Resumo em inglês This work presents a chemical study of human bones painted red located at the Morro dos Ossos site, Piauí State, Brazil. The pigment was studied using X-ray diffraction (XRD), energy dispersive spectroscopy (EDS), scanning electron microscopy (SEM), complexation reactions with thiocyanate and UV-Vis absorption spectroscopy. The results confirmed the presence of ochre and that the pigment layer is essentially composed of a mixture of clay and hematite, α-Fe2O3.
Resumo em português Neste trabalho avaliaram-se propriedades químicas de achocolatados do mercado brasileiro, sendo estas os teores de lipídios, proteínas, cinzas, umidade, pH, teobromina e alcalóides totais. Estas propriedades são influenciadas principalmente pelo conteúdo de cacau em pó e pelo conteúdo dos ingredientes lácteos, como o leite em pó e o soro de leite em pó. Foi feito um comparativo entre as marcas de achocolatados, dando ênfase às grandes diferenças, quando exis (mais) tentes, entre os achocolatados dietéticos (para dietas de restrição de sacarose, frutose e glicose (dextrose)) e "light" (com redução de açúcares) e os tradicionais. Resumo em inglês Some chemical properties of chocolate drink powders from Brazilian market, such as lipid, protein, ashes, moisture, pH, theobromine and total alkaloids content of the samples were evaluated. These properties are mainly influenced by cocoa powder content and by dairy products, such as milk powder and whey. A comparison among the brands, emphasizing their strong differences, when existing, among diet (without sugars) and light (low sugar) and the standard brands was made.
Química combinatória de materiais com análise por microdifração de raios X. Primeira parte: fundamentos/ Combinatorial chemistry of materials with analysis by X-ray microdiffraction. Part I: fundamentals
Resumo em inglês Combinatorial chemistry refers to techniques to rapidly fabricate tens, hundreds or even thousands of different micro samples. The analysis of the large number of samples generated by combinatorial methods requires highly efficient analytical methods. In this case, the challenges are due not only to the large number of samples to be analyzed, but also to the small amount of sample available for analysis. This paper describes the fundamentals of combinatorial chemical methods applied to discover of materials and the development in x-ray diffraction to analyze micro samples.
Microssistemas de análises químicas: introdução, tecnologias de fabricação, instrumentação e aplicações/ Micro chemical analysis systems: Introduction, fabrication technologies, instrumentation and applications
Resumo em inglês The amazing world of micro total analysis systems has provided a true revolution in analytical chemistry in recent years. The application of the microfluidic devices for chemical and biochemical processing has attracted considerable interest due to its advantages such as reduced sample and reagent consumption, processing time, energy, waste, cost, and portability. The aim of the present report is to disseminate the state of the art related to the miniaturization science i (mais) n Analytical Chemistry. Historical progress, microfabrication technologies, required instrumentation and applications of the mTAS are presented in the current article, with special attention to the Brazilian contributions.
Resumo em inglês Bisphosphonates are drugs that have been widely used in different bone diseases, and have recently been used successfully against many parasites. Various synthetic routes to prepare different types of bisphosphonates have been described, with distinct potency and pharmacological activity. A number of analytical techniques are currently being used to analyze these drugs; among these, the high performance liquid chromatography (HPLC), with different systems of detection, is (mais) worth highlighting. However, the development of more sensitive methods is still necessary, once they are essential for bioavailability and bioequivalence studies. This paper reports the major synthesis routes, chemical analysis methodologies and pharmacological applications of bisphosphonates.
Atributos químicos de solos sob diferentes usos em perímetro irrigado no semiárido de Pernambuco/ Soil chemical properties under different uses in an irrigated area in the semi arid region of Pernambuco, Brazil
Resumo em português Solos desenvolvidos em ambiente de clima semi-árido podem apresentar, naturalmente, acúmulo de sais que comprometem seu uso agrícola, o que pode ser incrementado pelo manejo inadequado da irrigação. Dependendo do uso, a degradação destes solos pode ocorrer com maior ou menor intensidade. Este trabalho teve como objetivo avaliar usos do solo utilizando atributos químicos em um perímetro irrigado na região semiárida do Nordeste do Brasil. Os usos do solo foram se (mais) parados em áreas com culturas de ciclo curto (C), com fruticultura (F), com pastagem (P), áreas descartadas (D) e áreas com vegetação nativa (V). Coletaram-se amostras de solo deformadas nas camadas de 0-10, 10-30 e 30-60 cm, e indeformadas nas duas primeiras camadas para as determinações químicas e de densidade do solo, respectivamente. Os indicadores pH e condutividade elétrica do extrato de saturação, pH do solo, P disponível, C orgânico total, Ca2+, Mg2+, K+ e Na+, CTC, soma de bases (SB), percentagem de saturação por bases (V %), percentagem de Na trocável e estoque de C foram submetidos à análise multivariada, pela técnica de análise de componentes principais, e agrupamento pelo método Tocher. Os usos relacionados a sistemas produtivos apresentaram-se diferentes quanto à qualidade química do solo em relação aos atributos analisados do uso V; entre os usos relacionados a sistemas produtivos, C e D apresentaram qualidade química mais semelhante, o mesmo ocorrendo para os usos C e P. Em relação ao uso V, os usos C, D, P e F apresentaram, nas três camadas analisadas, maiores valores dos atributos pHs, pH do extrato de saturação, condutividade elétrica do extrato de saturação, Ca e Mg trocáveis, SB, V % e P disponível. Os usos F e P apresentaram o menor teor de C orgânico total. Os usos C, D e P apresentaram maiores valores de condutividade elétrica do extrato saturado em comparação com os usos F e V, indicando o início de um processo de salinização do solo, tornando suas utilizações agrícolas menos sustentáveis. Resumo em inglês Soils developed at semi-arid climate can present salt accumulation, which compromise the agricultural use, being increased by inadequate irrigation management. Based on the use, the degradation of these soils can occur at higher or smaller intensity. This study aimed to evaluate the effect of soil uses based on physical and chemical properties of an irrigated area in the semi-arid region of northeastern Brazil. The soil uses were annual crops (C), fruticulture (F), pastur (mais) e (P), discarded lands (D), or native vegetation (V). Disturbed soil samples were collected from the 0-10, 10-30 and 30-60 cm layers for chemical analysis, and undisturbed samples from the first two layers for soil density analysis. The indicators pH and electrical conductivity of the saturation extract, soil pH, available phosphorus, total organic carbon, exchangeable cations, calcium, magnesium, potassium, and sodium, cation exchange capacity, sum of bases, base saturation percentage, percentage of exchangeable sodium, and carbon stocks were subjected to multivariate analysis by Principal Component Analysis, and clustering by the Tocher method. The soil chemical properties under production systems was different from V; the chemical quality of the production systems C and D, and that of C and P was similar. For the uses C, D, P, and F, the values of the soil properties (pH, pH and electrical conductivity of the saturation extract, exchangeable calcium and magnesium, sum of bases, base saturation and available phosphorus) was higher than for V in the three analyzed layers. The highest total organic carbon content was observed under F and P. The electrical conductivity of the saturation extract was higher under C, D and P than under F and V, indicating the beginning of a soil salinization process, thus characterizing them as less sustainable land uses.
Avaliação das características físico-químicas e fitoquímicas de diferentes tinturas de barbatimão (Stryphnodendron barbatiman)/ Evaluation of physico-chemical and phytochemical characteristics of different tinctures of barbatimão (Stryphnodendron barbatiman)
Resumo em português Como conseqüência da grande difusão e utilização de plantas medicinais, as indústrias vêm fabricando produtos a base de espécies vegetais, de diversas formas farmacêuticas, que têm sido comercializados em farmácias e casas de produtos naturais. No entanto, não há garantia para a grande maioria destes produtos, quanto à sua eficácia, segurança e qualidade, podendo trazer riscos à saúde do consumidor. Assim, torna-se importante o estabelecimento de protoco (mais) los padronizados de controle de qualidade para produtos fitoterápicos. Encontram-se disponíveis no mercado brasileiro tinturas de barbatimão provenientes de diversos fabricantes. Com a finalidade de avaliar a diferença entre a qualidade destas tinturas, foi realizado um estudo comparativo das características físico-químicas e fitoquímicas de tinturas de barbatimão provenientes de quatro fabricantes. Para a avaliação físico-química foram realizados ensaios de pH, densidade, resíduo seco e doseamento de taninos. A análise fitoquímica foi feita empregando cromatografia em camada delgada. As diferenças físico-químicas e fitoquímicas observadas evidenciaram a falta de padronização na produção destas tinturas. Resumo em inglês As a consequence of the large distribution and use of medicinal plants, the industries are producing products based on plant species in various pharmaceutical forms, which have been commercialized in pharmacies and natural products homes. However, there is no guarantee for the vast majority of these products, as to their effectiveness, safety and quality, which may cause risks to the health of consumers. Therefore it is important the establishment of standardized protocol (mais) s of quality control for phytotherapeutic products. Tinctures of barbatimão are available in the Brazilian market proceeding from diverse manufacturers. With the purpose to evaluate the difference between the quality of tinctures of barbatimão proceeding from four manufacturers, a comparative study of physico-chemical and phytochemical characteristics was carried out. For physico-chemical analysis, the pH, density, dry residue and tannins content were evaluated. The phytochemical analysis was made using thin layer chromatography. The differences observed in physico-chemical and phytochemical characteristics had evidenced the lack of standardization in the production of these tinctures.
Resumo em português Este artigo apresenta a análise térmica para os estudos das propriedades físicas e químicas de compostos e de suas misturas no contexto da área de cosméticos. Os autores relatam alguns trabalhos da literatura em que diferentes técnicas termoanalíticas são usadas na caracterização de matérias-primas, produtos cosméticos e amostras de cabelo. Resumo em inglês This paper presents the thermal analysis for the studies of the physical and chemical properties of compounds and their mixtures in the cosmetic area. The authors relate some papers in wich different thermoanalytic techniques have been used for characterization of raw material, cosmetic product and samples of hair.
