Avaliação de metodologia de preparo de amostra de petróleo por digestão ácida auxiliada por microondas para determinação de metais por ICP-OES

This project describes a methodology optimization that would allow for a more efficient microwave assisted digestion process for petroleum samples. With the possible chance to vary various factors at once to see if any one factor was significant enough in the answers, experimental planning was used. Microwave assisted digestion allows, through the application of potency, an increasing number of collisions between the HNO3 and H2O2 molecules, favoring sample opening for complex matrixes. For this, a 24 factorial experimental planning was used, varying potency, time and the volumes for HNO3 65% and H2O2 30%. To achieve the desired answers, several elements were monitored (C, Cu, Cr, Fe, Ni, Zn and V) through Inductively coupled plasma atomic emission spectroscopy (ICP-OES). With this initial study it was noticed that the HNO3 was not a significant factor for any of the statistical studies for any of the analytes and the other 3 factors and their interactions showed statistical significance. A Box Behnken experimental planning was used taking in consideration 3 factors: H2O2 volume, time (min) and Potency (W), Nitric Acid kept at 4mL for a mass of 0,1g of petroleum. The results were extremely satisfying showing higher efficiency in the digestion process and taking in a responsibility between the answers for each analyte and the carbon monitoring was achieved in the following conditions: 7mL of H2O2, 700 Watts of potency and a reaction time of 7 minutes with 4mL de HNO3 for a mass of 0,1g of petroleum. The optimized digestion process was applied to four different petroleum samples and the analytes determined by ICP-OES

Avaliação de metodologia de preparo de amostra de petróleo por digestão ácida auxiliada por microondas para determinação de metais por ICP-OES

This project describes a methodology optimization that would allow for a more efficient microwave assisted digestion process for petroleum samples. With the possible chance to vary various factors at once to see if any one factor was significant enough in the answers, experimental planning was used. Microwave assisted digestion allows, through the application of potency, an increasing number of collisions between the HNO3 and H2O2 molecules, favoring sample opening for complex matrixes. For this, a 24 factorial experimental planning was used, varying potency, time and the volumes for HNO3 65% and H2O2 30%. To achieve the desired answers, several elements were monitored (C, Cu, Cr, Fe, Ni, Zn and V) through Inductively coupled plasma atomic emission spectroscopy (ICP-OES). With this initial study it was noticed that the HNO3 was not a significant factor for any of the statistical studies for any of the analytes and the other 3 factors and their interactions showed statistical significance. A Box Behnken experimental planning was used taking in consideration 3 factors: H2O2 volume, time (min) and Potency (W), Nitric Acid kept at 4mL for a mass of 0,1g of petroleum. The results were extremely satisfying showing higher efficiency in the digestion process and taking in a responsibility between the answers for each analyte and the carbon monitoring was achieved in the following conditions: 7mL of H2O2, 700 Watts of potency and a reaction time of 7 minutes with 4mL de HNO3 for a mass of 0,1g of petroleum. The optimized digestion process was applied to four different petroleum samples and the analytes determined by ICP-OES

Desenvolvimento de metodologia de extração e pré-concentração utilizando sistema microemulsionado para determinação de Cd, Co, Cu, Ni, Pb e Tl em águas naturais e produzidas por HR-CS AAS

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.

Avaliação da influência da matéria orgânica, na determinação quantitativa de metais em amostras de sedimento, por espectrometria de absorção atômica e análise de metais traços por fluorescência de raios-X

