Determinação de metais em óleos lubrificantes utilizando a técnica de espectrometria de emissão óptica com plasma induzido por laser

IPEN/D

Uso do bivalve límnico Anodontites tenebricosus (LEA, 1834) no biomonitoramento de metais do Rio Ribeira de Iguape

This study investigated the contamination of the Ribeira de Iguape River - RIR by Cd, Zn, Cr and Pb, using the bivalve Anodontites tenebricosus as a biomonitor. Metal concentrations in tissue samples were measured by HR-ICPMS. Bivalve tissues exhibited mean levels of 1.00 µg/g Cd; 152.89 µg/g Zn; 14.79 µg/g Cr and 4.40 µg/g Pb. Lead concentrations were comparable to those reported for moderately contaminated sites. The results showed that Pb is bioavailable to the bivalves, exhibiting high concentrations and exceeding both natural and reference values for human consumption. The freshwater bivalve Anodontites tenebricosus is a suitable biomonitor of contamination by metals.

Adição do resíduo de biomassa da cana-de-açúcar em pastas para cimentação de poços petrolíferos produtores de óleos pesados

The Potiguar basin has large fields of viscous oil where the used method for recovering is based on vapor injection; this operation is carried out by injecting vapor in the oilwell directly, without the protection of a revetment through thermal insulation, what causes its dilation and, consequently, cracks in the cement placed on the annular, and lost of hydraulic insulation; this crack is occasioned by the phenomenon of retrogression of the compressive resistance due to the conversion of the hydrated calcium silicate in phases calcium-rich, caused by the high temperatures in the wells, subjected to thermal recuperation. This work has evaluated the application of composite pastes with addition of residue of biomass of ground sugar-cane bagasse as anti-retrogression mineral admixture for cementation of oil-wells subjected to thermal recuperation. The addition of the mineral residue was carried out considering a relative amount of 10, 20, 30, 40 and 59% in relation to cement mass, trying to improve the microstructure of the paste, still being developed a reference paste only with cement and a paste with addition of 40% of silica flour - renowned material in the oil industry as anti-retrogression additive. Pozzolanic activity of the ash was evaluated through XRD, TG/DTG, as the resistance to compression, and it was also determined the physical and mechanical behavior of the pastes when submitted to cure at low temperatures (22 and 38º C); besides it was evaluated the behavior of the pastes when submitted to two cycles of cure at high temperature (280ºC) and pressure (7 MPa). It was verified that the ash of the sugar-cane biomass presents pozzolanic reaction and has great efficiency in decrease the permeability of the paste by filler effect, as well as that addition of ash in a relative amount of 10, 20 e 30% increases cured compressive resistance at low temperatures. It was also showed that the ash in a relative amount of 40% and 59% has very significant efficiency as anti-retrogression additive, since it prevents the decrease of compressive resistance and forms hydrated calcium silicate type xenotlita and tobermorita which have more resistance and stability in high temperatures

Remoción de metales pesados con carbón activado como soporte de biomasa

El incremento en los niveles de contaminación del agua por metales pesados ha resultado en un aumento en la investigación y el desarrollo de métodos más efectivos para su eliminación

Determinación de metales pesados y evaluación de la biotransferencia de especies inorgánicas de arsénico en leche bovina cruda