Espacialização vertical e horizontal dos indicadores de qualidade para um latossolo vermelho cultivado com citros/ Vertical and horizontal spatialization of quality indicators of a typic haplortox under citrus
Resumo em português O objetivo deste trabalho foi verificar a forma de espacialização vertical e horizontal dos indicadores de qualidade química, física e hídrica de um Latossolo Vermelho distrófico textura média, cultivado com citros. O pomar de laranjeira Valência sobre limoeiro Cravo foi plantado em 1995, em Alto Paraná, região noroeste do Paraná. Em agosto de 2002, coletaram-se amostras deformadas e indeformadas de solo para realizar determinações químicas, físicas e hídr (mais) icas. A amostragem foi feita em 24 transeções perpendiculares aos troncos das laranjeiras, em duas profundidades (0-0,20 e 0,20-0,40 m) e em três posições (projeção da copa da laranjeira, rodado da entrelinha e centro da entrelinha). Os indicadores avaliados foram submetidos às análises multivariadas, por meio dos componentes principais, e agrupados pelo método de Tocher. Os resultados demonstraram que a qualidade do solo apresentou espacialização heterogênea entre os indicadores de qualidade física, química e hídrica do solo, resultante das ações de manejo do pomar de laranjeira. A integração dos indicadores de qualidade física, química e hídrica do solo caracterizou a espacialização vertical da qualidade do solo (0-0,40 m) na projeção da copa da laranjeira e a espacialização vertical e horizontal (0-0,20 e 0,20-0,40 m) no rodado da entrelinha e centro da entrelinha. No rodado da entrelinha (0-0,20 m) ocorreu a maior restrição física e hídrica associada à melhor condição química do solo para as laranjeiras. Resumo em inglês The objective of this report was to verify the form of vertical and horizontal spatialization of chemical, physical and water quality indicators of a Typic Haplortox cultivated with citrus. The 'Valencia' orange grove on 'Rangpur' lime was planted in 1995, in the county of Alto Paraná, northwestern Paraná, Brazil. In August 2002, undisturbed and disturbed samples were collected for chemical, physical and water analysis. Twenty-four transects were sampled perpendicular t (mais) o the tree trunk, in two layers (0-0.20 and 0.20-0.40 m depth) and three sampling positions (tree crown projection, underneath the wheel track and between the wheel tracks). The indicators measured were submitted to multivariate analysis by main components and were grouped by the Tocher method. The soil quality demonstrated heterogeneous spatialization among the soil physical, chemical and water soil quality indicators, as a result of the management actions on the plantation. The integration of the soil indicators of physical, chemical and water quality characterized a vertical spatialization (0-0.40 m) in the tree crown projection and vertical and horizontal spatialization (0-0.20 and 0.20-0.40 m) underneath and between the wheel tracks. Underneath the wheel tracks (0-0.20 m) the physical and water restrictions were strongest while soil chemical conditions for orange trees were the best.
Controles físico, físico-químico, químico e microbiológico dos frutos de Dimorphandra mollis Benth., Fabaceae/ Physic, physic-chemical, chemical and microbiological control of fruits of Dimorphandra mollis Benth., Fabaceae
Resumo em português Considerando-se a qualidade dos fitoterápicos, é importante salientar que a preocupação com esta questão inclui rigoroso acompanhamento das diferentes etapas de desenvolvimento e produção, desde a coleta do vegetal até o produto final. O controle de qualidade de drogas vegetais e seus extratos é essencial quando utilizados como matéria-prima para o desenvolvimento de fitoterápicos. Neste trabalho foram utilizadas diversas técnicas (farmacopeicas e não farmaco (mais) peicas) visando estabelecer parâmetros de qualidade dos frutos de Dimorphandra mollis Benth. (Leguminosae), popularmente conhecida como faveiro. Os resultados obtidos determinaram as características físico-químicas da droga vegetal e mostraram que o pó dos frutos e o extrato etanólico 70% de D. mollis apresentam um teor de flavonóides de 10,25% e 17,21%, respectivamente. A análise fitoquímica preliminar dos frutos caracterizou a presença de taninos, saponinas e flavonóides. Na análise microbiológica do extrato não houve crescimento de patógenos entre os testes realizados. Resumo em inglês Considering the quality of phytotherapic agents, it is important to point out that the concern with this subject includes rigorous attendance the different steps of development and production of these products, from the collection of the vegetable to the availability of the final product. The quality control for the plants and their extracts is essential when they are used in the development of phytotherapics. In this work, methodologies (pharmacopoeic and no pharmacopoei (mais) c) were employed to establish norms for the quality control of Dimorphandra mollis Benth. (Leguminosae) fruit, popularly known as faveira. Pharmacopoeic and no pharmacopoeic methodologies were employed to physic, physic-chemical, chemical and microbiological quality control. The results obtained established the physic-chemical characters of the drug and showed that the fruits and the ethanol 70% extract present a content of flavonoids of 10.25% and 17.21%, respectively. The preliminary phytochemical analysis of the D. mollis fruits evidenced tannins, saponnins and flavonoids. The microbiological analysis did not present pathogenic growth among the accomplished tests.
Limites de consistência e propriedades químicas de um latossolo amarelo distrocoeso sob aplicação de diferentes resíduos da cana-de-açúcar/ Limits of consistency chemical properties of a dystrophic cohesive yellow latosol under different sugarcane residues
Resumo em português Os solos dos tabuleiros costeiros cultivados com cana-de-açúcar, durante longo período de tempo, sob sistemas de manejo com diferentes aportes de matéria orgânica podem apresentar alterações nas propriedades físicas e químicas. O objetivo deste trabalho foi avaliar o efeito do aporte de matéria orgânica pelos diferentes sistemas de manejo da cana-de-açúcar sobre as propriedades físicas e químicas de um Latossolo Amarelo distrocoeso dos tabuleiros costeiros (mais) de Alagoas. Foram selecionadas áreas em talhões de produção com a cultura da cana-de-açúcar, sendo objeto de pesquisa experimental três áreas, representativas de três sistemas de manejo adotados pela unidade sucroalcooleira: uma área cultivada sob sistema de manejo irrigado (SMI), uma área sob sistema de manejo de fertirrigação com vinhaça (SMV) e uma área sob sistema de manejo com aplicação de vinhaça + torta de filtro (SMVT). Esses sistemas de manejo foram comparados entre si e em relação a uma testemunha-padrão, representada por um fragmento de Mata Atlântica nativa (MN). Para avaliar as propriedades físicas e químicas, amostras de solo foram coletadas ao acaso, nas áreas submetidas aos diferentes sistemas de manejo, nas profundidades de 0-0,20, 0,20-0,40 e 0,40-0,60 m, sendo retiradas num ponto situado nas entrelinhas da cana-de-açúcar. Os resultados foram submetidos à análise de variância e as médias comparadas pelo teste de Tukey a 5 %. Estudos de correlações simples foram realizados entre algumas variáveis medidas. Os resultados permitiram concluir que os diferentes sistemas de manejo investigados promoveram alterações nas propriedades físicas e químicas do solo. As medidas de consistência do solo apresentaram tendência de aumento em seus valores com o incremento do carbono orgânico total (COT) do solo, promovido pela adição de resíduos da cana-de-açúcar. Os sistemas de manejo que receberam adição de resíduos da cana-de-açúcar denotaram menor degradação nas propriedades físicas e químicas do solo. Resumo em inglês The physical and chemical properties of coastal plain soils cultivated with sugarcane for a long period under different management systems may undergo changes. The objective of this study was to evaluate the effects of different sugarcane management systems on the chemical and physical properties of a dystrophic cohesive Yellow Latosol of coastal tablelands in the state of Alagoas. Three experimental plots were selected in sugarcane growing areas, representing the three m (mais) anagement systems used for ethanol production, namely: a cultivated area under irrigation management, an area under fertirrigation with vinasse and an area with application of vinasse + filter cake. The management systems were compared with each other and with a control area of native forest. To assess physical and chemical properties, soil samples were randomly collected in the areas under different management systems at depths of 0-0.20; 0.20-0.40 and 0.40-0.60 m, from the sugarcane interrows. The results were subjected to analysis of variance and the means compared by the Tukey test at 5 %. Simple correlation analysis was performed between some variables. Results showed changes in the soil physical and chemical properties due to the different management systems. The soil consistency parameters tended to increase with the increase of total organic carbon, resulting from the application of sugar cane waste. In the management systems with application of sugar cane waste the deterioration in soil physical and chemical properties was reduced.
Atributos físicos, químicos e biológicos de solo de cerrado sob diferentes sistemas de uso e manejo/ Physical, chemical and biological properties of cerrado soil under different land use and tillage systems
Resumo em português À medida que o conhecimento do sistema plantio direto se amplia, verifica-se que o uso de indicadores químicos isolados não permite melhor caracterização dos solos, sendo necessário utilizar um conjunto de indicadores da qualidade do solo com a entrada de outros atributos, entre eles os físicos e os biológicos. Objetivou-se avaliar os efeitos de sistemas de manejo e uso do solo nos atributos físicos, químicos e biológicos de um Latossolo Vermelho distrófico e (mais) um Neossolo Quartzarênico órtico sob Cerrado, no entorno do Parque Nacional das Emas. Os aspectos avaliados no Latossolo foram: Cerrado nativo, pastagem, milheto em preparo convencional, nabo forrageiro em plantio direto e sorgo em plantio direto. No Neossolo: Cerrado nativo, pastagem nativa, integração agricultura-pecuária, pastagem cultivada, plantio direto com soja no verão e plantio direto com milho no verão. As amostras de solo foram coletadas na profundidade de 0 a 10 cm. O delineamento experimental foi o inteiramente casualizado, com cinco parcelas de 150 m², sendo coletadas 10 subamostras aleatórias. As análises químicas, físicas e biológicas foram realizadas no Laboratório de Solos da UFG/CJ. Os manejos promoveram alterações na densidade do solo, volume total de poros, macroporos e resistência do solo à penetração no Neossolo e no Latossolo, excetuando-se neste o volume total de poros. Houve pequena variação nos atributos químicos nos dois solos, com o Cerrado apresentando maior acidez potencial e menor teor de cátions trocáveis e P. Os atributos biológicos do solo foram alterados pelos sistemas de manejo, sendo mais prejudicados em sistemas com maior revolvimento do solo. A análise canônica dos dados demonstrou que os atributos físicos foram os de menor importância por apresentar maior coeficiente de ponderação nas variáveis canônicas. Os atributos do solo, isoladamente, pouco contribuíram para a avaliação da qualidade do solo: no entanto, quando se usou a análise multivariada, subsidiaram a constatação dos manejos do solo mais sustentáveis. Resumo em inglês As knowledge on no-till system expands, it has become quite clear that separate chemical indicators cannot provide a detailed soil characterization. The objective of this study was to evaluate the effects of tillage systems and soil use in the physical, chemical and biological properties of a clayey dystrophic Red Latosol - Oxisol and a sandy Neosol - Entisol. The treatments for the Oxisol consisted of: native savanna, pasture, conventional tillage, no-tillage with turnip (mais) and with forage sorghum as cover crop. For the Entisol: native savanna, native pasture, integrated crop-livestock, cultivated pasture, no-tillage with soybean and corn in the summer. Soil samples were collected from a depth of 0-10 cm, in a clayey dystrophic Red Latosol - Oxisol and a sandy Neosol - Entisol in a savanna ecosystem, near the Parque Nacional das Emas. Treatments were arranged in a completely randomized design, in 5 plots of 150m², where 10 sub-samples were collected randomly. Chemical, physical and biological analyses were carried out at a soil laboratory. In the Entisol, tillage influenced the soil density, total pore volume, macroporosity and penetration resistance. In the Oxisol, tillage induced variations in soil bulk density, macroporosity and penetration resistance. Small variations in chemical properties were observed in both soils, with higher potential acidity and lower exchangeable cation and phosphorus concentrations. The soil biological properties were influenced by tillage, and were most affected in systems with more anthropic action. In the canonical data analysis the greater weighting coefficient of the physical properties in the canonic variables demonstrated that these were the least important. The contribution of the separate soil properties to evaluate soil quality was minor, but the most sustainable management systems could be defined by multivariate analysis.
