%, and produced a final effluent concentration below 10 mg / L of NH3-N. In addition, carbon concentration was removed by 77%, producing final effluent with 24 mg/L COD. However, denitrification in anoxic filter was not effective even with the addition of an external carbon source. There was a reduction of up to 56% of nitrogen caused by the process of simultaneous nitrification and denitrification (SND). The high voids space presented by this type of support material coupled with direct aeration of the sludge, allows the respiration of biomass retained between the endogenous phase, increased cell retention time and sludge retention capacity, producing a final effluent with turbidity less than 5 UT and total suspended solids around 5.0 mg/L
Ocorrência de compostos de interesse emergente no aquífero Dunas-Barreiras e nos esgotos de Natal/RN
Resumo:
The detection of emerging interest microcontaminants in environmental samples of surface water, groundwater, drinking water, wastewater and effluents from water and sewage treatment plants (WTP and STP), in many countries, suggests these pollutants are widespread in the environment, mainly in urban areas. This is a reason for great concern, since many of these compounds are potentially harmful for humans other living beings, and they are not efficiently removed in the majority of WTP and STP, which is exacerbated by precariousness of water supply and sanitation services. In Natal, like other Brazilian cities, the sewage system serves only part of the urban area (about 30%), so that the rest of the wastewater is infiltrated in the sandy soil of the region in cesspool-dry well systems. This has resulted in contamination of groundwater in the area (sand-dune barrier aquifer, which supplies more than 50% of the city population), which has been observed by the increase in nitrate concentration in supply wells. The vulnerability of the sanddune barrier aquifer, combined with reports of the presence of emerging interest microcontaminants in Brazil and worldwide, led to this research, which investigated the occurrence of fifteen microcontaminants in Natal groundwater and sewage. Samples were collected at five wells used for water supply, the raw sewage and the effluents from biological reactors from STP (UASB and activated sludge reactors). Two samples of each sample were taken, with one week apart between the samples. To determine the contaminants, extraction of aquifer water, and raw and treated sewage samples were performed, through the technique of using SPE Strata X cartridge (Phenomenex®) to the aquifer water, and Strata SAX and Strata X (Phenomenex® ) for samples of raw and treated sewage. Subsequently the extracts were analyzed using GC-MS technique. Much of the analyzed microcontaminants were detected in groundwater and sewage. The concentrations in groundwater are generally lower than those found in the sewers. Some of the compounds (estrone, estradiol, bisphenol A, caffeine, diclofenac, naproxen, paracetamol and ibuprofen) are partially removed at STP.
Resumo:
This paper evaluate the performance of a Wastewater Treatment Plant (WWTP) in sequential batch activated sludge modality with tertiary treatment step, located in high temperature region. It also presents the analysis of organic matter’s removal and the evaluation of sludge sedimentation conditions through reactors in bench scale, fed with different substrate’s and biomass’ concentrations, from the WWTP in study. The results showed high efficiency and stability of the treatment process using Sequential Batch Reactors for domestic sewage, even with sudden changes of organic and hydraulic load, reaching more than 90% of efficiency in the removal of biodegradable organic matter. The removal of organic matter and sedimentation tests in bench reactors showed the good performance in respect of the organic matter’s removal, however, the high concentration of micro-organism results in a lower sludge sedimentation rate, which can compromise the quality of the final effluent. The relation Food/Microorganism in the conditions of the WWTP’s current operation showed a value of 0.06 gCOD/gVSS.d. and zonal sedimentation velocity of 0.59 m/h, the great ratio of the concentration of the substrate by biomass concentration, which obtained the maximum operational efficiency, showed a value of 0.09 gCOD/gVSS.d. and zonal sedimentation velocity of 1.4 m/h.
Resumo:
This paper evaluate the performance of a Wastewater Treatment Plant (WWTP) in sequential batch activated sludge modality with tertiary treatment step, located in high temperature region. It also presents the analysis of organic matter’s removal and the evaluation of sludge sedimentation conditions through reactors in bench scale, fed with different substrate’s and biomass’ concentrations, from the WWTP in study. The results showed high efficiency and stability of the treatment process using Sequential Batch Reactors for domestic sewage, even with sudden changes of organic and hydraulic load, reaching more than 90% of efficiency in the removal of biodegradable organic matter. The removal of organic matter and sedimentation tests in bench reactors showed the good performance in respect of the organic matter’s removal, however, the high concentration of micro-organism results in a lower sludge sedimentation rate, which can compromise the quality of the final effluent. The relation Food/Microorganism in the conditions of the WWTP’s current operation showed a value of 0.06 gCOD/gVSS.d. and zonal sedimentation velocity of 0.59 m/h, the great ratio of the concentration of the substrate by biomass concentration, which obtained the maximum operational efficiency, showed a value of 0.09 gCOD/gVSS.d. and zonal sedimentation velocity of 1.4 m/h.