Propósito y método de estudio: En el presente estudio se evaluó el factor de biotransferencia (FBT) de arsénico (As) inorgánico en leche bovina cruda a través de agua de consumo en zonas contaminadas con este metaloide en México. Las muestras de leche y agua fueron colectadas en municipios de Durango, San Luis Potosí y Zacatecas zonas lugares donde se lleva a cabo la minería y con antecedente de contaminación por As. Para el análisis de As total fue empleado el método de digestión acida asistido por microondas (EPA 3052). La extracción de especies inorgánicas de As fue asistida por microondas empleando H3PO4 0.3 M a 90 °C durante 30 min, para su posterior separación en una resina de intercambio aniónico fuerte (SAX). La determinación de As total y de especies de arsénico se llevó a cabo por Espectrometría de Masas con Fuente de Plasma de Acoplamiento Inductivo (ICP-MS). Adicionalmente en las muestras leche previamente digeridas se analizó el contenido total de Pb, Cd, Cu, Zn y Fe por ICP-MS con la finalidad de evaluar el grado de contaminación por estos metales y establecer una correlación con la concentración de As en leche y el posible origen de la contaminación. Contribuciones y conclusiones La concentración de As total en el agua de la mayoría de las zonas de estudio superó el límite permisible para agua de consumo según la norma oficial NOM-127-SSA1-1994-2000 (25 μg/L). En cuanto a las muestras de leche, las concentraciones de As se encontraron entre el límite de detección y 472.80 μg/kg, siendo los estados de Durango y San Luis Potosí los que presentaron las concentraciones mayores. Las concentraciones de los otros metales analizados en leche mostraron que el promedio de Pb en leche en Zacatecas y San Luis Potosí, superó el límite permisible de acuerdo a la Comisión Europea. Así mismo para el caso del Cd la concentración media en el estado de San Luis Potosí superó los niveles ya reportados. Las zonas de San Luis Potosí, Durango y Zacatecas presentaron niveles altos de metales esenciales (Zn, Cu y Fe). Además se encontró que para los metales analizados (Pb, Cd, Cu, Zn y Fe) se presentó una correlación positiva estadísticamente significativa (p < 0.05) con As en leche, lo cual sugiere una fuente de contaminación común la minera que se realiza en los sitios de estudio. En cuanto a la concentración de especies de As inorgánico en leche, las concentraciones para la especie de As (V) fueron mayores (79.60-242.20 μg/kg) que las de As (III) (31.00-96.81 μg/kg); dado que la especie de As (V) presenta un menor grado de toxicidad podría indicar menor riesgo para la población que ingiere este alimento. Por último, se determinó el FBT de especies de As inorgánicas a través del agua de consumo, obteniéndose valores superiores a los ya reportados para As total (2.6 x 10-6 a 6 x 10-4); sin embargo, no se encontró una correlación significativa entre As en leche y arsénico en agua (p ˃0.05), lo cual sugiere que el agua no es la única vía de exposición de este metaloide. Para una posterior evaluación del factor de biotransferencia se sugiere el analizar el contenido de As en alimento y el suelo donde habita el organismo e incorporar estas fuentes de contaminación al modelo del FBT.

Impregnação de metais em xisto retortado para uso como adsorventes

Concern with the environment has lead to an increase in the research for new adsorption techniques, low cost adsorvent materials and with high availability. Many works search the development of higher selectivity modified adsorvents. The Brazil has the second world reserve of oiled shale, because of it, the use of that reject is of great interest. This study has the goal of characterize and analyze the retorted shale, reject of the pirobetuminous shale pyrolysis, and the retorted shale modified through the humid impregnation method, wich the precursors were the metals nitrates ( Cobalt, Nickel and Copper), to the usage has adsorvent materials. The samples were characterized chemically, textually and structurally by the X ray fluorescence (XRF), BET, X ray diffraction (XRD) and scanning electronic microscopy (SEM) techniques. The impregnated samples showed a reduction in the superficial area and in the pore volume when compared with the retorted shale. Besides that, diffractions referred to the impregnated metals where observed in the XRD analysis, wich were the same metals detected in the XRF and SEM analysis. The materials showed homogeneity in it s composition. The results shows that the materials presents adequate adsorption characteristics

Estudo paramétrico do processo de injeção de solventes em poços horizontais para reservatórios de óleos pesados

The world has many types of oil that have a range of values of density and viscosity, these are characteristics to identify whether an oil is light, heavy or even ultraheavy. The occurrence of heavy oil has increased significantly and pointing to a need for greater investment in the exploitation of deposits and therefore new methods to recover that oil. There are economic forecasts that by 2025, the heavy oil will be the main source of fossil energy in the world. One such method is the use of solvent vaporized VAPEX which is known as a recovery method which consists of two horizontal wells parallel to each other, with a gun and another producer, which uses as an injection solvent that is vaporized in order to reduce the viscosity of oil or bitumen, facilitating the flow to the producing well. This method was proposed by Dr. Roger Butler, in 1991. The importance of this study is to analyze how the influence some operational reservoir and parameters are important in the process VAPEX, such as accumulation of oil produced in the recovery factor in flow injection and production rate. Parameters such as flow injection, spacing between wells, type of solvent to be injected, vertical permeability and oil viscosity were addressed in this study. The results showed that the oil viscosity is the parameter that showed statistically significant influence, then the choice of Heptane solvent to be injected showed a greater recovery of oil compared to other solvents chosen, considering the spacing between the wells was shown that for a greater distance between the wells to produce more oil

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

Extração de metais (K, Mg, Ba, Ca, Cr, Mn, Li, Fe) de água produzida utilizando sistema microemulsionado