Resumo em português No estudo do mapeamento da fertilidade do solo, pelas técnicas de geoestatística, algumas características estruturais da variabilidade espacial devem ser consideradas, tais como continuidade espacial e ausência de anisotropia. Neste contexto, o presente trabalho apresenta uma análise da anisotropia no estudo da variabilidade espacial das variáveis químicas do solo: ferro (Fe), acidez potencial (H + Al), matéria orgânica (MO) e Mn, de um conjunto de dados de 128 p (mais) arcelas sem manejo químico localizado, espacialmente referenciados, estudados entre 1998 e 2002, em um Latossolo Vermelho distroférrico, em Cascavel-PR. A identificação da anisotropia foi realizada por meio da construção de semivariogramas direcionais com modelos ajustados, e a correção da anisotropia realizou-se por meio de transformações lineares e de modelos combinados. Em seguida, utilizou-se um modelo ajustado ao semivariograma omnidirecional para construção de mapas temáticos de variabilidade das variáveis estudadas. Observou-se a existência de anisotropia geométrica para a variável H + Al. Já as variáveis MO, Mn e Fe mostraram a presença de anisotropia combinada, sendo corrigida inicialmente a anisotropia geométrica e, posteriormente, a anisotropia zonal. Por meio do estudo da anisotropia, foi possível eliminar as direções privilegiadas, melhorando assim o ajuste dos semivariogramas e produzindo mapas temáticos das variáveis químicas estudadas com maior acurácia. Resumo em inglês Studies on soil fertility mapping based on geostatistics should consider some spatial variability characteristics such as spatial continuity and absence of anisotropy. The present study reports an anisotropic analysis of the spatial variability of the following soil chemical variables: iron (Fe), potential acidity (H + Al), organic matter (OM) and manganese (Mn) of a data set of 128 plots without local chemical management, spatially referenced, studied between 1998 and 20 (mais) 02 in a dystrophic Red Latosol (Oxisol), in Cascavel, Paraná, Brazil. Anisotropy was identified through the construction of directional semivariograms with adjusted models and corrected through linear transformations and by combined models. Thereafter a model was used adjusted to the omnidirectional semivariogram for the construction of thematic variability maps of the studied variables. The existence of geometric anisotropy was observed for the variable H + Al. The variables MO, Mn and Fe evidenced the presence of combined anisotropy. The geometric anisotropy was first corrected and then the zonal anisotropy was adjusted. Based on anisotropy it was possible to eliminate the biased directions, enhancing the semivariogram fitting and precision of the thematic maps of chemical variables.
Resumo em inglês In this work, the perovskite-type oxides LaNiO3, LaMnO3, La0,7Sr0,3NiO3 and La0,7Sr0,3MnO3 were prepared by co-precipitation and tested in the NO reduction with CO at 400 and 500 ºC for 10 h. The catalysts were characterized by X-ray diffraction, temperature programmed reduction with hydrogen, nitrogen adsorption and chemical analysis. The nonstoichiometric oxygen was quantified by temperature programmed reduction, and the catalytic tests showed that the La0,7Sr0,3MnO3 c (mais) atalyst presented the higher performance for the reduction reaction of NO with CO. The partial substitution of lanthanum by strontium increased the NO conversion and the N2 yield.
In this study, the profile of tocopherols and tocotrienols in chestnut (Castanea sativa Mill.) kernel oilwas evaluated. Four Portuguese chestnut varieties were selected: Aveleira, Boaventura, Judia, andLongal. The vitamin E determination had already been applied to similar matrices, but, to theau...
Variação anual do rendimento e composição química dos componentes voláteis da Siparuna guianensis Aublet/ Annual variation of yield and chemical composition of volatile components of Siparuna guianensis Aublet
Resumo em inglês This work describes the volatile composition obtained by hidrodistillation of fresh leaves of Siparuna guianensis Aublet collected from Cuiabá (MT), Brazil. The composition of DCM extract of hydrolate was determined by GC-MS analysis and the results showed that the specie present a range of components according to their phenology and period of the leaves were collects. The highest volatile components yield was obtained during the reproductive period and the principal compound was the siparunone.
Variabilidade espacial e temporal de parâmetros físico-químicos nos rios Turvo, Preto e Grande no estado de São Paulo, Brasil/ Spatial and seasonal variability of physic-chemical parameters in Turvo, Preto and Grande rivers on São Paulo state, Brazil
Resumo em inglês This work aims to study spatial and seasonal variability of some chemical-physical parameters in the Turvo/Grande watershed, São Paulo State, Brazil. Water samples were taken monthly, 2007/07-2008/11, from fourteen sampling stations sited along the Turvo, Preto and Grande Rivers and its main tributaries. The Principal Component Analysis and hierarchical cluster analysis showed two distinct groups in this watershed, the first one associated for the places more impacted by (mais) domestic effluent (lower levels of dissolved oxygen in the studied region). The sampling places located to downstream (Turvo and Grande rivers) were discriminate by diffuse source of pollutants from flooding and agriculture runoffs in a second group.
Resumo em português O objetivo do presente estudo foi analisar a variabilidade espacial de atributos químicos de um Latossolo Vermelho-Amarelo húmico. O estudo foi realizado em uma área cultivada com Coffea arabica L. variedade Catuaí. As amostras de solo foram coletadas na profundidade de 0-20 cm, distribuídas em uma malha amostral, com 50 pontos. Os atributos químicos estudados foram: P, Na e S disponíveis, Ca, Mg e Al trocáveis, pH, H + Al, SB, t, T, V, m, MO, ISNa, P-remanescente (mais) e micronutrientes (Zn, Fe, Mn, Cu e B). Os dados foram analisados por meio da análise da estatística descritiva, seguida de uma análise de componentes principais com posterior análise de agrupamento. A geoestatística foi utilizada para verificar a existência e quantificar o grau de dependência espacial dos componentes principais. O método de análise multivariada com base nos componentes principais forneceu componentes interpretáveis, sendo o primeiro relacionado com a acidez e o segundo com o teor de matéria orgânica do solo. As técnicas de análise multivariada, em associação com a geoestatística, facilitaram a avaliação da variabilidade do solo; os componentes principais 1 e 2 apresentaram dependência espacial moderada, com maior continuidade espacial observada para o componente 1, o que permitiu melhor caracterização da acidez do solo. O solo em estudo apresentou, ao longo da encosta, disponibilidade reduzida de nutrientes, considerável acidez, menores teores de matéria orgânica na porção central da área e valores elevados de Al trocável na porção superior desta. Resumo em inglês The objective of this study was to analyze the spatial variability of chemical attributes of an Oxisol. The experiment was conducted with Coffea arabica L., variety Catuai, at a depth of 0-0.2 m in a grid area totaling 50 points. The studied chemical attributes were: P, K, Ca, Mg, Na, S, Al, pH, H + Al, SB, t, T, V, m, MO, ISNa, equilibrium P and micronutrients (Zn, Fe, Mn, Cu, and B). The data were analyzed by descriptive statistical analysis, followed by principal compo (mais) nent with subsequent cluster analysis. The existence of spatial dependence was verified and the degree quantified using the principal components and geostatistics. The method of multivariate analysis based on principal components provided interpretable components; the first were correlated with acidity and the second with soil organic matter. Techniques of multivariate analysis, in combination with geostatistics, facilitated the evaluation of soil variability. The principal components 1 and 2 indicated moderate spatial dependence, with greater spatial continuity in component 1, which allowed a better characterization of soil acidity. Reduced availability of soil nutrients and considerable acidity were observed along the slope, lower levels of organic matter in the center of the area and high Al contents in the upper part.
Uso de scanner em espectrofotometria de absorção molecular: aplicação em experimento didático enfocando a determinação de ácido ascórbico/ Molecular absorption spectrophotometry using a scanner: proposal of a didactic experiment for ascorbic acid determination
Resumo em inglês Quantitative analysis of colored substances is generally performed using a spectrophotometer for detection of radiation. However, the combination of digital images and mathematical conversion of colors is an alternative for quantitative procedures based on colored chemical reactions. This work proposes a didactic experiment using a scanner for determination of ascorbic acid in medicines based on the formation of the Prussian blue complex. Results were in good agreement wi (mais) th a conventional spectrophotometer method and the procedure is attractive for instrumental analysis undergraduate courses.
Resumo em inglês This paper describes a comparative analysis on natural product chemistry between the Brazilian Chemical Society journals and twelve representative international publications in the area. The search using the ISI Web of Knowledge disclosed 41,362 publications in the years 2000-2002 containing at least one researcher from a Brazilian Institution, from which 12% belongs to natural products.
Um novo modelo para os sítios de interação dos antagonistas H2, baseado na caracterização química dos sítios primário e secundário por QSAR- 3D/ A new model for the H2 antagonists binding site based on 3D QSAR analysis
Resumo em inglês A new model for the H2 antagonists binding site is postulated based on adsorption coefficient values of sixteen antagonists, in the affinities constants of the primary and secondary binding sites, and in the chemical characterization of these sites by 3D-QSAR. All study compounds are in the extended conformation and deprotonated form. The lateral validation of the QSARs, CoMFA analysis, affinity constants and chemical similarity data suggest that the antagonists block the proton pump in the H2 receptor interacting with two tyrosines - one in the helix 5, and other in the helix 6.
Resumo em inglês A series of open source benchmarks for computer performance analysis of personal computers with a focus on computational chemistry calculations is presented. The results returned by these tests are discussed and used to correlate with the actual performance of a set of computers available for research on two computing intensive fields of chemistry, quantum chemical and molecular simulation calculations.
Resumo em inglês The chemical study of the propolis produced in Teresina city, state of Piaui, resulted in the identification of six cycloartane triterpenoids: isomangiferolic acid, 24-methylenecycloartane-3beta,26-diol, mangiferolic acid, mangiferonic acid, ambonic acid and ambolic acid. The substances were characterized by one and two-dimensional ¹H and 13C NMR analysis.
Resumo em inglês Chemical investigation of the leaves of Styrax camporum (Styracaceae) resulted in the isolation of the lignan lariciresinol and six triterpenes: ursolic acid, 2alpha,3alpha-dihydroxy-urs-12-en-28-oic acid and mixtures of uvaol and erythrodiol, as well as 3beta-O-trans-p-coumaroyl-2alpha-hydroxy-urs-12-en-28-oic acid and 3b-O-trans-p-coumaroylmaslinic acid. The structures of these compounds were established by spectroscopic analysis. This paper deals with the first report of these compounds in S. camporum.
Resumo em inglês This paper describes the isolation of the furanocassane-type diterpene, named vinhaticoic acid, along with beta-farnesene and spatulenol from fruit shells of D. lacunifera. Structural determinations were accomplished by chemical derivatization and spectral analysis, including 1D and 2D NMR and X-ray crystallography. The fatty portion was extracted from the fruit kernels, transesterfied and analysed by HRGC/MS. Oleic acid (75.8 ± 4.3%) was the major component. Essen (mais) tial oil extracted from the fruit shells of D. lacunifera was analysed by HRGC/MS and nine sesquiterpenes were identified; beta-farnesene (48.6%) and spatulenol (21.61%) were the major constituents.