Resumo:
Increasing concern with the environment, in addition to strict laws, has induced the industries to find altenatives to the treatment of their wastes. Actually, the oil industry has sought solutions to overcome a big environmental problem, i.e., oil field produced water being discharged to the sea. These effluents have organic compounds dissolved, such as polycyclic aromatic hydrocarbons, phenols, benzene, toluene, ethylbenzene and xylenes (BTEX). These compounds are difficult to be removed and have high toxicity. The advanced oxidation processes - AOP are effective to degradation of these organic compounds, because they generate hydroxyl radicals with high potential of oxidation. This work includes the reactor photochemical development applied in the photodegradation treatment (by photo-Fenton process) of wastewaters containing organic compounds dissolved, aiming at treatment and recovery the oil field produced water. The studied reactor allowed the evaluation of two ultraviolet radiation sources that is the main factor to describe the feasibility of the photo¬Fenton treatment, i.e., sun and black light fluorescent lamps, and other relevant variables the process: concentration of reagents, irradiated area and also various reactor configurations to maximize the use of radiation. The organic matter degradation was verified with samples collected during the experimental and analyzed with a total organic carbon analyzer (TOC), which expressed the results in terms of mgC/L. The solar radiation was more effective than radiation from the lamps. it's an important factor for the operation costs cutting. Preliminary experiments applied to oil field produced water treatment have showed satisfactory results, reducing up to 76 % of organic matter
Resumo:
Increasing concern with the environment, in addition to strict laws, has induced the industries to find alternatives to the treatment of their wastes. Actually, the oil industry has sought solutions to overcome a big environmental problem, i.e., oil field produced water being discharged to the sea. These effluents have organic compounds dissolved, such as polycyclic aromatic hydrocarbons, phenols, benzene, toluene, ethylbenzene and xylenes (BTEX). These compounds are difficult to be removed and have high toxicity. The advanced oxidation processes - AOP are effective to degradation of these organic compounds, because they generate hydroxyl radicals with high potential of oxidation. This work includes the reactor photochemical development applied in the photodegradation treatment (by photo-Fenton process) of wastewaters containing organic compounds dissolved, aiming at treatment and recovery the oil field produced water. The studied reactor allowed the evaluation of two ultraviolet radiation sources that is the main factor to describe the feasibility of the photo- Fenton treatment, i.e., sun and black light fluorescent lamps, and other relevant variables the process: concentration of reagents, irradiated area and also various reactor configurations to maximize the use of radiation. The organic matter degradation was verified with samples collected during the experimental and analyzed with a total organic carbon analyzer (TOC), which expressed the results in terms of mgC/L. The solar radiation was more effective than radiation from the lamps. It's an important factor for the operation costs cutting. Preliminary experiments applied to oil field produced water treatment have showed satisfactory results, reducing up to 76 % of organic matter
Resumo:
This study presents the Environmental Sensibility Mapping to oil spillings on the Potengi estuary - RN and neighboring coastline through remote sensing data, collecting, treatment and integration of the geomorphologic, oceanographic (temperature, salinity, density, direction and intensity), meteorological (wind speed and direction) and high resolution seismic (bathymetry and sonography) data. The Potengi river estuary is located on the eastern coastline of the Rio Grande do Norte State, being inserted in the geological context for the coastal Pernambuco-Paraíba basin and spreading over 18 km; it shelters the Natal harbor zone and an oil terminal, centralizing, therefore, important oil transport operations that can cause accidental spillings. Under the oceanographic point of view, the Potengi estuary is characterized by the absence of any expressive thermic stratification, being classified as partially mixed, B type according to Pritchard (1955), and 2 type in conformity to the stratification-circulation diagram by Hansen & Rattray (1966). Two main wind systems are responsable for the formation of wave sets that occur in the area. The dynamic tide presents, in the Natal Harbor, mean amplitude in spring and quadrature tides, with around 2.8 and 2m, respectively. The