The proposal of this work is to evaluate the influence of the organic matter on the results of the analyses of the metals (Zn, Pb, Al, Cu, Cr, Fe, Cd e Ni) for Atomic Absorption Spectrometry (AAS), so much in the extraction stage as in the reading using for that the chemometrics. They were used for this study sample of bottom sediment collected in river Jundiaí in the vicinity of the city of Macaíba-RN, commercial humus and water of the station of treatment of sewer of UFRN. Through the analyses accomplished by EAA it was verified that the interference of the organic matter happens in the extraction stage and not in the reading. With relationship to the technique of X Ray Fluorescence Spectrometry (XRFS), the present work has as intended to evaluate the viability of this technique for quantitative analysis of trace metals (Cr, Ni, Cu, Zn, Rb, Sr and Pb) in having leached obtained starting from the extraction with acqua regia for an aqueous solution. The used samples constitute the fine fraction (<0.063 mm) of sediments of swamp of the river Jundiaí. The preparation of tablets pressed starting from the dry residue of those leached it allowed your analysis in the solid form. This preliminary study shows that, in the case of the digestion chemistry partially of the fine fractions of bottom sediments used for environmental studies, the technique of applied EFRX to the analysis of dry residues starting from having leached with acqua regia, compared her it analyzes of the leached with ICP-OES, it presents relative mistakes for Cu, Pb, Sr and Zn below 10%

Determinação da concentração de metais no material particulado (PM10 e PM2,5) do ar atmosférico em uma área urbana da cidade do Natal – RN

This study aimed to assess ambient air quality in a urban area of Natal, capital of Rio Grande do Norte (latitude 5º49'29 '' S and longitude 35º13'34'' W), aiming to determine the metals concentration in particulate matter (PM10 and PM2,5) of atmospheric air in the urban area o the Natal city. The sampling period for the study consisted of data acquisition from January to December 2012. Samples were collected on glass fiber filters by means of two large volumes samplers, one for PM2,5 (AGV PM 2,5) and another for PM10 (PM10 AGV). Monthly averages ranged from 8.92 to 19.80 g.m-3 , where the annual average was 16,21 g.m-3 for PM10 and PM2,5 monthly averages ranged from 2,84 to 7,89 g.m -3 , with an annual average of 5,61 g.m-3 . The results of PM2,5 and PM10 concentrations were related meteorological variables and for information on the effects of these variables on the concentration of PM, an exploratory analysis of the data using Principal Component Analysis (PCA) was performed. The results of the PCA showed that with increasing barometric pressure, the direction of the winds, the rainfall and relative humidity decreases the concentration of PM and the variable weekday little influence compared the meteorological variables. Filters containing particulate matter were selected in six days and subjected to microwave digestion. After digestion samples were analyzed by with Inductively Coupled Plasma Mass Spectrometry (ICP-MS). The concentrations for heavy metals Vanadium, Chromium, Manganese, Nickel, Copper, Arsenic and lead were determined. The highest concentrations of metals were for Pb and Cu, whose average PM10 values were, respectively, 5,34 and 2,34 ng.m-3 and PM2,5 4,68 and 2,95 ng.m-3 . Concentrations for metals V, Cr, Mn, Ni, and Cd were respectively 0,13, 0,39, 0,48, 0,45 and 0,03 ng.m-3 for PM10 fraction and PM2,5 fraction, 0,05, 0,10, 0,10, 0,34 and 0,01 ng.m-3. The concentration for As was null for the two fractions

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

Diagnóstico ambiental das águas do estuário Jundiaí-Potengi pela determinação dos índices de qualidade da água e toxidez

This study is an environmental diagnosis of the Jundiaí-Potengi/RN estuarine system waters, using calculations of pollution indicator indices such as the Water Quality Index (WQI) and the Toxicity Index (TI). The samples were collected at twelve points on the estuary, at high and low tide, between August and November 2007, over four campaigns. The study area, located in a high impact region, has various activities on its banks such as: discharge of untreated or undertreated domestic and industrial sewage, shrimp farming, immunizer stabilization lakes, riverside communities, etc. All the parameters analyzed were compared to the limits of CONAMA Resolution No. 357 of 2005 for healthy and saline Class 1 waters. The results found prove the impact caused by various activities, mainly the parameters related to the presence of organic material, such as DQO, DBO, COT and thermotolerant colliforms. The IQA for most of the collection points was of medium quality. For the metals, although values above the Resolution limits were found, most of them were lower than the detection limits of ICP-OES used, indicating that they tend to be transported by the dynamic of the tides or rainfall and are deposited in bottom sediments, resulting in a TI of 1.0 in this water, when they are absent, which occurs in most cases, or 0.0, when heavy metals are found in these waters

Determinação da composição química do molusco anadara notabilis encontrado em Galinhos no Rio Grande do Norte