Síntese e caracterização de nanopartículas de óxido de ferro suportadas em matriz carbonácea: remoção do corante orgânico azul de metileno em água/ Synthesis and characterization of iron oxide nanoparticles supported on carbon matrix: oxidation of the dye methylene blue in water
Resumo em inglês In this work were prepared composites of iron oxide and carbonaceous materials in two different weight proportions (Carbon/Fe 1/1 and 1/2). The physico-chemical properties of the composites were determined by temperature programmed reduction (TPR), adsorption/dessorption of N2, X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and pulse titration H2. The XRD and XPS analysis showed a cubic iron oxide phase, identified as maghemite, formed over the carbon sur (mais) face. The particle size of maghemite showed to be within 10-30 nm. Carbon/Fe 1/2 was the most active in MB removal kinetics and ESI-MS studies showed that MB removal by both composites leads to oxidized intermediates.
Resumo em inglês Classical methods of analysis played a fundamental role in the development of Chemistry and the chemical industry. They have been tools for analytical procedures since the 18th century, remaining useful until today. The technological appeal of the instrumental methods seems to dazzle the incoming generations of chemists who do not recognize the importance of titrimetry. A short description of the development of titrimetry is presented in order to call attention to histori (mais) cal landmarks for teaching and learning activities in Portuguese. A compilation of some current standard analytical methods that employ titrations is presented to illustrate the availability of titrimetry nowadays.
Sintesis de poliuretanos a partir de polioles obtenidos a partir del aceite de higuerilla modificado por transesterificación con pentaeritritol/ Polyurethanes sintetized of polyols obtained from castor oil modified by transesterification with pentaerythritol
Resumo em inglês Castor oil was reacted by transesterification with various percentages in mass of pentaerythritol to obtain different esters of pentaerythritol. Alternatively, glycerol was also used instead of pentaerythritol for the same reaction in order to establish comparative reference products. The products of the reactions were characterized by matrix-assisted laser desorption/ionization time-of-flight mass spectroscopy in order to detect and quantify (in terms of the molecular ma (mais) ss and structural information) the components of the products obtained. Analysis for hydroxyl value, acid value, viscosity and specific gravity were used to complete the characterization of the polyols obtained and also of the original castor oil. The polymer characterization was accomplished by tensile stress-strain tests, Shore A hardness, thermogravimetric analysis and chemical resistance to solvents.
Resumo em inglês Chemical composition and dry matter (DM) productivity of 25 genotypes of sorghum were obtained. The experiment was carried out in a randomized block design with 25 treatments and three replications each. The data were submitted to analysis of variance and the means grouped by Scott-Knot Test (5%). The level of DM productivity varied from 6.82 to 14.17ton/hectare, and the higher level was obtained by VOLUMAX genotype (16.09 ton/hectare). The levels of crude protein varied (mais) from 5.24 to 7.79%. No differences were detected between the genotypes to neutral detergent fiber levels, which varied from 59.03 to 73.04%. Considering the level of acid detergent fiber, the variation interval was 26.78 to 40.92%. The better genotypes for silage production were ATF54*9929036, CMSXS212*9929048, CMSXS217*9929012, and VOLUMAX.
Resumo em inglês Glass-ceramics foams prepared from glasses of the SiO2-Na2O-CaO-P2O5 by replication process were obtained and characterized in terms of their chemical and physical properties by X-ray fluorescence, X-ray diffraction, laser diffraction, thermal analysis, density, mechanical strength, microstructural and cytotoxic analysis. The results showed that it is possible to produce glass-ceramic foams by the replication method with optimized properties but cytotoxic analysis indicat (mais) es that the glass-ceramic foams are not bioactive materials. Mechanical strength values varying from 0.5 to 1.0 MPa and from 0.8 to 2.3 MPa were reached for mean particle sizes of 10 and 6 µm, respectively.
Preparo de óxido de nióbio suportado em alumina por deposição química em fase vapor: caracterização por espectroscopia vibracional e termogravimetria/ Alumina supported niobium oxide prepared by chemical vapor deposition: characterization by vibrational spectroscopy and thermogravimetric analysis
Resumo em inglês Alumina supported niobium oxide was prepared by chemical vapor deposition (CVD) of NbCl5. The alumina was calcined and pretreated at differents temperatures in order to vary the density of OH groups on the surface which was determined by thermogravimetric analysis. A good correlation was found between the amount of anchored niobium and the total number of anionic sites (oxide and hydroxyl groups) on the surface of the alumina. The infrared spectra on the OH stretching region indicate that OH groups coordinated to at least one tetrahedral aluminum were more reactive towards NbCl5.
Pilarização de uma argila brasileira com poliidroxications de alumínio: preparação, caracterização e propriedades catalíticas/ Pillarization of a brazilian clay with aluminium polyhydroxications: preparation, characterization and catalytic properties
Resumo em inglês Montmorillonite clay from Brazil was pillared with aluminium polyhydroxications. The influence of aging of the pillaring solution and the concentration of the clay suspension on the properties of the prepared materials was studied. The materials were characterized by chemical analysis, XRD and pore analysis by N2 adsorption. The catalytic properties were evaluated in the cumene cracking reaction. Results showed that the pillarization process increases the basal spaces of natural clay from 9.7 to 18.5 Å and the surface area from 41 to 300 m²/g.
Analysis of phenolic compounds in sixteen Portuguese wild mushrooms species has been carried out byhigh-performance liquid chromatography coupled to photodiode array detector and mass spectrometer(HPLC–DAD–ESI/MS). No flavonoids were detected in the analysed samples, but diverse phenolic acidsnam...
Perfil químico de cultivares de feijão (phaseolus vulgaris) pela técnica de high resolution magic angle spinning (HR-MAS)/ Chemical profile of beans cultivars (phaseolus vulgaris) by ¹h nmr - high resolution magic angle spinning (HR-MAS)
Resumo em inglês The application of one-dimensional proton high-resolution magic angle spinning (¹H HR-MAS) NMR combined with a typical advantages of solid and liquid-state NMR techniques was used as input variables for the multivariate statistical analysis. In this paper, different cultivars of beans (Phaseolus vulgaris) developed and in development by Embrapa - Arroz e Feijão were analyzed by ¹H HR-MAS, which have been demonstrated to be a valuable tool in its differentiation according chemical composition and avoid the manipulation of the samples as used in other techniques.
Four Portuguese chestnut cultivars from the “Castanha da Terra Fria” protected designation of originwere selected: Aveleira, Boa Ventura, Judia and Longal. The nutritional parameters (moisture, fat,protein, carbohydrates, ash and energy) as well as fibers (neutral detergent fiber, acid detergentf...
Resumo em inglês A new version of the normal coordinate analysis package NCT is presented. The upgrade was mainly devised to enable the NCT package to manipulate easily the Hessian matrix evaluated by quantum chemical calculations. Program codes were almost wholly rewritten to be more efficient with GNU Fortran77, or g77, and compiled under FreeBSD and MS-DOS with the DJGPP implementation. Three typical usages of the program package are presented by giving the related input and output files. Functionality of the programs was carefully and satisfactorily checked for some sample calculations.
Resumo em inglês Fumonisins are mycotoxins occurring worldwide, mainly in maize and maize-based food products, which could affect animal and human health. This paper reviews analytical methodologies for the determination of these fungal toxins in foods. It includes extraction, cleanup, derivatization procedures, detection, quantification, and confirmation procedures. Initial attempts at gas chromatographic methods and thin layer chromatography were supplanted by liquid chromatographic met (mais) hods, mainly performed with fluorometric detection, or mass spectrometry detection, enabling the analysis of polar and thermolabile chemicals without chemical derivatization, which results in lower limits of detection. Alternative methods, such as enzyme linked immunosorbent assay or zone capillary zone electrophoresis, are also described.
Lipídios estruturados obtidos a partir da mistura de gordura de frango, sua estearina e triacilgliceróis de cadeia média: I- Composição em ácidos graxos e em triacilgliceróis/ Structured lipids from chicken fat, its atearin and medium chain triacyglycerol blends: I- Fatty acid and triacyglycerol compositions
Resumo em inglês The purpose of this study is to analyze the interactions that occur in binary and ternary fat blends between medium and long chain triacylglycerols and their structured lipids obtained by chemical interesterification through the analysis of their physico-chemical properties. The synthesized structured triacylglycerols presented from 14.8 to 58.4% medium chain fatty acids, from 15.7 to 37.2% saturated fatty acids, from 19.2 to 47.5% monounsaturated fatty acids, and from 6. (mais) 7 to 15.2% essential fatty acids. Chemical interesterification modified the behavior of binary and ternary mixtures and new types of triacylglycerol groups were formed.
Interesterificação química de óleo de soja e óleo de soja totalmente hidrogenado: influência do tempo de reação/ Chemical interesterification of soybean oil and fully hydrogenated soybean oil: Influence of the reaction time
Resumo em inglês Chemical interesterification is an important alternative to produce zero trans fats. In practice, however, excessive reaction times are used to ensure complete randomization. This work evaluated the influence of the reaction time on the interesterification of soybean oil/fully hydrogenated soybean oil blend, carried out in the following conditions: 100 ºC, 500 rpm stirring speed, 0.4% (w/w) sodium methoxide catalyst. The triacylglycerol composition, solid fat content and (mais) melting point analysis showed that the reaction was very fast, reaching the equilibrium within 5 min. This result suggests the interesterification can be performed in substantially lower times, with reduction in process costs.
Resumo em inglês The quantitative chemical analysis of the Brazilian sugar cane spirit distilled from glass column packaged with copper, stainless steel, aluminum sponge, or porcelain balls is described. The main chemical compounds determined by gas chromatography coupled with flame ionization (FID) and flame photometric (FPD) detectors and liquid chromatography coupled with diode array detector are aldehydes, ketones, carboxylic acids, alcohols, esters and dimethylsulfite (DMS). The spir (mais) its produced either in columns filled with copper or aluminum pot still exhibits the lowest DMS contents but the higher sulfate and methanol contents, whereas spirits produced in stainless steel or porcelain showed higher DMS concentration and lower teors of sulfate ion and methanol. These observations are coherent with DMS oxidation to sulfate, with methanol as by product, in the presence of either copper or aluminum.
Hidrólise do óleo de Azadirachta indica em água subcrítica e determinação da composição dos triacilglicerídeos e ácidos graxos por cromatografia gasosa de alta resolução a alta temperatura e cromatografia gasosa de alta resolução acoplada à espectrometria de massas/ Hydrolysis of Azadirachta indica oil using subcritical water and determination of triacylglycerides and fat acids by HT-HRGC-FID and HRGC-MS
Resumo em inglês The development of modern analytical tools plays an important role in quality control. The main purpose of this study was to explore the use of subcritical water as a versatile analytical tool, employed simultaneously as a reagent and solvent, as well as the application of high temperature-high resolution gas chromatography (HT-HRGC) to develop a procedure for the analysis of triacylglycerides and fatty acids in Azadirachta indica A. Juss. (Neem) oil without the need for (mais) solvents, chemical reagents, or catalytic agents. The developed method presented satisfactory results and is in agreement with the concepts of Green Analytical Chemistry (GAC).
