Validação da metodologia da avaliação de incerteza em curvas de calibração melhor ajustadas por polinômios de segundo grau

The most widespread literature for the evaluation of uncertainty - GUM and Eurachem - does not describe explicitly how to deal with uncertainty of the concentration coming from non-linear calibration curves. This work had the objective of describing and validating a methodology, as recommended by the recent GUM Supplement approach, to evaluate the uncertainty through polynomial models of the second order. In the uncertainty determination of the concentration of benzatone (C) by chromatography, it is observed that the uncertainty of measurement between the methodology proposed and Monte Carlo Simulation, does not diverge by more than 0.0005 unit, thus validating the model proposed for one significant digit.

Otimização de metodologia analítica para o doseamento de flavonoides de Bauhinia cheilantha (Bongard) Steudel

The present study examined the optimization of stabilization and extraction processes of the flavonoids of Bauhinia cheilantha (Bongard) Steudel. Four drying temperatures (room temperature, 40, 60 and 80 ºC) and seven extraction systems (distilled water, 100% methanol, 80% methanol, 100% ethanol, 80% ethanol, 80% acetone and 60% acetone) were examined. The results demonstrated a reduction in flavonoid levels with increasing drying temperatures; and 80% acetone, 80% ethanol, and methanol p.a extraction systems were found to be most efficient and its weren't differents statisticaly (p<0.05).

Salinidade em petróleo bruto: otimização de metodologia e proposta de um novo método para extração de sais em petróleo

The quantity of salts in the crude oils depends on the origin and of the wells production and these salts cause several problems during the transport and the process of refine as corrosions, incrustations and deactivation of the employed catalysts in the refineries. In this study were implemented changes for improvements in the execution of ASTM D 6470 method and has also developed a new methodology of extraction system of salts using process of mechanical agitation without heating. The results of the optimization produce larger efficiency and safety to the process compared to the traditional ASTM method.

Validação de metodologia analítica para determinação de mercúrio total em amostras de urina por espectrometria de absorção atômica com geração de vapor frio (CV-AAS): estudo de caso

Mercury is a toxic metal used in a variety of substances over the course history. One of its more dubious uses is in dental amalgam restorations. It is possible to measure very small concentrations of this metal in the urine of exposed subjects by the cold vapor atomic absorption technique. The present work features the validation as an essential tool to confirm the suitability of the analytical method chosen to accomplish such determination. An initial analysis will be carried out in order to evaluate the environmental and occupational levels of exposure to mercury in 39 members of the auxiliary dental staff at public consulting rooms in the city of Araguaína (TO).

Desenvolvimento de metodologia para determinação de piretroides em manteiga

The objective of this study was to evaluate the use of the matrix solid-phase dispersion technique associated with purification at low temperature for the determination of pyrethroids in butter. Evaluated parameters included: sample/adsorbent ratio, type of adsorbent and extractor solvent. The optimized method was validated based on predetermined requirements. The detection limits of the pyrethroids cypermethrin and deltamethrin were 0.082 and 0.11 μg g-1, and quantification limit were 0.28 and 0.32 μg g-1, respectively, with extraction percentages near 90% and coefficients of variation less than of 10%..

Metodologia para o estudo da porosidade de dolomita em ensaio de sulfatação interrompida

The aim of this work is to propose a methodology to evaluate the evolution of the pore blockage of limestone during the sulfation reaction. The experiments were performed for a national limestone (dolomite) with average particle size of 545 μm in interrupted sulfation tests were conducted at seven different times and at three different temperatures of the process. The empirical data were obtained from porosimetry tests to establish BET surface area, volume and average size of pore and distribution of pore sizes of the sulfated samples. Thermogravimetric tests were performed to evaluate the preparation methodology of the samples used in the porosimetry tests.

Síntese hidrotermal assistida por micro-ondas como metodologia sintética eficiente para obtenção da rede metalorgânica [ZN(BDC)(H2O)2]n

This work presents the optimization of the microwave-assisted hydrothermal synthesis of [Zn(BDC)(H2O)2]n . The reactions were carried out at the fixed temperature of 120 ºC for 10, 20, 30 and 40 min. Pure crystalline [Zn(BDC)(H2O)2]n was obtained in high yield (ca. 90%) with a reaction time of 10 min. The phase obtained and its purity was confirmed by Rietveld refinement, with a final value for Rwp/Rexp equal to 1.48. Increased reaction times (20, 30 and 40 min) favored the formation of unwanted by products, resulting in mixtures of several crystalline phases.

