Utilização de zeólita preparada a partir de cinza residuária de carvão como adsorvedor de metais em água

Coal ashes produced in coal-fired power plant could be converted into zeolites and can be used as low-cost adsorbents for the treatment of effluents contaminated with high levels of toxic metals. The capacity of synthetic zeolites for the removal of cadmium, zinc and copper ions from aqueous solutions has been investigated under different operating conditions. Zeolite from bottom chimney showed higher removal efficiency for metals ions than zeolite from feed hopper and mixing mill. The results indicated that the treated bottom ash could be applied in environmental technology as an immobilizer of pollutants.

Otimização dos parâmetros de extração para determinação multiresíduo de pesticidas em amostras de água empregando microextração em fase sólida

In this study the factors that affect the extraction of pesticide residues from water samples for their determination by solid-phase micro-extraction (SPME) and GC/MS were optimized. The fiber polymer, the extraction mode, the ionic strength, the stirring rate, the pH and the extraction time were the most significant parameters evaluated. The recovery obtained with the proposed method ranged from 94 to 110% and the sensitivity of the method, determined by calculating the detection limit (DL), ranged from 0.004 to 0.1 mug l-1. The results obtained with spiked real samples, at the 0.1 mug l-1 level, showed acceptable conformity with the expected values.

Análise de praguicidas organofosforados em água por extração em fase sólida (SPE) utilizando discos C18 e cromatografia em fase gasosa: avaliação da contaminação do reservatório de Furnas (MG-Brasil)

Solid phase extraction (SPE) in C18 disks has been optimized and validated for extraction of 5 organophosphorus (OP) pesticides in water. Extraction has been followed by separation and detection by gas chromatography/flame photometry. Excellent linearity was obtained for all compounds (r greater than 0.99), with CVs between 1.0-6.9%, recoveries between 73-95% and quantification limits between 2.5-5.0 µg L-1. Samples from Furnas dam were analyzed monthly during one year and 10% showed OP pesticide residues.

Materiais magnéticos baseados em diferentes zeólitas para remoção de metais em água

In this work the adsorption features of zeolites (NaY, Beta, Mordenite and ZSM-5) have been combined with the magnetic properties of iron oxides in a composite to produce a magnetic adsorbent. These magnetic composites can be used as adsorbents for contaminants in water and subsequently removed from the medium by a simple magnetic process. The magnetic zeolites were characterized by XRD, magnetization measurements, chemical analyses, N2 adsorption isotherms and Mössbauer spectroscopy. These magnetic adsorbents show remarkable adsorption capacity for metal ion contaminants in water.

Otimização e validação da técnica de extração líquido-líquido com partição em baixa temperatura (ELL-PBT) para piretróides em água e análise por CG

The liquid-liquid extraction with the low temperature partition technique was developed for the analysis of four pyrethroids in water by CG. Using a factorial design the extraction technique was optimised evaluating the effect of the variables ionic strength, contact time and proportion between sample and solvent volumes. The validation parameters sensitivity, precision, accuracy and detection and quantification limits were evaluated. The LOD and LOQ of the method varied from 1.1 to 3.2 µg L-1 and 2.7 to 9.5 µg L-1, respectively.

Extração seletiva de metais pesados em sedimentos de fundo do Rio Tietê, São Paulo

Sediment samples from Tietê river were submitted to chemical and sequential extractions of heavy metals (Cd, Cr, Cu, Ni, Pb and Zn). It was followed a single extraction by using 0.1 mol L-1 hydrochloric acid and a sequential procedure to evaluate possible chemical associations described as exchangeable, carbonate, reducible oxides, sulfide, organic matter and residual fractions. High concentrations of heavy metals were determined at Pirapora reservoir, which is closer to the Metropolitan Area of São Paulo while for Barra Bonita reservoir, the results showed low concentrations for such elements. Acid volatile sulfides, grain size distribution and carbon contents were also determined.

Otimização e validação de métodos analíticos para determinação de BTEX em água utilizando extração por headspace e microextração em fase sólida

Three analytical methods for the determination of BTEX in water were optimized and validated. With the best method the analytes were extracted of 10 mL of sample with 2.50 g of NaCl in headspace vial of 20 mL by HS and SPME to 40 ºC for 30 min for adsorption and to 250 ºC for 4 min for desorption and were analyzed by GC-MS. The recovery was between 97.9% and 104.3%, and the limit of detection was 2.4 ng L-1 for o-xylene. This method was using to analyze BTEX in water supply and surface water in Ouro Preto city. No sample had concentrations of BTEX above the legislation.