Resumo em inglês The concentration of 15 polycyclic aromatic hydrocarbons (PAHs) in 57 samples of distillates (cachaça, rum, whiskey, and alcohol fuel) has been determined by HPLC-Fluorescence detection. The quantitative analytical profile of PAHs treated by Partial Least Square - Discriminant Analysis (PLS-DA) provided a good classification of the studied spirits based on their PAHs content. Additionally, the classification of the sugar cane derivatives according to the harvest practice (mais) was obtained treating the analytical data by Linear Discriminant Analysis (LDA), using naphthalene, acenaphthene, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, benz[a]anthracene, benz[b]fluoranthene, and benz[g,h,i]perylene, as a chemical descriptors.
Resumo em inglês Technological innovation connects competitiveness and knowledge. In Brazil, knowledge is mainly concentrated in the universities which undertake R&D. This article aims to show the importance of Brazilian university extension activities, which transfer knowledge to society, contributing, in the case of the chemical sector, to a reduction in the country's total trade deficit of around US$8.5 billion, which is result of the importation of innumerable products. On the other h (mais) and, developed countries are resorting to technical barriers, which impose documentation and regulations based on testing products for conformity with standards. This demands a technical and scientific infrastructure, concentrated in the universities.
Estudos químicos e biológicos de Microgramma vacciniifolia (Langsd. & Fisch.) Copel (Polypodiaceae)/ Chemical and biological studies of Microgramma vacciniifolia (Langsd. & Fisch.) Copel (Polypodiaceae)
Resumo em inglês Chemical studies with aerial parts of Microgramma vacciniifolia (Langsd. & Fisch.) Copel. afforded ²-sitosterol, hopan-22-ol, 6-metoxiapinenin-7-O-²-D-allopyranoside and a mixture containing ethyl esters of carboxilic acids. The structures of the coumpounds were elucidated by spectroscopy and GC-MS analysis. The total phenolics contents of the crude extract and fractions were determined by Folin-Ciocalteau method. The antioxidant activity was evaluated using the 2,2-dip (mais) henyl-1-picrylhydrazyl (DPPH). The AcOEt fraction showed better activity in DPPH assay (9.9 ± 0.03 µg/mL), and presented also higher contents of the total phenolic (93.60 ± 1.11 µg/mg). Antimicrobial and allelopathic effects of the crude etanolic extract and fractions also were evaluated. In addition, the combination of biological activities was discussed.
Estudo químico e perfil cromatográfico das cascas de Aspidosperma parvifolium A. DC. ("pau-pereira")/ Chemical constituents and chromatographic profile of the stem bark of Aspidosperma parvifolium A. DC. ("pau-pereira")
Resumo em inglês Four known alkaloids, uleine, epiuleine, apparicine and desmethyluleine, besides the isoprenoids lupeol and stigmasterol were isolated from the stem bark of Aspidosperma parvifolium. Their identification was based on spectroscopic analysis (UV, IR, ¹H-NMR, 13C-NMR, MS). The chromatographic profile of the ethanolic extract was obtained by HPLC and uleine, epiuleine and apparicine were identified in the extract.
Resumo em inglês This survey determined the physical and chemical properties of the gravel place where urban sludge from Rio Descoberto's Water Treatment Plant is disposed. Physical, chemical and biological analysis of the soil samples (n=54), sludge samples (n=2), chemical coagulant (n=20) and samples from superficial waters (n=9) and water table (n=60) were performed. As results we can emphasize the horizontal distribution of mineral phases like gibbsite, organic material, exchanged Ca, (mais) available Mn and P on the soils are originated from the sludge. Some of these mobile elements could stimulate the growing of the vegetation, but they also could contaminate the water table.
Resumo em inglês Chemical investigation from root barks of Z. rigidum, resulted in the isolation of lupeol, a mixture of steroids campesterol, sitosterol, stigmasterol, sacarose, hesperidin, N-methylatanine and 6-acetonyldihydrochelerythrine. Their structures were established by spectral data analysis. No previous work has been reported on Z. rigidum species.
Resumo em inglês From the perspective of the uncertainties in chemical measurements all uncertainty sources should be part of the uncertainty of the reference material. When the primary methods are not available, interlaboratorial comparisons are used as a means of certification. The material to be distributed to the laboratories should have its homogeneity confirmed. The uncertainty due to this factor will be added to the characterization uncertainty. This work presents a homogeneity stu (mais) dy of a lot of silicon metal of chemical degree where the uncertainty due to inhomogeneity is obtained using analysis of variance.
Resumo em inglês The synthesis of ZSM-5 zeolite was studied by three synthesis methods: standard synthesis, three day synthesis and synthesis employing clays (kaolin and montmorillonite). The raw materials and prepared materials were characterized by Chemical Analysis by X-Ray Fluorescence (XRF) and X-Ray Diffraction (XRD). The results show that it is possible to synthesized ZSM-5 zeolite using clays as raw materials. Kaolin gives phases of higher crystalinity than montmorillonite.
Estudo comparativo de métodos para a determinação da concentração de carbono em solos com altos teores de Fe (Latossolos)/ Comparative study of carbon quantification methods in soil with high Fe contents (Oxisols)
Resumo em inglês Soil organic matter (SOM) plays an important role in physical, chemical and biological properties of soil. Therefore, the amount of SOM is important for soil management for sustainable agriculture. The objective of this work was to evaluate the amount of SOM in oxisols by different methods and compare them, using principal component analysis, regarding their limitations. The methods used in this work were Walkley-Black, elemental analysis, total organic carbon (TOC) and t (mais) hermogravimetry. According to our results, TOC and elemental analysis were the most satisfactory methods for carbon quantification, due to their better accuracy and reproducibility.
Efeitos dos escoamentos urbanos e rurais na qualidade das águas do córrego verruga em vitória da conquista - Bahia, Brasil/ Effects of the urban and rural drainages in the quality of waters of verruga stream in vitória da conquista - Bahia, Brazil
Resumo em inglês This study examined the spatial and temporal variations of 13 physico-chemical parameters in water and sediment samples collected along the rural and urban section of Verruga Stream. The metal concentrations were determined by FAAS. The conductivity and the concentration of Na+, Cl-, and Ca2+ showed the largest variations in the urban area demonstrating that these parameters are appropriate indicators of urban contamination. The application of cluster and principal component analysis showed that the Cd2+ and Mn2+ are associated with the use of fertilizers in the rural area.
Resumo em inglês Plectranthus barbatus is largely used in the Northeast region of Brazil by the local population for treatment of digestive problems as substitute of boldo (Pneumus boldus). Phytochemical analysis of the leaf extracts of Plectranthus barbatus (Labiatae) cultivated in this region yielded two abietane diterpenoids, cyclobubatusin (1) and barbatusin (2) and a new one named 7beta-acetyl-12-deacetoxycyclobutatusin (3). The structures of the isolated compounds were established b (mais) y spectral analysis, using mainly mass spectra and ¹H and 13CNMR (1D and 2D). These procedures permitted the assignment of all chemical shifts in the diterpenoids.
Resumo em inglês One hundred fifteen cachaça samples derived from distillation in copper stills (73) or in stainless steels (42) were analyzed for thirty five itens by chromatography and inductively coupled plasma optical emission spectrometry. The analytical data were treated through Factor Analysis (FA), Partial Least Square Discriminant Analysis (PLS-DA) and Quadratic Discriminant Analysis (QDA). The FA explained 66.0% of the database variance. PLS-DA showed that it is possible to dis (mais) tinguish between the two groups of cachaças with 52.8% of the database variance. QDA was used to build up a classification model using acetaldehyde, ethyl carbamate, isobutyl alcohol, benzaldehyde, acetic acid and formaldehyde as chemical descriptors. The model presented 91.7% of accuracy on predicting the apparatus in which unknown samples were distilled.
Determinação de misturas de sulfametoxazol e trimetoprima por espectroscopia eletrônica multivariada/ Determination of sulfamethoxazole and trimethoprim mixtures by multivariate electronic spectroscopy
Resumo em inglês In this work a multivariate spectroscopic methodology is proposed for quantitative determination of sulfamethoxazole and trimethoprim in pharmaceutical associations. The multivariate model was developed by partial least-squares regression, using twenty synthetic mixtures and the spectral region between 190 and 350 nm. In the validation stage, which involved the analysis of five synthetic mixtures, prediction errors lower that 3% were observed. The predictive capacity of t (mais) he multivariate models is seriously affected by spectral changes induced by pH variations, a fact that acquires a great significance in the analysis of real samples (pharmaceuticals) that contain chemical additives.
Resumo em inglês Crystalline structures of zeolites can be studied using different representations: the internal symmetry obtained by X-Ray or neutron diffraction crystallography techniques or a systematic analysis of the basic structural units which can be arranged to build the geometries of each kind of zeolite. In this work the basic concepts of three building units, SBU (Secondary Building Units), SSU (Structural SubUnits) and PBU (Periodic Building Units) are presented. The propertie (mais) s of the resulting crystalline structures are discussed (pores, cavities, channels), describing the influence of each one of these properties in processes of physical-chemical interest. Representative case studies of known zeolite crystalline structures are also discussed in terms of their space group classification.
Constituintes químicos isolados de simira glaziovii (K. schum) steyerm. e a atribuição dos deslocamentos químicos dos átomos de carbono e hidrogênio do alcalóide ofiorina e seus derivados/ Chemical constituents from simira glaziovii (K. schum) steyerm. and ¹H and 13C NMR assignments of ophiorine and its derivatives
Resumo em inglês Chromatographic fractionation of bark extracts from Simira glaziovii (Rubiaceae) afforded the steroids beta-sitostenone, stigmastenone, beta-sitosterol and stigmasterol, methyl trans-4-hidroxy-3-methoxycinamate (1), the alkaloids harmane (2) and the new stereoisomer of ophiorine B (3). The structures were established by ¹H and 13C NMR, including 2D techniques and mass spectral analysis, of the natural products and pentaacetyllyalosidic acid (4a) and beta-carboline monote (mais) rpene tetraacetylglucoside (5, 1,22-lactamlyaloside) derivatives obtained by chemical transformations.
Constituintes químicos e avaliação do potencial alelopático de Adiantum tetraphyllum Humb. & Bonpl. Ex. Willd (Pteridaceae)/ Chemical composition and evaluation of allelopathic potentials of Adiantum tetraphyllum Humb. & Bonpl. Ex. Willd (Pteridaceae)
Resumo em inglês Chemical studies of green leaves of A. tetraphyllum afforded beta-sitosterol, a mixture containing the ethyl esters of long chain carboxylic acids, 30-normethyl-lupan-20-one, hopan-22-ol, phytol, phyten-3(20)-1,2-diol, quercetin and quercetin-3-O-beta-D-glucoside. The structures of the compounds were elucidated by spectroscopic and GC analysis. The allelopathic potentials of the crude ethanolic extract and fractions were evaluated against Lactuca sativa (letuce) and Allium cepa (onion) seeds.
Constituintes químicos e atividade inseticida dos extratos de frutos de Trichilia elegans E T. catigua (Meliaceae)/ Chemical constituents and insecticidal activity from fruits extracts of Trichilia elegans AND T. catigua (Meliaceae)
Resumo em inglês Phytochemical investigation of the fruits extracts of Trichilia elegans and Trichilia catigua (Meliaceae) has led to the identification of the limonoids 11β-acetoxyobacunone, cedrelone, methylangolensate and epimeric mixture of photogedunin besides known coumarins (scoparone, scopoletin, umbeliferone) and the steroids stigmasterol, β-sitosterol, sitostenone and campesterol. The structures of the compounds were proposed by spectroscopic analysis and comparison wi (mais) th literature data. An evaluation of the insecticidal activity of the fruits extracts of Trichilia ssp. was carried out and the extracts of T. elegans revealed to have strong insecticidal activity and the extracts of T. catigua showed moderate larval mortality on Spodoptera frugiperda.