mechanism of saline tide mixing was defined through the salinity which is the main parameter for the identification of this mechanism. Important variations of the salinity mean values (36.32 psu), temperature (28.11ºC) and density (22.96 kg/m3) in the estuarine waters presented features belonging to low latitude regions. The water temperature follows the air temperature variations, in the region, with expressive daily amplitudes. In this study, the identification of the estuarine bed morphology through bathymetric and sonographic analysis, had the purpose to evaluate the influence of the superficial and bottom currents for the bottom shaping. In this way, the use of the side scan sonar showed, to be very useful in the identification of the bottom morphology and its relationship with the predominant action of the tidal currents in the Potengi estuary. Besides, it showed how the sonograms can be a support to the comparison of the several patterns derived from the local hydrodynamic variations. The holocene sediments, which fill the estuarine channel, are predominantly sandy, varying from selected, sometimes silty. The sedimentation is controlled by the environmental hydrodynamic conditions, being recognized two important textural facies: Muddy Facies and Sandy Facies. The distribution of these textural facies apparently oscillates owing to the tidal cycle and flow intensity. Each one of the above mentioned data was integrated in a Geographic Information System (GIS), from which was produced the Environmental Sensibility Map to oil spillings with Coastal Sensibility Index (CSI) to the Potengi estuary. The integrated analysis of these data is essential to oil spilling contingency plans, in order to reduce the spilling environmental consequences and to make efficient the endeavours of contention and cleaning up/removal on the Natal Harbor. This study has the aim to collaborate for the increase of informations about the estuarine environment and contribute to a better management of the question: environment/polluting loads
Resumo:
The determination and monitoring of metallic contaminants in water is a task that must be continuous, leading to the importance of the development, modification and optimization of analytical methodologies capab le of determining the various metal contaminants in natural environments, because, in many cases, the ava ilable instrumentation does not provide enough sensibility for the determination of trace values . In this study, a method of extraction and pre- concentration using a microemulsion system with in the Winsor II equilibrium was tested and optimized for the determination of Co, Cd, P b, Tl, Cu and Ni through the technique of high- resolution atomic absorption spectrometry using a continuum source (HR-CS AAS). The optimization of the temperature program for the graphite furnace (HR-CS AAS GF) was performed through the pyrolysis and atomization curves for the analytes Cd, Pb, Co and Tl with and without the use of different chemical modifiers. Cu and Ni we re analyzed by flame atomization (HR-CS F AAS) after pre-concentr ation, having the sample introduction system optimized for the realization of discrete sampling. Salinity and pH levels were also analyzed as influencing factors in the efficiency of the extraction. As final numbers, 6 g L -1 of Na (as NaCl) and 1% of HNO 3 (v/v) were defined. For the determination of the optimum extraction point, a centroid-simplex statistical plan was a pplied, having chosen as the optimum points of extraction for all of the analytes, the follo wing proportions: 70% aqueous phase, 10% oil phase and 20% co-surfactant/surfactant (C/S = 4). After extraction, the metals were determined and the merit figures obtained for the proposed method were: LOD 0,09, 0,01, 0,06, 0,05, 0,6 and 1,5 μg L -1 for Pb, Cd, Tl, Co, Cu and Ni, re spectively. Line ar ranges of ,1- 2,0 μg L -1 for Pb, 0,01-2,0 μg L -1 for Cd, 1,0 - 20 μg L -1 for Tl, 0,1-5,0 μg L -1 for Co, 2-200 μg L -1 and for Cu e Ni 5-200 μg L -1 were obtained. The enrichment factors obtained ranged between 6 and 19. Recovery testing with the certified sample show ed recovery values (n = 3, certified values) after extraction of 105 and 101, 100 and 104% for Pb, Cd, Cu and Ni respectively. Samples of sweet waters of lake Jiqui, saline water from Potengi river and water produced from the oil industry (PETROBRAS) were spiked and the recovery (n = 3) for the analytes were between 80 and 112% confirming th at the proposed method can be used in the extraction. The proposed method enabled the sepa ration of metals from complex matrices, and with good pre-concentration factor, consistent with the MPV (allowed limits) compared to CONAMA Resolution No. 357/2005 which regulat es the quality of fresh surface water, brackish and saline water in Brazil.