Otimização das condições de extração de saponinas em Ampelozizyphus amazonicus usando planejamento experimental e metodologia de superfície de resposta

This works describes the use of experimental design and surface response methodology for optimization of saponin extraction from Ampelozizyphus amazonicus. For this purpose, a method employing extraction based on maceration assisted by ultrasound technique was utilized. The following factors were studied: extraction length of time and solvent composition. The total saponin was determined by using a gravimetric method and the results expressed by their relative proportion to total crude extract. For the specific condition, 60% hydro-alcoholic solution and 18 minutes extraction length of time has shown the best results. This method can be useful for extraction of substances with biological importance

Metodologia para preservação do fungicida mancozebe em amostras de solo

The influence of temperature, storage time and the addition of hydrochloride L-cysteine in the preservation of the fungicide mancozeb was studied under field conditions in the surface layer of a Cambisol collected in an area planted with cabbage in Nova Friburgo - RJ, Brazil. The results of this study showed an efficiency of up to 42% in the preservation of the fungicide in the samples treated with cysteine and stored at low temperatures compared to those not treated and kept at room temperature

Avaliação de metodologia eletroquímica no monitoramento da conversão de óleo de girassol em biodiesel

The development of analytical procedures to evaluate transesterification process is still a challenge in biodiesel production. Then, this paper shows an electroanalytical methodology to transesterification process assessment, proposing the application of nanostructured TiO2 electrodes. The results showed, for sunflower oil - methanol reaction catalyzed by KOH, a reduction peak in - 1050 mV and the gradual appearance of a second peak at - 1160 mV. This peak was observed as originated by the transesterification process and is probably related to intermediates. By measuring the intensity of this peak a kinetic profile was determined, showing that the conversion is almost finished in 2 h.

Desenvolvimento de metodologia para avaliar remoção de estrogênios em estações de tratamento de esgotos

The present research aimed to study the parameters that affect the determination of estrogens in sewage upon the use of SPE and determination by using gas chromatography mass spectrometry (GC/MS). The study evaluated the stabilization pond technology with regard to estrogens removal. The results showed that the methodology was able to identify and quantify the estrogens E1, E2, E2-17A and EE2 in sewage. Moreover, the estrogens sometimes were not removed in the stabilization pond, showing that even the high hydraulic retention time (HRT) and high sunlight intensity were not enough to degrade these compounds completely during load peaks.

Metodologia de ensino jigsaw em disciplina de química medicinal

In this paper, we describe an educational experience involving the use of the jigsaw method on the Medicinal Chemistry course at the University of São Paulo, Brazil. The goal of this proposal was to investigate acceptance and contributions of the method to undergraduate chemistry teaching. Feedback on the jigsaw method collected from the focus groups and questionnaires showed that participants generally acknowledged the advantages of the jigsaw method in helping them learn the Medicinal Chemistry subject. Suggestions for improving the jigsaw method were also received from participants.

ADAPTAÇÃO DA METODOLOGIA DE ANÁLISE DE METEMOGLOBINA COMO BIOMARCADOR DE EFEITO DA EXPOSIÇÃO AO AGROTÓXICO DIFLUBENZURON

This work aimed to adapt the analysis of methemoglobin recommended by Evelyn - Malloy (visible spectrophotometry), in order to facilitate its application in the field, or to analysis in clinical laboratory, of existing sites of diflubenzuron application. The parameters changed included: centrifuge rotation speed; time between the collection of biological sample and analysis, and storage temperature of the samples; and the volume of reagents. The comparison of the rotation speed (rpm) of the reference methodology with the rpm of a "clinical centrifuge" did not reveal a statistically significant difference in the levels of methemoglobin. The time between the collection of biological sample and analysis was extended for a period of up to 48 hours for both conservation by refrigeration and ambient temperature, producing no statistically significant difference when compared to the standard duration of 2 hours. Regarding the reagents, the reference methodology already uses the volume necessary to ensure complete reaction, whereas a wider range from the recommended volume to a 5-fold reduction in comparison to the reference methodology could be used. It was concluded that the proposed changes to the methodology for adapting the analysis are applicable to studies of field / workplace exposure and ensure the reliability of results. The adapted methodology was inter-laboratory validated and the parameters changed can be selected according to the requirements of the laboratory at which the methemoglobin is to be measured.