Constituintes químicos e atividade antioxidante de extratos das folhas de Terminalia fagifolia Mart. et Zucc/ Chemical constituents and antioxidant activity from leaves extracts of Terminalia fagifolia Mart. et Zucc
Resumo em inglês Phytochemical investigation of ethanolic leaves extracts of T. fagifolia led to the isolation of (+)-catechin, sitosterol-3-O-β-D-glucopyranoside, α- and β-tocopherol, a mixture of lupeol, α- and β-amyrin, sitosterol and a mixture of glicosid flavonoids (CP-13). The structures of these compounds were identified by ¹H and 13C NMR spectral analysis and comparison with literature data. Absolute configuration of the catechin was determinate by circul (mais) ar dichroism. Antioxidant activity (EC50), evaluated by 2,2-diphenyl-1-picrylhidrazyl (DPPH) assay system, decreased in the order: (+)-catechin > hydroalcoholic fraction > CP-13 > aqueous fraction > EtOH extract.
Resumo em inglês Phytochemical investigation of the hexane extract of fruit shells of Copaifera langsdorffii Desf. (Caesalpinioideae) afforded ent-kaur-16-en-19-oic acid, polyalthic acid, nivenolide and the mixture of caryophyllene oxide and ent-kaur-16-en-19-oic acid. The chloroform extract of unripe seeds led to the isolation of coumarin and the GC/MS analysis of the extract allowed the identification of 81.8% of the fatty acid composition after hydrolysis followed by methylation. The m (mais) ain fatty acid identified was oleic acid (33.1%). The isolation of all secondary metabolites was accomplished by modern chromatographic methods and the structure determination was accomplished by spectrometric methods (IR, MS, NMR ¹H and 13C).
Resumo em inglês The phytochemical investigation of the wood extracts of Senna reticulata (Leguminoseae) yielded six anthraquinones: chrysophanol, physcion, aloe-emodin, 1,3,8-trihydroxyanthraquinone, 3-methoxy-1,6,8-trihydroxyanthraquinone, emodin and the chrysophanol-10,10' bianthrone. The triterpenes a and b-amirin, the steroids b-sitosterol and stigmasterol as well as the flavonoid kaempferol were also identified. The structures were established by spectral analysis, including two-dim (mais) ensional NMR techniques. It is the first report of 1,3,8-trihydroxyanthraquinone and 3-methoxy-1,6,8-trihydroxyanthraquinone in higher plants.
Resumo em inglês The chemical investigation of the hexane and ethanol extracts from aerial parts of Vernonia chalybaea conducted to the isolation and characterization of a new aliphatic tetrahydroxyl ether, along with a series of known compounds such as 4 α,10 α-epoxyaromadendrane, friedelin, taraxasteryl acetate, pseudotaraxasteryl acetate, lupeyl acetate, lupeol, α-amiryn, β-amiryn, β-sitosterol, stigmasterol, 2,3-dimethyl-1,2,3-tri-hydroxybuthanol, angophorol, (mais) angophorol-7-O-glucoside, angophorol-7-O-rutinoside, 3,7-dimethoxy-5,3',4'-trihydroxyflavone and acacetin. The structures of all compounds were determined by spectroscopic analysis and comparison with published spectral data.
Resumo em inglês The chemical composition of the ethanolic extract of the leaves and roots from Philodendron imbe Schott was investigated. The main constituents isolated the leaves were beta-sitosterol one polyprenoid hexaprenol, and 6beta-hydroxy-stigmast-4-en-3-one, a steroid, not yet reported in the Philodendron gender. A mixture of constituents, namely, ethyl myristoleate, alpha-bisabolol, ethyl isopalmitate, 3-octadecenyl-phenol and the major component ethyl palmitate, were isolated (mais) from the roots. Structure elucidation of these secondary metabolites was accomplished by spectrometric analysis, including 1D and 2D NMR experiments such as ¹H, ¹H and ¹H,13C-COSY.
Constituintes químicos de Ottonia corcovadensis Miq. da floresta Amazônica: atribuição dos deslocamentos químicos dos átomos de hidrogênio e carbono/ Chemical constituents of Ottonia corcovadensis Miq. from Amazon forest: ¹h and 13c chemical shift assignments
Resumo em inglês In an ethanolic extract of leaves of Ottonia corcovadensis (Piperaceae) were identified sixteen terpenoids of essential oil and the three flavonoids 3',4',5,5',7-pentamethoxyflavone (1), 3',4',5,7-tetramethoxyflavone (2) and 5-hydroxy-3',4',5',7-tetramethoxyflavone (3) and cafeic acid (4). Two amides (5 and 6) were isolated from an ethanolic extract of the roots. The structures were established by spectral analysis, meanly NMR (1D and 2D) and mass spectra. Extensive NMR a (mais) nalysis was also used to complete ¹H and 13C chemical shift assignments of the flavonoids and amides. The components of the essential oil were identified by computer library search, retention indices and visual interpretation of mass spectra.
Resumo em inglês Chemical studies of the leaves of L. divaricata afforded 3beta-p-hydroxybenzoyl-tormentic acid, a triterpene with an ursene-type skeleton, a mixture whose main compound was an oleanene derivative, the maslinic acid, a C-glycoside flavone, vitexin and glucopyranosylsitosterol. A flavonoid, characterized as (-)-epicatechin, which belongs to the flavan-3-ol class, was isolated from the stem's bark. The structures of the compounds were elucidated by spectroscopic analysis. Th (mais) e antibacterial, antifungal and antiproliferative activities of the crude methanolic extracts of leaves and bark were evaluated and the antibacterial properties of the fractions of the barks were also investigated.
Resumo em inglês The chemical study of the barks of the stem and roots of Bombacopsis glabra (Bombacaceae) led to the isolation and identification of 5-hydroxy-3,7,4'-trimethoxyflavone (1), 5-hydroxy-3,6,7,4'-tetramethoxyflavone (2), the naphtoquinone isohemigossypolone (3), the ester triacontil p-coumarate (4) besides lupeol and a mixture of beta-sitosterol and stigmasterol. Their structures were elucidated by spectroscopic analysis, including IR, ¹H and 13C NMR and MS. All these compounds, except 3, were isolated for the first time in the family.
Resumo em inglês Chemical investigation of Arrabidaea samydoides resulted in the isolation of the flavone chrysin; five triterpenes: lupeol, ursolic acid, 3b,16a-dihydroxy-urs-12-ene, uvaol, and erythrodiol; and two sterols: sitosterol and stigmasterol. The structures of these compounds were established by spectroscopic analysis. This paper deal with the first phytochemical study of Arrabidaea samydoides.
Resumo em inglês Chemical investigation of the leaves of Alchornea glandulosa (Euphorbiaceae) afforded a mixture of b-sitosterol and stigmasterol, the terpenoid loliolide, the guanidine alkaloid N-1,N-2,N-3-triisopentenylguanidine and the phenolic compound corilagin. The structures of these compounds were elucidated by spectroscopic analysis. The antimicrobial and antiproliferative properties of the crude methanolic extract of the leaves and of fractions from its fractionation, were investigated against a series of bacteria and fungi, as well as against four human cancer cell lines.
Constituintes químicos das folhas de Senna spectabilis (DC) Irwin & Barneby var. excelsa (Schrad.) Irwin & Barneby/ Chemical compounds of leaves from Senna spectabilis (DC) Irwin & Barneby var. excelsa (Schrad.) Irwin & Barneby
Resumo em inglês From leaves of Senna spectabilis var. excelsa were isolated caffeine, the triterpenes lupeol, α-amyrin, β-amyrin, cycloeucalenol, friedelin and ursolic, oleanolic and betulinic acids, besides the steroids sitosterol and stigmasterol and their respective glucosides. The structures of these compounds were established by spectroscopic analysis including two-dimensional NMR methods and comparison with published spectral data. This paper deals with the first report of these compounds in S. spectabilis var. excelsa.
Resumo em inglês Phytochemical investigation of the bark of Cenostigma macrophyllum (Leguminosae-Caesapinioideae) resulted in the isolation and identification of valoneic acid dilactone, ellagic acid, lupeol, alkyl ferulate, four free sterols (cholesterol, campesterol, stigmasterol and sitosterol), a mixture of sitosteryl ester derivatives of fatty acids, sitosterol-3-O-beta-D-glucopyranoside, stigmasterol-3-O-beta-D-glucopyranoside and saturated and unsaturated fatty acids. The structure (mais) s of the isolated compounds were identified by ¹H and 13C NMR spectral analysis and comparison with literature data. The mixtures of 3-beta-hydroxysterols and fatty acids were analysed by GC/MS.
Resumo em inglês The phytochemical analysis of the ethanol extract trunk bark of Amburana cearensis allowed the isolation and identification of twelve constituents: coumarin, sucrose, two phenol acids (vanillic acid and protocatechuic acid), five flavonoids (afrormosin, isokaempferide, kaempferol, quercetin and 4'-methoxy-fisetin), a phenol glucoside (amburoside A) and a mixture of glucosilated b-sitosterol and stigmasterol. Their structures were elucidated by spectroscopic methods such a (mais) s IR, MS, ¹H and 13C NMR, including uni and bidimensional techniques, in addition to comparison with literature data.
Constituintes químicos da ascídia didemnum psammatodes (sluiter, 1895) coletada na costa cearense/ Chemical constituent from the ascidian didemnum psammatodes (sluiter, 1895) collecter on the shores of ceara state
Resumo em inglês Chemical investigation of the methanolic extract of the ascidian Didemnum psammatodes has led to the identification of the nucleosides 2'-deoxyuridine (1), thymidine (2), 2'-deoxyinosine (3) and 2'-deoxyguanosine (4), the steroids cholestanol, cholestanone and stigmasterol in mixture and batyl alcohol plus two analogs, 1-heptadecyloxy-2,3-propanediol and 1-nonadecyloxy-2,3-propanediol in mixture. Their structures were proposed by NMR, MS and comparison with literature data and GC-MS analysis.
Resumo em inglês Chemical investigation of the MeOH extract of the leaves of Machaonia brasiliensis (Rubiaceae) resulted in the isolation and identification of 3beta-O-beta-glucopyranosyl stigmasterol, 3beta-O-beta-glucopyranosyl sitosterol, secologanoside, 7-O-beta-glucopyranosyl quercetagetin, 4,5-O-dicaffeoylquinic acid and 5-O-caffeoylquinic acid. The structures of these compounds were established by spectroscopic analysis, including 2D NMR experiments. The chemotaxonomic relevance of the isolation of secologanoside is discussed.