Sulfetos volatilizáveis por acidificação e metais extraídos simultaneamente na avaliação de sedimentos de água doce

This paper discusses the historical and methodological fundaments of the dynamics and quantification of acid volatile sulfides (AVS) and simultaneously extracted metals (SEM) in aquatic sediments. It also discusses the SEM/AVS relationship, which involves several controversial aspects such as sulfide stability, sulfide-organic matter interaction, and the inability to predict the toxicity of organic compounds in the environment. This relationship is an important tool for the inference of metal bioavailability. The use of ecotoxicological tests with target organisms regulated by international standards is also a relevant aspect.

Modelagem termodinâmica por extração por solvente de metais divalentes em meio sulfato usando D2EHPA

The extraction of divalent metals (Mn2+, Ni2+, Co2+ and Cu2+) in the system MSO4 - H2SO4 - H2O - D2EHPA in isoparaffin (17/21) was studied by a thermodynamic model based on chemical equilibria with mass and charge balance equations. The activity coefficients of all solutes in the aqueous phase were calculated by Davies equation. By applying this model, the equilibrium concentrations of solutes were calculated from de concentration of divalent metals and pH. The predicted distribution coefficients for the divalents metals were in good agreement with experimental results.

Análise de agrotóxicos em água usando extração líquido-líquido com partição em baixa temperatura por cromatografia líquida de alta eficiência

This study optimized and validated the liquid-liquid extraction technique with partition at low temperature (LLE-PLT) for identification and quantification of four pesticides (chlorpyrifos, λ-cyhalothrin, permethrin, bifenthrin) in water samples. Analyses were performed by HPLC-UV. The technique was efficient for pesticide recovery with extraction exceeding 86%. Chromatographic response was linear for the four compounds in the 10-45 µg L-1 range, with correlation coefficients greater than 0.99. Limits of detection and quantitation were less than 3.5 µg L-1 and equal to 10 µg L-1, respectively. The proposed method was applied to 29 water samples from the Jaíba Project in northern Minas Gerais.

Floculação de Chlorella sp. produzida em concentrado de dessalinização e estudo de método de extração de lipídeos intracelulares

Chlorella sp. was used to assess algal lipid production with concentrated desalination. In order to investigate the action of the flocculating agent calcium chloride and pH, a Box-Behnken Design and a Central Composite Design (CCD) were carried out. Also, Soxhlet and Supercritical Fluid Extraction (SFE), with and without sonication lipid extraction methods, were examined. The optimal flocculation conditions were pH 10.0 and 2.0 g/L of calcium chloride concentration. The highest lipid content of Chlorella sp. was obtained using the Soxhlet extraction method. The most abundant fatty acid extracted by Soxhlet and SFE, with and without sonication, was palmitic acid, whose proportions were 57.4%, 35.3% and 25.5%, respectively.

AVALIAÇÃO DA BIOACUMULAÇÃO DE METAIS EM Cyprinus carpio PELA INTERAÇÃO COM SEDIMENTO E ÁGUA DE RESERVATÓRIO

Bioaccumulation of Ag, Al, Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb and Zn was determined in the gills and liver of Cyprinus carpio and related to concentrations in the sediment and water of the Alagados Reservoir, Ponta Grossa/Paraná. Cd and Fe exceeded the legal limit for water. Fe was the most abundant metal in the reservoir's water and sediment. The metals in the sediment were below the level of probable adverse effects on biota. There were no significant differences between sampling sites for water and sediment. Liver and gills had higher concentrations of Al, Fe and Zn, with a significant increase in Al (P > 0.05) compared to the increase in weight and size of the specimens. Statistically, gills showed higher concentrations of Al, Cd, Co, Cr, Mn and Zn and liver higher concentrations of Cu and Fe. Co, Cu, Fe, Mn and Zn showed significant differences (P < 0.01) between the organs. The bioaccumulation factors (BAF) showed that the interaction of water with gills promotes greater accumulation of metals in this organ. Despite the low concentrations in the reservoir, bioaccumulation of metals in gills and liver of C. carpio occurs by its interaction with contaminated water and sediment, respectively.