The produced water is a byproduct formed due to production of petroleum and carries with it a high amount of contaminants such as oil particles in suspension, organic compounds and metals. Thus, these latter pollutants are very difficult to treat because of its high solubility in water. The objective of this work is to use and evaluate a microemulsioned system to remove metals ( K , Mg , Ba , Ca , Cr , Mn , Li , Fe ) of synthetic produced water. For the extraction of metals, it was used a pseudoternary diagram containing the following phases: synthetic produced water as the aqueous phase (AP), hexane as organic phase (OP), and a cosurfactant/surfactant ratio equal to four (C/S = 4) as the third phase, where the OCS (saponified coconut oil) was used as surfactant and n-butanol as cosurfactant. The synthetic produced water was prepared in a bench scale and the region of interest in the diagram for the removal of metals was determined by experimental design called. Ten points located in the phase Winsor II were selected in an area with a large amount of water and small amounts of reagents. The samples were analyzed in atomic absorption spectrometer, and the results were evaluated through a statistical assesment, allowing the efficiency analysis of the effects and their interactions. The results showed percentages of extraction above 90% for the metals manganese, iron, chromium, calcium, barium and magnesium, and around 45% for metals lithium and potassium. The optimal point for the simultaneous removal of metals was calculated using statistical artifact multiple response function (MR). This calculation showed that the point of greatest extraction of metals occurs was the J point, with the composition [72% AP, 9% OP, 19% C/S], obtaining a global extraction percentage about 80%. Considering the aspects analyzed, the microemulsioned system has shown itself to be an effective alternative in the extraction of metals on synthetic produced water remediation

Determinación de metales pesados (plomo y arsénico) y oligoelementos (hierro, cobre y zinc) en hojas de Crotalaria longirostrata (chipilin) por el método de absorción atómica

La presente investigación tuvo como finalidad analizar esta especie vegetal cultivada en la zona Central y Occidental del territorio salvadoreño; para ello, se llevó a cabo una investigación de campo visitando los Municipios de Colón y Ciudad Arce ubicados en el Departamento de la Libertad; y los Municipios de Izalco y Nahuizalco, ambos pertenecientes al Departamento de Sonsonate; donde se recolectaron las muestras (hojas de C. longirostrata); Se elaboraron encuestas dirigidas a Técnicos ó Ingenieros agrónomos que laboraran en Agroservicios de mayor afluencia en el país y a los productores de los cultivos seleccionados; con la finalidad de conocer los productos agroquímicos aplicados al tratamiento del cultivo de esta hortaliza. Se realizó un análisis químico e instrumental para determinar elementos metálicos como metales pesados (plomo y arsénico) y oligoelementos (hierro, cobre y zinc) utilizando las técnicas de Espectrofotometría de Absorción Atómica (EAA): - Horno de grafíto para plomo. - Generador de Hidruros para arsénico. - Llama para hierro, cobre y zinc. Los resultados se compararon con los límites máximos establecidos por la normativa de JECFA - Comité Mixto FAO/OMS de Expertos en Aditivos Alimentarios y Codex Alimentarius; y se evaluaron estadísticamente a través del análisis de varianza de un factor (ANOVA), las pruebas de comparación DMS y Bonferroni; para evaluar el comportamiento de los datos experimentales obtenidos en el análisis. Según los resultados obtenidos se encontraron trazas de plomo y arsénico en algunas muestras analizadas; así como un alto contenido de hierro, cobre y zinc en todas las muestras de C. longirostrata. Se recomienda que se analicen muestras de suelos, agua de riego y otros cultivos de C. longirostrata ubicados en diversas zonas geográficas de El Salvador; con la finalidad de evaluar la calidad de las distintas hortalizas de esta especie vegetal existentes en el país.

Coeficientes de difusão de metais em materiais não convencionais (agarose e acetato de celulose) usados na técnica de difusão em filmes finos por gradientes de concentração

The DGT technique allows one to measure quantitatively free and labile metal species in aquatic systems. Nevertheless, for this approach, knowledge is required of the diffusion coefficients of the analytes in a diffusive layer. In this study, the diffusion coefficients of Hg(II), As(III), Mn(II), Mg(II), Cu(II), Cd(II) were determined in agarose gel and those of Ba(II), Cd(II), Cu(II), Mg(II), Mn(II) e Zn(II) in cellulose acetate membranes. These materials presented good performance and the reported results can be used as a data base for further DGT studies.

Novos complexos micelares de metais de transição para aplicação na terapia dirigida contra o cancro