Conceitos de química dos ingressantes nos cursos de graduação do Instituto de Química da Universidade de São Paulo/ Chemistry concepts held by freshmen students of the Institute of Chemistry, University of São Paulo
Resumo em inglês A diagnostic instrument was developed to evaluate the basic chemistry concepts held by freshmen students of the three Chemistry undergraduate courses offered by the University of São Paulo. The instrument minimizes the use of algorithms or memorization by students and values high-order cognitive skills. Analysis of the students' performances reveals systematic use of "displacement reaction" as an algorithm and a mechanical use of Le Chatelier's Principle. Failure in comp (mais) rehending the chemical equation and chemical language drives students to alternative models for chemical reactions in aqueous solution. For instance, reaction would occur between "ionic pairs" and/or between species situated in separate compartments.
Composição elementar do material particulado presente no aerossol atmosférico do município de Sete Lagoas, Minas Gerais/ Elemental composition of the particulate matter present in the atmospheric aerosols of Sete Lagoas, MG
Resumo em inglês The main objective of this study was the identification of sources generating particulate matter in the atmospheric aerosols of Sete Lagoas, Minas Gerais. The measurement of the mineral composition was accomplished by X-ray diffractometry and the elemental concentration by neutron activation analysis. The results showed that Al, Cl, Cu, Fe, K, Mg and Na are the predominant chemical elements in the total suspended particles (TPS). The presence of Na, Ba, Cl, Cu, Eu, Fe and (mais) Sm in those particles with aerodynamic diameter smaller than 10 µm (PM10), indicates that soil dust and ceramic and pig iron industries are the main sources of air quality degradation in the region.
Composição química volátil, em diferentes estádios de maturação, de manga 'Tommy Atkins' produzida no Vale do São Francisco/ Volatile chemical composition of mango fruit 'Tommy Atkins', cultivated in São Francisco Valley, at different stages of maturity
Resumo em inglês The effect of the maturation stages on the volatile chemical composition of mango fruit cv. Tommy Atkins, cultivated in São Francisco Valley, was investigated using SPME. GC/MS and GC-FID analysis allowed the identification of 32 compounds, consisting mainly of monoterpenes. δ-3-Carene was the major component in all the stages, while α-terpinolene, trans-β-caryophyllene e α-pinene succeded each other as the second most abundant constituent, during the (mais) ripening. The aroma of the ripe fruit was characterized by presence of short-chain ethyl esters (C2-C6), whereas the green mango contained the highest concentration of δ-3-carene. Furthermore, some terpenes were detected exclusively at one of the stages.
Resumo em inglês Behavior of mercury in soil profiles with archaeological black earth (ABE) and surroundings area (SA) from Sítio Ilha de Terra, Caxiuanã, can provide information on anthropogenic activity of the Amazonian habitat. The samples of ABE and SA soil profiles were submitted to mineralogical chemical (total and sequential) analysis. The data show that the Hg occurs mainly in goethite and kaolinite in the two soil profiles. The highest concentrations of Hg and Fe are observed i (mais) n the SA profile. These results indicate that the prehistoric human occupation contributed to the decrease of the concentration of Hg in soil ABE from Caxiuanã.
Resumo em inglês An analytical comparison of three different techniques for quantitative profile of esters in cachaça is reported. The Ministério da Agricultura Pecuária e Abastecimento (MAPA) recommends the use of GC/FID or volumetry. Despite being laborious and lacking in chemical speciation, the volumetric technique for total ester content shows to be appropriate, reproducible, and accurate for the analysis of cachaça. However, the GC/FID suggested by MAPA, considering only ethyl a (mais) cetate, shows inaccuracy, underestimating the total ester content by a median factor of 72%, mainly due to the absence of ethyl lactate analysis. On the other hand, the GC/MS technique that comprises the analysis and speciation of nine esters, including ethyl lactate, proved to be reproducible, simple, fast and accurate for the analysis of total ester content in cachaça. Thus, the total ester content results obtained using GC/FID must be considered with precaution.
Resumo em inglês A dataset of chemical properties of the elements is used herein to introduce principal components analysis (PCA). The focus in this article is to verify the classification of the elements within the periodic table. The reclassification of the semimetals as metals or nonmetals emerges naturally from PCA and agrees with the current SBQ/IUPAC periodic table. Dataset construction, basic preprocessing, loading and score plots, and interpretation have been emphasized. This acti (mais) vity can be carried out even when students with distinct levels of formation are together in the same learning environment.
Resumo em inglês In order to elucidate the traditional classification of archaeological artefacts, a multielemental analytical method for characterisation of its micro and macro chemical constituents. combined with statistical multivariate analysis for classification, were used. Instrumental thermal neutron activation analysis, for elemental chemical determination, and three statistical methods: discriminant, cluster and modified cluster analysis were applied. The statistical results obta (mais) ined for the samples from Iquiri, Quinari and Xapuri archaeological phases were in good agreement with the conventional archaeological classification. Iaco and Jacuru archaeological phase were not characterised as homogenous groups. Iquiri phase were the most distinct in relation to the other analysed groups. An homogeneous group for 54% collected samples at the Los Angeles site was also found, this could be characterised as a new archaeological phase.
Resumo em inglês The production of cashew apple wine has the purpose of minimizing the wastage in the Brazilian cashew production. Knowing that the cashew apple fermentation produces a good cashew wine, a study of alcoholic fermentation kinetics of the cashew apple and the physico-chemical characterization of the product were made. The cashew wine was produced in an stirred batch reactor. The results of the physico-chemical analysis of volatiles, residual sugars, total acidity and pH of c (mais) ashew wine showed that their concentrations were within the standard limits established by the Brazilian legislation for fruit wines.
In this study eight samples of monofloral honey from Portugal, selected from four different botanical origins: Eucalyptus spp., Erica spp., Lavandula spp. And Citrus spp. were studied. For each monofloral honey two samples from different producers were analysed. Several analyses were carried out: mo...
Caracterização físico-química de queijo prato por espectroscopia no infravermelho e regressão de mínimos quadrados parciais/ Physico-chemical characterization of prato cheese by infrared spectroscopy and partial least squares regression
Resumo em inglês In this work an analytical methodology for the determination of relevant physicochemical parameters of prato cheese is reported, using infrared spectroscopy (DRIFT) and partial least squares regression (PLS). Several multivariate models were developed, using different spectral regions and preprocessing routines. In general, good precision and accuracy was observed for all studied parameters (fat, protein, moisture, total solids, ashes and pH) with standard deviations comp (mais) arable with those provided by the conventional methodologies. The implantation of this multivariate routine involves significant analytical advantages, including reduction of cost and time of analysis, minimization of human errors, and elimination of chemical residues.
Caracterização dos níveis de elementos químicos em solo, submetido a diferentes sistemas de uso e manejo, utilizando espectrometria de fluorescência de raios-x por energia dispersiva (EDXRF)/ Characterization of chemical elements in soil submitted to different systems use and management by energy dispersive x-ray fluorescence spectrometry (EDXRF)
Resumo em inglês This study aimed to evaluate the chemical elements levels in soil, submitted to different management systems and use by the Energy Dispersive X-Ray Fluorescence Spectrometry - EDXRF. The systems were T1 - agro forestry (SAF), T2 - Native Field (CN), T3 - Native Forest (NM), T4 - Tillage Forest (PF); T5 - conventional tillage system (SPC) and T6 - System tillage (NT). Samples were collected at 0-10 and 10-20 cm, dried and ground for analysis in EDX-720. The soil showed no (mais) difference in the average concentrations of chemical elements analyzed in the profiles, but the systems presented different concentrations of metal elements, and T3 had the highest K, Ca and Zn at 0-10 cm and higher contents of K, Ca, Cu, Zn and Mn in the layer of 10-20 cm.
Resumo em inglês This work presents the results of morphological and physical-chemical characteristics of a sugar cane bagasse ash material sample produced under controlled burning conditions. The investigation was carried out by analyzing chemical composition, X-ray diffraction, 29Si nuclear magnetic resonance, morphology, thermal analysis, particle size, specific surface, and density. Moreover, the pozzolanic activity of the ash was evaluated by pozzolanic activity index and Chapelle's (mais) method. The results suggest that the sugar cane bagasse ash has adequate properties to be used as pozzolan in construction materials.
Resumo em inglês Five samples of natural clays denominated: diatomite, CN-20, CN-29, CN-40 and CN-45 from Aliança Latina LTDA were characterized by differents supplementary techniques such as: XRD, chemical analysis, adsorption N2 measurements, infrared spectroscopy analysis, thermogravimetric analysis. Clays were tested in adsorption of blue methylene. All of isotherms adjust in a model of physics adsorption with formation of multilayers, however in the case of diatomite was a favorable (mais) adsorption (type II) and the CNs were a not favorable adsorption (type III). In the case of CNs had flocculation of clay in high concentration of coloring.
Caracterização de amostras petroquímicas e derivados utilizando cromatografia gasosa bidimensional abrangente (GCxGC)/ Characterization of petrochemical samples and their derivatives by comprehensive two-dimensional gas chromatography
Resumo em inglês The goal of this article is to discuss the application of comprehensive two-dimensional gas chromatography (GCxGC) to petrochemical samples. The use of GCxGC for petroleum and petroleum derivatives characterization, through group type analysis, or BTEX (benzene, toluene, ethylbenzene, xylenes), total aromatic hydrocarbons, polyaromatic hydrocarbons, sulfur-containing, oxygen-containing, and nitrogen-containing compounds is presented. The capability of GCxGC to provide add (mais) itional specific chemical information regarding petroleum processing steps, such as dehydrogenation of linear alkanes, the Fischer-Tropsch process, hydrogenation and oligomerization is also described. In addition, GCxGC analyses of petrochemical biomarkers and environmental pollutants derived from petrochemicals are reported.
Resumo em inglês The chemical analysis of the acetone, chloroform, toluene and methanol extracts of a pitch sample was carried out by IR and GC-MS, leading to the identification of sixty nine compounds, including fatty acids, alcohols and hydrocarbons. Analysis of the acetone extractive of a eucalyptus wood used in Brazil for pulp production was also carried out, resulting in identification of fifty nine compounds, including mainly fatty acids, phenolic compounds, beta-sitosterol and othe (mais) r steroids. This analysis showed that pitch formation had a contribution from wood extractives and other sources of contamination. The results obtained and the methodology applied can be used by the pulp industry to develop new methods of pitch control.
Resumo em inglês Gravimetric and Bailey-Andrew methods are tedious and provide inflated results. Spectrofotometry is adequate for caffeine analysis but is lengthy. Gas chromatography also is applied to the caffeine analysis but derivatization is needed. High performance liquid chromatography with ultraviolet detection (HPLC-UV) and reversed phase is simple and rapid for xanthine multianalysis. In HPLC-UV-gel permeation, organic solvents are not used. HPLC-mass spectrometry provides an une (mais) quivocal structural identification of xanthines. Capillary electrophoresis is fast and the solvent consumption is smaller than in HPLC. Chemometric methods offer an effective means for chemical data handling in multivariate analysis. Infrared spectroscopy alone or associated with chemometries could predict the caffeine content in a very accurate form. Electroanalytical methods are considered of low cost and easy application in caffeine analysis.
