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Item DLLME-GC/ECD Method for the Residual Analysis of Parathion-Methyl and its Application in the Study of the UV-Photodegradation Process(Journal of the Brazilian Chemical Society, 2017-11) Pimenta, Gustavo G.; Queiroz, Maria E. L. R. de; Victor, Raquel P. D.; Noronha, Luiz M.; Neves, Antônio A.; Oliveira, André F. de; Heleno, Fernanda F.A new method has been developed to determine trace levels of organophosphorus pesticide parathion-methyl in water samples by using dispersive liquid-liquid microextraction (DLLME), followed by gas chromatograph coupled with electron capture detector (GC/ECD) analysis. The optimized and validated method showed high extraction recovery (101.1%), high enrichment factor (57.3), low limits of detection and quantification, 0.083 and 0.250 µg L-1, respectively. The established DLLME-GC/ECD method has been successfully applied for the evaluation of the photodegradation of the parathion-methyl by UV254nm radiation in different conditions of pH and temperature. The parathion-methyl photodegradation at pH 3 and 35 °C achieved > 99.5% after 120 min of exposition. For this condition, it was observed the kinetic rate of 0.0515 min-1, the quantum yield of 1.22 × 10-5 mol Einstein-1 and a half-life time of 13.46 min. All experimental conditions tested proved to be strongly influenced by pH and temperature. The application of the optimized process in distilled and drinking water spiked with parathion-methyl provided residues of this pesticide at levels below the maximum permitted by Brazilian legislation, which is 9.0 µg L-1.Item Multivariate calibration to determine phorbol esters in seeds of Jatropha curcas l. Using near infrared and ultraviolet spectroscopies(Journal of the Brazilian Chemical Society, 2017-08) Roque, Jussara V.; Dias, Luiz A. S.; Teófilo, Reinaldo F.The building of partial least squares (PLS) regression models using near infrared (NIR) and ultraviolet (UV) spectroscopies to estimate the concentrations of phorbol esters (PEs) in Jatropha curcas L. is presented. The models were built using two algorithms for variable selection, ordered predictors selection (OPS) and genetic algorithm (GA). Chromatographic analyses were performed to determine the concentrations of PEs. Spectral data were obtained from seeds and oil extract. The results of PLS models were performed by analyzing statistical parameters of quality such as root mean square error of prediction (RMSEP) and correlation coefficient of external predictions (Rp). The parameters obtained for NIR-PLS and UV-PLS models with OPS were respectively: RMSEP 0.48 and 0.22 mg g-1 and Rp 0.49 and 0.96. For GA were obtained, respectively: RMSEP 0.52 and 0.28 mg g-1 and Rp 0.12 and 0.95. The models built from seeds and oil extracts can be used respectively for screening and to accurately predict the PEs content. The OPS method provided simpler and more predictive models compared to those obtained by the selection of variables using the GA. Thus, the UV-PLS-OPS model can be used as an alternative method to quantification of PEs.Item Removal of beta-lactams antibiotics through zero-valent copper nanoparticles(Journal of the Brazilian Chemical Society, 2018) Oliveira, Lucas M. F.; Nascimento, Mayra A.; Guimarães, Yuri M.; Oliveira, André F.; Silva, Antônio A.; Lopes, Renata P.The removal of the beta-lactam antibiotics (ceftriaxone and cefadroxil) through zero-valent copper nanoparticle (nZVC) was studied in this work. Excellent removal degrees (> 85%) were obtained for both analytes in only 20 min of reaction. Studies were performed in both oxic and anoxic conditions, and in the presence of t-butyl alcohol (TBA), an inhibitor of radicals. The results did not show significant changes. Therefore, the hydroxyl radicals are not the main species responsible for the removal. Total organic carbon cefadroxil analysis indicated a removal of 57% after 180 min of reaction. Studies involving Cu+ indicated that probably these are the principal species responsible for the removal of antibiotics. Kinetic studies have shown that two-phase reaction occurred in the antibiotics removal