O cancro é a segunda causa de mortalidade a nível mundial. Um dos problemas nos tratamentos atuais de quimioterapia relaciona-se com os efeitos secundários causados pela falta de seletividade dos fármacos utilizados. Assim, um dos desafios atuais é o desenvolvimento de sistemas terapêuticos que permitam potenciar o efeito dos fármacos e diminuir os seus efeitos nocivos. Neste contexto, neste trabalho, foram sintetizados complexos de Fe, Co e Zn com fórmula geral [M(bipy-R)3]x+, a partir dos quais foi possível obter sistemas micelares formados in situ pela adição de um copolímero de PLA-b-PEG ou por introdução de macroligandos poliméricos anfifílicos. Os resultados mostram que as nanopartículas formadas apresentam tamanho e características adequadas para aplicações na terapia dirigida contra o cancro. Os resultados preliminares de citotoxicidade na linha tumoral humana da mama MDAMB231 indicam que todos os compostos estudados apresentam atividade citotóxica relevante, sendo os compostos micelares os mais promissores; Abstract: New micellar transition metals complexes for targeted therapy of cancer Cancer is the second leading cause of mortality worldwide. One problem in the current chemotherapy treatments is related to the severe side effects caused by the lack of selectivity of the drugs in clinical use. Thus, one of the current challenges is the development of new therapeutic systems that allow maximizing the effect of the drugs and reducing their harmful effects. In this context, several Fe, Co and Zn compounds of the general formula [M (bipy-R)3]x+ were synthesized in order to obtain micellar systems, either by in situ addition of a PLA-b-PEG copolymer or by introducing amphiphilic macroligands. The results show that the formed nanoparticles have size and characteristics suitable for applications in targeted therapy against cancer. Preliminary results of cytotoxicity in human breast cancer line MDAMB231 indicate that all the studied compounds show significant cytotoxic activity, being the micellar compounds the most promising agents.

Mobilidade de metais potencialmente tóxicos numa área de tratamento de minério, em clima tropical

Neste trabalho avaliou-se a mobilidade de metais com vista à escolha da metodologia de remediação mais adequada à recuperação de uma área contaminada pela actividade de uma fábrica de zinco situada em Três Marias, Estado de minas Gerais.

Metais, ambiente e vida: Interferência dovanádio nos sistemas vivos e sua contextualização no ensino das ciências experimentais

A actividade aqui descrita teve como objectivo aproximar alunos do ensino secundário a uma abordagem fisiológica e molecular sobre os efeitos dos metais nos seres vivos. Os alunos ficaram familiarizados com abordagens teóricas e experimentais que permitiram avaliar o crescimento celular por observação qualitativa, determinação do conteúdo proteico e da actividade específica fosfatase alcalina (ALP), recorrendo a centrifugação diferencial, leituras de absorvência e tratamento informático dos resultados. Os estudantes concluíram que a presença de metavanadato de amónio inibiu o crescimento da levedura vínica Saccharomyces cerevisiae UE-ME3, causando um decréscimo significativo do conteúdo proteico e da actividade específica ALP, um marcador da proliferação celular. A avaliação de competências adquiridas, bem como, os inquéritos de opinião mostraram que a maior parte dos alunos do 10° e 12° ano da Escola Secundária Dom Manuel Martins de Setúbal, envolvidos nesta acção, atingiram com sucesso e satisfação os objectivos previamente traçados, revelando uma aprendizagem significativa. ABSTRACT: The work described here aimed to bring high school students to a physiological and molecular approach on the effects of metals in living organisms. The students were familiar with theoretical and experimental approaches that allowed them to evaluate cell growth by qualitative observation, protein contents and alkaline phosphatase (ALP) determination, using differential centrifugation, absorbance readings and computational analysis of data. The students concluded that the presence of ammonium metavanadate inhibited the wine-wild yeast Saccharomyces cerevisiae UE-ME3 growth, and cause a significant decrease of protein content and ALP specific activity, a cell proliferation marker. The assessment of acquired skills, as well as opinion surveys showed that the vast majority of students of 10th and 12nd years of High School Dom Manuel Martins of Setúbal, involved in this project have reached with success and satisfaction the goals previously set for this action and reveals a significant learning.

Sistema de monitoramento de perdas visíveis de cana-de-açúcar em colhedora de cana picada

In the last few years the sugar-cane mechanical harvested area has increased, especially in regions with appropriated slop. The use of this technology brings some inconveniences, such as, the increase in the percentage of extraneous matter, which causes the reduction of technological quality of the raw material, and losses in the field. Extraneous matter (trash) is composed of tops and leaves in major percentage, plus soil and roots, and eventually some metal parts. In the green cane harvest system the percentage of extraneous matter has a tendency to increase due to the great amount of vegetal matter to be processed. The increase in the blower fan speed to reduce the amount of extraneous matter can lead to an unacceptable economic level of raw material losses. The main objective of this work was, using a cane loss monitor, to evaluate and quantify the amount of visible losses of sugar cane through the primary extractor at two different fan speeds. Afterwards these losses were related to the harvester cleaning efficiency. The piezoelectric transducer shows a reasonable sensibility. The results show that the cleaning efficiency in the primary extractor (85% mean), the cane losses (between 5.68% and 2.15%) and fan speed are interrelated. The total losses and specially splinters (between 3.19% and 0.91%), showed a significant difference among the treatments.