Tendo em vista a grande biodiversidade existente no litoral brasileiro, onde muitas espécies ainda são pouco conhecidas, inclusive sob o aspecto nutricional, e considerando que os moluscos bivalves se constituem em um recurso natural de boa aceitação pela população mundial, escolheu-se o molusco bivalve Anadara notabilis, por não ter sido encontrado na literatura nenhuma informação nutricional ou toxicológica sobre ele e devido seu tamanho ser bem maior que outras espécies de moluscos mais popularmente encontrados nessa região. Foram determinados neste trabalho teores de umidade, cinzas, proteínas, macro e microminerais, além de íons metálicos de importância toxicológica. Todas as determinações seguiram as Normas Analíticas do Instituto Adolfo Lutz. A determinação de proteína foi realizada pelo método de Kjeldahl. Todos os íons metálicos foram determinados por espectroscopia de emissão ótica com plasma indutivamente acoplado (ICP-OES) descrito pela metodologia USEPA 6010C. Os resultados mostraram que a Anadara notabilis pode ser introduzida na alimentação dos seres humanos, tendo em vista sua riqueza mineral. Merecem destaque entre os macronutrientes o magnésio e o fósforo que apresentaram os respectivos valores em mg/kg 918,7 e 586,7. Com relação aos micronutrientes destacam-se o ferro presente com 586,7 mg/kg e o Zinco com 12,31 mg/kg. Não foi encontrado índice elevado de metais contaminantes para este molusco, o que impediria seu consumo, apenas o cromo esta 0,7 mg/kg acima do valor estabelecido pela legislação brasileira. Os resultados obtidos certamente serão muito úteis em futuras pesquisas nutricionais e para construção de uma tabela brasileira de composição química de alimentos

Determinação da composição química do molusco Anadara notabilis encontrado em Galinhos no Rio Grande do Norte

Given the large existing biodiversity in the Brazilian coast, where many species are still little known, even under the nutritional aspect, and considering that bivalve molluscs are constituted by a natural resource of well accepted by the population, chose the bivalve Anadara notabilis, it was not found in the literature any nutritional or toxicological information about it and because its size is much larger than other species of mollusks commonly found in this region. Were studied moisture, ash, protein, macro and micro minerals, and metal ions of toxicological significance. All analytical determinations followed the standards of the Institute Adolfo Lutz. The protein determination was performed by the Kjeldahl method. All metal ions were determined by optical emission spectroscopy with inductively coupled plasma (ICP-OES) method described by USEPA 6010C. The results showed that Anadara notabilis can be introduced into food for human beings, in view of its mineral wealth. Noteworthy among the macronutrients phosphorus and magnesium showed that their values in mg / kg 918.7 and 586.7. With regard to micronutrients stand out with this iron 586.7 mg / kg and zinc with 12.31 mg / kg. Was not found high content of metal contaminants to this mollusc, which would prevent their use, only this chromium 0.7 mg / kg above the value established by Brazilian legislation. The results will certainly be very useful in future studies of nutrition and to build a table of chemical composition of Brazilian foods

Monitoramento das águas da bacia hidrográfica pirangi pela determinação dos índices de qualidade da água-iqa e índice de toxidez-it

The problems of water supply in Northeast Brazil are severe and require more focused studies. This work was intended to assess water quality in the watershed Pirangi, located in the Northeastern state of the newborn using the Water Quality Index, AQI associated with the Index of Toxicity-IT. The data presented in this study were collected in November 2008, June 2009 and March 2010 at eight sampling stations distributed throughout the basin. The study covered nine parameters, based on guidelines established by CETESB, and seven members of Metal Toxicity index-IT. These waters are framed in the classification between GOOD and BAD showing AQI 41.34 minimum and a maximum of 76.23. Virtually all seven metals analyzed were below the detection limits of ICP-OES giving IT a water equal to one when they are absent and 0 when there are levels of trace metals

Determinação de Ba, Cd, Cr, Cu, Ni, Pb, Sn e Zn em Tainha (Mugil brasiliensis) nos estuários potiguares