process and both phases followed pseudo-first order kinetic model. The first mechanism is related to the antibiotics degradation by Cu+ species and the second mechanism is related to the antibiotics adsorption by hydroxides/oxides of Cu2+ species.Item Preparation, X-ray structural studies and plant growth regulatory activity of methyl 6a,7b-thiocarbonyldioxyvouacapan-17 b-oate(Journal of the Brazilian Chemical Society, 2004-03) Rubinger, Mayura M. M.; Borges, Eduardo E. L.; Castelo-Branco, Pedro de A.; Guilardi, Silvana; Souza, Elysângela M. R.; Gambardella, Maria T. do P.; Ferreira-Alves, Dalton L.; Piló-Veloso, DorilaThe 6a,7b-dihydroxyvouacapan-17b-oic acid (1) and methyl 6a,7b-dihydroxyvouacapan-17b-oate (2) are natural products isolated from the hexane extract of Pterodon polygalaeflorus Benth fruits. Here we describe the preparation and characterization by infrared and nuclear magnetic resonance spectroscopy, and by elemental analysis of the novel derivative methyl 6a,7b-thiocarbonyldioxyvouacapan-17b-oate (5), from the ester 2. The structure of compound 5 was determined by X-ray diffraction. At the concentration of 100 ppm, this compound inhibited the radicle growth of Sorgum bicolor L. (-28%) and showed no significant effect on Cucumis sativus L..Item Características físico-químicas de ácidos húmicos em diferentes etapas da vermicompostagem(Eclética Química, 2010) Reis, E. L.; Reis, C.; Brighenti, C. R. G.Amostras de materiais coletados em diferentes estádios de vermicompostagem foram submetidas a procedimentos de extração de ácidos húmicos. Técnicas de titulação potenciométrica, termogravimetria (DTG), difração de raios X e espectrofotometria no uv/visível e no infravermelho foram utilizadas no estudo desses materiais. Os dados de titulação foram submetidos ao ajuste por regressão não-linear, determinando-se, assim, cinco valores de pKa característicos de cinco classes de grupos tituláveis. Nas curvas DTG, foram observadas duas etapas, sendo a primeira característica da separação de estruturas alifáticas e, ou, alicíclicas e a segunda, a decomposição de estruturas aromáticas. A difratometria de raios X apresentou diferenças marcantes nos resultados, principalmente nos três primeiros picos onde parecem ocorrer reorganização estrutural e polimerização ao longo do processo de vermicompostagem. Os espectros do infravermelho não apresentaram diferenciação entre os espectros. Os valores da razão E4/E6 encontrados estão de acordo com os característicos dos ácidos húmicos, mas não fornecem informações que possam contribuir para a elucidação da estrutura e formação desses ácidos.Item Evaluation of aerobic and anaerobic biodegradability and toxicity assessment of real pharmaceutical wastewater from industrial production of antibiotics(Brazilian Journal of Chemical Engineering, 2016-07) Marcelino, R. B. P.; Andrade, L. N.; Starling, M. C. V. M.; Amorim, C. C.; Barbosa, M. L. T.; Lopes, R. P.; Reis, B. G.; Leão, M. M. D.This study evaluates aerobic and anaerobic biodegradability and toxicity of a real pharmaceutical wastewater, which focuses on antibiotics production. Zahn-Wellens and Organization for Economic Cooperation and Development (OECD) methodologies were applied in order to verify the wastewater's biodegradability and Microtox® analysis was performed for toxicity tests. Tests achieved more than 89% and 63% of Total Organic Carbon reduction, showing 80% and 50% of antibiotic removal, for aerobic and anaerobic processes, respectively. Moreover, acute ecotoxicological tests revealed that both techniques decreased the toxic character of real pharmaceutical wastewater. Desorption tests showed that the antibiotic was not degraded, but, in fact, adsorbed onto the sludge. Since biological treatment is the most widely used method for industrial wastewater treatment, this study indicates that this kind of treatment is probably unable to mineralize antibiotics present in pharmaceutical wastewaters, which may induce the development of resistant pathogens. Therefore, efforts must be taken to elucidate the main mechanisms of biological antibiotic removal from wastewaters since the presence of