Controle químico de Fusarium moniliforme em sementes de milho: metodologia de avaliação e efeitos sobre a qualidade fisiológica

Objetivou-se verificar o efeito da luz sobre o crescimento micelial de Fusarium moniliforme em meio de cultura contendo fungicidas, o melhor regime luminoso e a variável a ser utilizada para detectar o patógeno em sementes tratadas de milho (Zea mays), e o efeito do tratamento sobre a qualidade sanitária e fisiológica das sementes. Os fungicidas avaliados foram fludioxonil + metalaxil-m (três concentrações), difenoconazole, acibenzolar-S-metílico e captan + tiabendazole. Para avaliação do crescimento micelial, os fungicidas foram adicionados em meio de cultura, nas concentrações de 100, 10 e 1 æg/ml. Incubaram-se as placas sob temperatura de 20±2 ºC e três condições de luz: escuro contínuo, luz branca e luz próxima da ultra violeta (12h de luz/12 de escuro). Para verificar o efeito da luz na avaliação das sementes tratadas, utilizou-se o método do papel de filtro com congelamento; a sanidade foi avaliada pelas variáveis incidência e severidade. Duas amostras de sementes tratadas foram submetidas aos testes de sanidade, germinação, emergência em casa de vegetação e frio, para verificar o efeito do tratamento sobre a qualidade sanitária e fisiológica. O teste in vitro indicou que a luz branca diminuiu o efeito dos ingredientes ativos fludioxonil + metalaxil-m (7,5 g + 11,51 g/l e 25 g + 10 g/l) e captan + tiabendazole; no teste de sanidade não se observou esse efeito. A severidade foi mais sensível para discriminar a eficiência dos fungicidas. Os resultados obtidos, avaliando-se as amostras de sementes tratadas, demonstraram que: F. moniliforme não afeta a qualidade fisiológica dessas sementes; o fungicida que ofereceu controle do patógeno na semente, acima de 90%, foi captan + tiabendazole, seguido de fludioxonil + metalaxil-m (97,2 g + 147,86 g/l); Pythium sp. foi controlado por captan + tiabendazole e por fludioxonil + metalaxil-m nas três concentrações.

Geoestatística como metodologia para estudar a dinâmica espaço-temporal de doenças associadas a Colletotrichum spp. transmitidos por sementes

Objetivou-se no presente trabalho caracterizar o progresso espaço-temporal da severidade da antracnose do feijoeiro comum e da ramulose do algodoeiro por meio da Geoestatística. Os experimentos foram conduzidos no campo, durante o período das águas, em diferentes épocas. Sementes inoculadas pelo método da restrição hídrica foram semeadas no centro de parcelas experimentais constituindo fonte de inóculo do tipo ponto. Foram realizadas semanalmente seis avaliações da severidade das doenças com base em escalas de notas. Pelos modelos de semivariograma isotrópicos esféricos e gaussianos ajustados aos dados, verificou-se o padrão de distribuição agregado e a dependência espacial de ambos os patossistemas. Com o mapeamento da severidade das doenças pelo método da krigagem ordinária em blocos, verificou-se menor severidade das doenças nos primeiros estádios, com aumento gradual ao longo do tempo. A antracnose apresentou formação inicial de focos de inóculo secundário, além do foco com inóculo inicial, que coalesceram com o tempo. A severidade da ramulose diminuiu gradualmente de forma radial e contínua do centro da parcela para as extremidades, com maior capacidade de infecção de plantas vizinhas, quando comparada à antracnose, possivelmente pela maior agressividade do patógeno e hábito de crescimento arbustivo do algodoeiro.