Heavy metals can cause problems of human poisoning by ingestion of contaminated food, and the environment, a negative impact on the aquatic fauna and flora. And for the presence of these metals have been used for aquatic animals biomonitoramento environment. This research was done in order to assess the environmental impact of industrial and domestic sewage dumped in estuaries potiguares, from measures of heavy metals in mullet. The methods used for these determinations are those in the literature for analysis of food and water. Collections were 20 samples of mullet in several municipality of the state of Rio Grande do Norte, from the estuaries potiguares. Were analyzed the content of humidity, ash and heavy metals. The data were subjected to two methods of exploratory analysis: analysis of the main components (PCA), which provided a multivariate interpretation, showing that the samples are grouped according to similarities in the levels of metals and analysis of hierarchical groupings (HCA), producing similar results. These tests have proved useful for the treatment of the data producing information that would hardly viewed directly in the matrix of data. The analysis of the results shows the high levels of metallic species in samples Mugil brasiliensis collected in Estuaries /Potengi, Piranhas/Açu, Guaraíra / Papeba / Arês and Curimataú

Determinação de CD, PB, e TL em água produzida por HR-CS GF AAS após extração em ponto nuvem

Produced water is a major problem associated with the crude oil extraction activity. The monitoring of the levels of metals in the waste is constant and requires the use of sensitive analytical techniques. However, the determination of trace elements can often require a pre-concentration step. The objective of this study was to develop a simple and rapid analytical method for the extraction and pre-concentration based on extraction phenomenon cloud point for the determination of Cd, Pb and Tl in produced water samples by spectrometry of high resolution Absorption source continues and atomization graphite furnace. The Box Behnken design was used to obtain the optimal condition of extraction of analytes. The factors were evaluated: concentration of complexing agent (o,o-dietilditilfosfato ammonium, DDTP), the concentration of hydrochloric acid and concentration of surfactant (Triton X -114). The optimal condition obtained through extraction was: 0,6% m v-1 DDTP, HCl 0,3 mol L-1 and 0,2% m v-1 of Triton X - 114 for Pb; 0,7% m v-1 DDTP, HCl 0,8 mol L-1 and 0,2% m v-1 Triton X-114 for Cd. For Tl was evidenced that best extraction condition occurs with no DDTP, the extraction conditions were HCl 1,0 mol L-1 e 1,0% m v-1 de Triton X - 114. The limits of detection for the proposed method were 0,005 µg L-1 , 0,03 µg L-1 and 0,09 µg L-1 to Cd, Pb and Tl, Respectively. Enrichment factors Were greater than 10 times. The method was applied to the water produced in the Potiguar basin, and addition and recovery tests were performed, and values were between 81% and 120%. The precision was expressed with relative standard deviation (RSD) is less than 5%

Aplicação da tecnologia eletroquímica para a remoção e monitoramento de metais pesados em efluentes aquosos

Heavy metals are present in industrial waste. These metals can generate a large environmental impact contaminating water, soil and plants. The chemical action of heavy metals has attracted environmental interest. In this context, this study aimed to test t he performance of electrochemical technologies for removing and quantifying heavy metals. First ly , the electroanalytical technique of stripping voltammetry with glassy carbon electrode (GC) was standardized in order to use this method for the quantificatio n of metals during their removal by electrocoagulation process (EC). A nalytical curves were evaluated to obtain reliability of the determin ation and quantification of Cd 2+ and Pb 2+ separately or in a mixture. Meanwhile , EC process was developed using an el ectrochemical cell in a continuous flow (EFC) for removing Pb 2+ and Cd 2+ . The se experiments were performed using Al parallel plates with 10 cm of diameter (  63.5 cm 2 ) . The optimization of conditions for removing Pb 2+ and Cd 2+ , dissolved in 2 L of solution at 151 L h - 1 , were studied by applying different values of current for 30 min. Cd 2+ and Pb 2+ concentrations were monitored during electrolysis using stripping voltammetry. The results showed that the removal of Pb 2 + was effective when the EC pro cess is used, obtaining removals of 98% in 30 min. This behavior is dependent on the applied current, which implies an increase in power consumption. From the results also verified that the stripping voltammetry technique is quite reliable deter mining Pb 2+ concentration , when compared with the measurements obtained by atomic absorption method (AA). In view of this, t he second objective of this study was to evaluate the removal of Cd 2+ and Pb 2+ (mixture solution) by EC . Removal efficiency increasing current was confirmed when 93% and 100% of Cd 2+ and Pb 2+ was removed after 30 min . The increase in the current promotes the oxidation of sacrificial electrodes, and consequently increased amount of coagulant, which influences the removal of heavy metals in solution. Adsortive voltammetry is a fast, reliable, economical and simple way to determine Cd 2+ and Pb 2+ during their removal. I t is more economical than those normally used, which require the use of toxic and expensive reagents. Our results demonstrated the potential use of electroanalytical techniques to monitor the course of environmental interventions. Thus, the application of the two techniques associated can be a reliable way to monitor environmental impacts due to the pollution of aquatic ecosystems by heavy metals.