antibiotics in the environment is considered to be an emerging environmental issue.Item Synthesis and phytotoxicity of 4,5 functionalized tetrahydrofuran-2-ones(Journal of the Brazilian Chemical Society, 2012-12) Resende, Gabriela C.; Alvarenga, Elson S.; Galindo, Juan C. G.; Macias, Francisco A.In this work we report a versatile synthesis of fourteen γ-lactones all structurally related, nine of which are novel compounds, accomplished from the readily available furfural. The phytotoxic activity of the synthesized compounds was evaluated in vitro by the influence on the growth of wheat coleoptiles. The percentages of inhibition were mostly small and not statistically different from control after the third dilution (100 µmol L-1). In general, α,β-unsaturated lactones presented better activities than the saturated ones. The most active compounds presented 51, 68 and 76% of inhibition in 1000 µmol L-1. The results indicate that regardless of saturation, the presence of the γ-lactone moiety is important for the bioactivity, but their presence has no implications with potency.Item Modificação de procedimento para extração de Boro em solos(RECIE, 2006-01) Reis, César; Reis, Efraim Lázaro; Silva, Claudinei Alves daExtração com água quente é o procedimento mais frequentemente usado na etapa inicial da determinação do boro disponível em solos. Por outro lado é um procedimento difícil de padronizar, consome tempo e a rotina usada é tediosa. Um procedimento de extração alternativo foi desenvolvido, consistindo na extração de boro com uma solução de sulfato de alumínio a 5 mmol L-1. O boro foi determinado através do método da azometina-H, que é o método espectrofotométrico mais comumente utilizado para determinação de boro. Boas correlações foram encontradas entre a extração de boro de um solo brasileiro com água quente e com solução de sulfato de alumínio. Palavras-Chave: boro, extração, azometina-H.Item Effects of composted urban solid waste addition on yield and metal contents of lettuce(Journal of the Brazilian Chemical Society, 2007) Jordão, Cláudio P.; Nascentes, Clésia C.; Fontes, Renildes L. F.; Cecon, Paulo R.; Pereira, José L.A study was performed to evaluate Cu, Mn, Ni, Pb, Ni and Zn accumulations in lettuce grown in an oxisol amended with composted urban solid wastes collected in Brazil from a big city (Rio de Janeiro, Rio de Janeiro State) and from a small city (Coimbra, Minas Gerais State). The compost samples were applied to the soil at increasing doses and different times of contact between compost and soil. The influence of the metals on the fresh and dry matter yield of leaves was also examined. Lettuce yield enhanced when the doses of the composts were increased and maximum yield was achieved in the cropping time between 15 and 20 days. The metal concentrations in the leaves augmented with the increase of the applied compost and with the increase of the time of contact between compost and soil. However, metal concentrations in the plant were below the maximum limits allowable by the food Brazilian legislation. The application of the compost from the smaller city resulted in increased lettuce productivity and lowest metal concentrations in the plants as compared to the results of the application of the compost from the bigger city.Item Avaliação de bis(4-metilfenilditiocarbimato)zincato(II) de tetrabutilamônio como acelerador em composições de borracha natural(Polímeros, 2008) Mariano, Roberta M.; Visconte, Leila L. Y.; Oliveira, Marcelo R. L.; Rubinger, Mayura M. M.Neste trabalho a substância ZNIBU [bis(4-metilfenilditiocarbimato)zincato(II) de tetrabutilamônio] foi usada em formulações de borracha natural (NR) e o seu efeito como acelerador de vulcanização foi investigado. As composições, vulcanizadas com a substância em questão, foram submetidas a testes mecânicos e os resultados comparados com os de outras composições vulcanizadas com os aceleradores comerciais CBS (N-ciclohexil-2-benzotiazol-2-sulfenamida), TMTD (dissulfeto de tetrametiltiuram) e MBTS (dissulfeto de benzotiazol). Propriedades como dureza, resiliência e densidade foram avaliadas em presença ou não da carga negro de fumo.