USO DO PLANEJAMENTO EXPERIMENTAL PARA OTIMIZAÇÃO DE UM PROCEDIMENTO VOLTAMÉTRICO PARA DETERMINAÇÃO SIMULTÂNEA DAS CONCENTRAÇÕES DOS METAIS Zn, Cd, Pb E Cu LIVRES EM ÁGUA DE COCO

Optimization of the main parameters of SWASV using boron-doped diamond electrode was described for the simultaneous determination of Zn, Cd, Pb and Cu free in coconut water. The values of electroanalytical parameters studied were optimized with the factorial design and center composite design. The optimized parameters for the preconcentration of metals were -1.50 V for potential, and 240 s for deposition time. For SWV, the optimized value was 11.56 mV for step potential. In addition, frequency and pulse height were defined at 100 Hz and 55 mV, respectively. Furthermore, the concentration of the supporting electrolyte (acetate buffer, pH 4.7) was optimized in 0.206 mol L-1. The optimized procedure was applied in two samples of coconut water: natural and processed. The limits of detection (LOD) obtained for Zn, Cd, Pb and Cu were 7.2; 4.4; 3.3 and 1.5 µg L-1, respectively. The concentrations of Cd and Pb were not detected. On the other hand, the values found for the concentrations of Zn and Cu were: < LOD (29 µg L-1) and (6.8 ± 0.9) µg L-1 for the natural sample; and (85.8 ± 4.2) µg L-1 and (7.7 ± 0.6) µg L-1 for the processed sample, respectively.

Distribuição de Cr, Ni, Cu, Cd e Pb em frações húmicas de diferentes tamanhos moleculares extraídas de amostras de água e de sedimentos do reservatório de captação de água superficial Anhumas - Araraquara-SP

Estudou-se a distribuição de Cr, Ni, Cu, Cd e Pb em frações de substâncias húmicas (SH) de diferentes tamanhos moleculares. As SH foram extraídas de amostras de água (SHA) e de sedimentos de superfície (SHSS), interface/água (SHSI) e fundo (SHSF) coletados no reservatório de captação de água superficial Anhumas, localizado no município de Araraquara-SP. Para a extração das SH utilizaram-se os procedimentos recomendados pela Sociedade Internacional de Substâncias Húmicas. Após purificação por diálise, as SH foram fracionadas com base no tamanho molecular utilizando-se sistema de fracionamento seqüencial por ultrafiltração e fluxo tangencial. O fracionamento das amostras de SHA permitiu caracterizar uma distribuição de massa relativamente uniforme dentre as frações de diferentes tamanhos moleculares, com valores maiores nas frações F2 (20,8%) e F4 (23,8%). Exceto para os íons Pb(II) e Cu(II) os quais apresentaram concentrações relativamente mais altas nas frações F2 e F4, respectivamente, de maneira geral, crômio, níquel, cádmio e chumbo têm distribuições similares nas cinco frações com tamanhos moleculares maiores e médios (F1 a F5). Quanto às distribuições de massa nas diferentes frações de substâncias húmicas extraídas de amostras de sedimento de superfície (SHSS), sedimento interface/água (SHSI) e sedimento de fundo (SHSF), as três amostras apresentaram 42-48% das SH nas frações com maiores tamanhos moleculares (F1 e F2), 29-31% nas frações intermediárias (F3 e F4) e 13-20% nas frações com menores tamanhos moleculares (F5 e F6). De modo geral, caracterizaram-se para os íons metálicos, distribuições similares dentre as respectivas frações F1 a F6. Exceções para Pb(II) e Ni(II) em sedimento de superfície com concentrações relativamente menores nas frações F2 e F4, respectivamente.

Comparação de técnicas analíticas para a extração de potássio de amostras de tecido vegetal com água e soluções ácidas concentrada e diluída

O aprimoramento dos métodos analíticos faz com que a busca por novas tecnologias rápidas, exatas e de custo reduzido estejam constantemente sendo revistas e avaliadas. O objetivo deste trabalho foi comparar três formas de extração de K (decomposição nítro-perclórica, extração com água e extração com solução diluída de HCl) de amostras da parte aérea de capim-tanzânia (Panicum maximum cv. Tanzânia) e de alfafa (Medicago sativa cv. Crioula). Os métodos de extração de K de amostras de tecido vegetal de capim-tanzânia e alfafa com solução ácida diluída ou com água apresentaram-se equivalentes ao método tradicional da decomposição nítro-perclórica e podem substituí-lo.