Aplicação e otimização de métodos eletroquímicos combinados para remoção e determinação de cromo hexavalente em efluentes simulados

Hexavalent chromium is a heavy metal present in various industrial effluents, and depending on its concentration may cause irreparable damage to the environment and to humans. Facing this surrounding context, this study aimed on the application of electrochemical methods to determine and remove the hexavalent chromium (Cr6+) in simulated wastewater. To determine was applied to cathodic stripping voltammetry (CSV) using ultra trace graphite electrodes ultra trace (work), Ag/AgCl (reference) and platinum (counter electrode), the samples were complexed with 1,5- diphenylcarbazide and then subjected to analysis. The removal of Cr6+ was applied electrocoagulation process (EC) using Fe and Al electrodes. The variables that constituted the factorial design 24, applied to optimizing the EC process, were: current density (5 and 10 mA.cm-2), temperature (25 and 60 ºC), concentration (50 and 100 ppm) and agitation rate (400 and 600 RPM). Through the preliminary test it was possible the adequacy of applying the CSV for determining of Cr6+, removed during the EC process. The Fe and Al electrodes as anodes sacrifice showed satisfactory results in the EC process, however Fe favored complete removal in 30 min, whereas with Al occurred at 240 min. In the application of factorial design 24 and analysis of Response Surface Methodology was possible to optimize the EC process for removal of Cr6+ in H2SO4 solution (0.5 mol.L-1), in which the temperature, with positive effect, was the variable that presented higher statistical significance compared with other variables and interactions, while in optimizing the EC process for removal of Cr6+ in NaCl solution (0.1 mol.L-1) the current density, with positive effect, and concentration, with a negative effect were the variables that had greater statistical significance with greater statistical significance compared with other variables and interactions. The utilization of electrolytes supports NaCl and Na2SO4 showed no significant differences, however NaCl resulted in rapid improvement in Cr6+ removal kinetics and increasing the NaCl concentration provided an increase in conductivity of the solution, resulting in lower energy consumption. The wear of the electrodes evaluated in all the process of EC showed that the Al in H2SO4 solution (0.5 mol.L-1), undergoes during the process of anodization CE, then the experimental mass loss is less than the theoretical mass loss, however, the Fe in the same medium showed a loss of mass greater experimental estimated theoretically. This fact is due to a spontaneous reaction of Fe with H2SO4, and when the reaction medium was the NaCl and Na2SO4 loss experimental mass approached the theoretical mass loss. Furthermore, it was observed the energy consumption of all processes involved in this study had a low operating cost, thus enabling the application of the EC process for treating industrial effluents. The results were satisfactory, it was achieved complete removal of Cr6+ in all processes used in this study.

Uma proposta de slam com determinação de informações geométricas do ambiente

PEDROSA, Diogo P. F. ; MEDEIROS, Adelardo A. D. ; ALSINA, Pablo J. . Uma Proposta de SLAM com Determinação de Informações Geométricas do Ambiente. In: CONGRESSO BRASILEIRO DE AUTOMÁTICA, 16, Salvador, BA, 2006. Anais... Salvador: CBA, 2006. v. 1. p. 1704-1709