CGAR E CGAR-EM na análise dos constituintes químicos isolados do extrato hexanico de Sebastiania argutidens (Euphorbiaceae)/ HRGC and HRGC-MS in the analysis of the chemical constituents isolated from hexanic extract of Sebastiania argutidens (Euphorbiaceae)
Resumo em inglês The fractionation column with SiO2 of the hexane extract of Sebastiania argutidens (Euphorbiaceae) yielded fractions containing hydrocarbons, carboxylic acids, sterols and pentacyclic triterpenes. Besides, one fraction showed the presence of several methyl esters, including four uncommon long chain palmitate esthers as minor components. The characterization of these chemical constituents have been done by High Resolution Gas Chromatography (HRGC) and HRGC coupled to Mass (mais) Spectrometry (GC/MS). Campesterol, stigmasterol, b-sitosterol, glutin-5-en-3-ol were identified by HRGC co-injection with standards.
Resumo em inglês Biodiesel was obtained by transesterification of babassu oil in anhydrous ethanol and methanol, employing NaOH as catalyst. The products obtained were characterized by physico-chemical and thermogravimetric analysis. It could be concluded that the properties of the two types of biodiesel (ethanolic and methanolic) are very similar when compared with diesel oil.
Avaliação da contaminação do Igarapé do Sabino (Bacia do Rio Tibiri) por metais pesados, originados dos resíduos e efluentes do Aterro da Ribeira, em São Luís, Maranhão/ Evaluation of contamination on Sabino streamlet (Basin Rio Tibiri) by heavy metals originated from waste and effluents of the Ribeira landfill, in São Luis island, state of Maranhão, Brazil
Resumo em inglês This work aimed to carry out an environmental monitoring in sabino narrow river (affluent of Tibiri Basin, in São Luís - MA, Brazil), in order to verify the main environmental impacts caused by effluent residues from Ribeira landfill. Chemical analysis and bibliographic and cartographic researches on this ecosystem were also carried out. In addition, heavy metals, such as Hg, Pb and Zn, were investigated in water samples by ICP-MS technique. It was observed that the con (mais) tents of such heavy metals were above the tolerance limits established by the Brazilian legislation, showing a strong impact level on the evaluated ecosystem.
Avaliação da biodegradação de matrizes porosas à base de hidroxiapatita para aplicação como fontes radioativas em braquiterapia/ Evaluation of the biodegradation of porous hydroxyapatite matrices for application as radioactive sources in brachytherapy
Resumo em inglês Porous ceramic materials based on calcium phosphate compounds (CPC) have been studied aiming at different biomedical applications such as implants, drug delivery systems and radioactive sources for brachytherapy. Two kinds of hydroxyapatite (HAp) powders and their ceramic bodies were characterized by a combination of different techniques (XRF, BET method, SEM, ICP/AES and neutron activation analysis - NAA) to evaluate their physico-chemical and microstructural characteris (mais) tics in terms of chemical composition, segregated phases, microstructure, porosity, chemical and thermal stability, biodegradation and incorporation of substances in their structures. The results revealed that these systems presented potential for use as porous biodegradable radioactive sources able to be loaded with a wide range of radionuclides for cancer treatment by the brachytherapy technique.
Aplicação da química quântica computacional no estudo de processos químicos envolvidos em espectrometria de massas/ Application of computational quantum chemistry to chemical processes involved in mass spectrometry
Resumo em inglês The field of application of mass spectrometry (MS) has increased considerably due to the development of ionization techniques. Other factors that have stimulated the use of MS are the tandem mass spectrometry (MS/MS) and sequential mass spectrometry (MSn) techniques. However, the interpretation of the MS/MS and MSn data may lead to speculative conclusions. Thus, various quantum chemical methods have been applied for obtaining high quality thermochemical data in gas phase. (mais) In this review, we show some applications of computational quantum chemistry to understand the formation and fragmentation of gaseous ions of organic compounds in a MS analysis.
The antioxidant activity of Portuguese honeys was evaluated considering the different contribution ofentire samples and phenolic extracts. Several chemical and biochemical assays were used to screen theantioxidant properties of entire honeys with different colour intensity and phenolic extracts: r...
Pigments from two master-pieces of Ethiopian art of the 17th c. are analyzed by Raman micro-spectography technic. One is an illuminated manuscript of the Miracles of Mary (BnF Eth Abb 114), the other the mural painting of Abba Antonios church (Gondar), today kept in Paris. Both were commissioned in ...
Resumo em inglês This review presents some characteristics related to slurry sampling in trace analysis in terms of its advantages, limitations and applications, as well as the latest advance in this area, such as mechanization, chemical modifiers, stabilization agents and others. The reviewed applications include foods, biological and geological materials.
Resumo em inglês The chemical composition of two specimens of Esenbeckia grandiflora, collected in the south and northeast regions of Brazil, was investigated. In this study, three β-indolopyridoquinazoline alkaloids from the leaves (rutaecarpine, 1-hydroxyrutaecarpine) and roots (euxylophoricine D) were isolated for the first time in this genus. In addition, the triterpenes α-amyrin, β-amyrin, α-amyrenonol, β-amyrenonol, 3α-hydroxy-ursan-12-one, and 3α- (mais) hydroxy-12,13-epoxy-oleanane, the coumarins auraptene, umbelliferone, pimpinelin, and xanthotoxin, the furoquinoline alkaloids delbine and kokusaginine, and the phytosteroids sitosterol, stigmasterol, campesterol and 3β-O-β-D-glucopyranosylsitosterol were also isolated from the leaves, twigs, roots and stems of this species. Structures of these compounds were established by spectral analysis.
Resumo em inglês The spread of Brasília isn't accompanied by correct support of land occupation, situation that is reflected in water quality. Under the optics of land use and occupation, working with multivariate statistics as main tool, water physical and chemical quality of Gama Catchment were assessed. During two years samples were collected and analyzed for 24 parameters. The statistical analysis showed the influence of civil buildings, agricultural activities and the best statistical parameters to a quickly assessment: nitrate, ammonia, suspended solids and aluminium.
Resumo em inglês In this paper historical aspects of analytical pyrolysis, the equipment used, the fundamentals and the mechanisms of pyrolysis of different polymeric materials are discussed. The latest work on analytical pyrolysis applied to various types of synthetic and natural samples is reviewed. Current applications of this technique that are discussed include identification of microorganisms, analysis of trace compounds by forensic laboratories, investigation of food and agricultur (mais) al products, study of the chemical composition of wood, authentication and conservation of artworks, and the study of environmental and geochemical samples.
Resumo em inglês This work presents an evolution profile of labels and containers of commercial chemicals employed in laboratories since 1870. Most chemicals were made in Germany before the Second World War, after which many other manufacturers arrived on the Brazilian market. North-american products were dominant in the 1940s, but Brazilian chemicals have increased their participation along time. Labels presented increasingly more information, from originally simple names of the compound (mais) s at the beginning of the XXth century to the data presented today such as chemical formulae, safety regards and detailed chemical analysis. The raw material for container manufacturing also changed: glass was dominant until the 1950s, but nowadays plastic flasks are preferred whenever possible. Cork covers were replaced by screw caps. The diversity of commercial products also sharply increased with time, especially after the 1950s, following the many new and specific applications of chemicals for research and commercial purposes.
Análise multivariada de parâmetros físico-químicos em amostras de vinhos tintos comercializados na região metropolitana do Recife/ Multivariate analysis of phisico-chemical parameters in samples of red wines sold in the metropolitan area of Recife
Resumo em inglês The Brazilian legislation requires analysis of certain parameters to classify a wine and allow its commercialization. Some physico-chemical and some color parameters were determined in this work in samples of different red wines sold in the metropolitan area of Recife. Multivariate analysis comprising principal component analysis and hierarchical cluster analysis was employed to distinguish the analyzed wines. The results for pH, chloride concentration, color parameters a (mais) nd ammonium content were the most important variables for sample classification. It was also possible to classify the wines as soft or dry wines and amongst the soft wines we could determine two out of four winegrowing producers.
Análise multivariada de atributos microbiológicos e químicos do solo em florestas com Araucaria angustifolia/ Multivariate analysis of soil microbiological and chemical attributes in forests with Araucaria angustifolia
Resumo em português Araucaria angustifolia é uma espécie de árvore ameaçada de extinção no Brasil e pouco se conhece sobre os atributos edáficos dessas florestas. Este estudo foi realizado com o objetivo de identificar diferenças entre áreas com araucária naturais e reflorestadas, com base em atributos microbiológicos e químicos do solo, por meio de métodos multivariados, como a análise canônica discriminante (ACD) e a análise de correlação canônica (ACC). As áreas estuda (mais) das incluem: 1. floresta nativa com araucária (NF); 2. reflorestamento de araucária (R); 3. reflorestamento de araucária submetido a incêndio acidental (RF); e 4. pastagem natural com araucárias nativas e ocorrência de incêndio (NPF). Foram selecionadas, ao acaso, quinze árvores de araucária por área e sob a copa de cada uma delas foram retiradas três amostras de solo, em três épocas contrastantes. A ACD foi aplicada aos atributos microbianos: C da biomassa microbiana (CBM), respiração basal (C-CO2) e quociente metabólico (qCO2), enquanto a ACC foi aplicada aos atributos microbianos e químicos do solo [pH (CaCl2), C orgânico total (COT) e teores de P, K, Ca, Mg e (H+Al). Os atributos microbianos e químicos do solo apresentaram alta correlação canônica, com destaque para o CBM e C-CO2, entre os atributos microbianos, e para COT e P, entre os atributos químicos do solo. A ACC mostrou que 52 % da variação total dos atributos microbianos é explicada pela variação dos atributos químicos, e 36 % da variação total dos atributos químicos é explicada pelos atributos microbianos do solo das áreas estudadas. A ACD identificou que a contribuição de cada atributo microbiano para a separação das áreas sofreu variação ao longo do tempo, e discriminou o CBM como sendo o atributo microbiano mais importante, seguido pelo C-CO2. ACC e ACD são importantes ferramentas no estudo de indicadores de qualidade do solo. Resumo em inglês Araucaria angustifolia is an endangered tree species in Brazil and little is known about the soil attributes of these pine forests. This study was carried out to identify differences between natural and reforested Araucaria areas, in terms of soil microbiological and chemical attributes, with multivariate canonical discriminant analysis (CDA) and canonical correlation analysis (CCA). The studied areas included: 1. native forest with Araucaria (NF); 2. Araucaria reforestat (mais) ion (R); 3. Araucaria reforestation burnt by an accidental fire (RF); and 4. native grass pasture with native Araucaria and burnt by an intense accidental fire (NPF). In each area, 15 pine trees were selected and three soil samples collected from under each tree crown, in three different seasons. The CDA was applied to the soil microbiological attributes: carbon of microbial biomass (CMB), basal respiration (C-CO2) and metabolic quotient (qCO2), while CCA was performed with the soil microbiological and soil chemical attributes [pH (CaCl2), total organic carbon (TOC), and the contents of P, K, Ca, Mg, and H+Al]. The canonical correlation between soil microbiological and chemical attributes was highly significant, with a higher contribution of CMB and C-CO2 to the microbiological attributes, and of TOC and P to the chemical attributes. The CCA indicated that the variation of the chemical attributes can explain 52 % of the total data variability of the microbiological attributes, and the soil microbiological attributes of the areas 36 % of the total data variability of the chemical attributes. The CDA suggested that the contribution of each microbiological attribute to the discrimination of the areas was season-dependent, and discriminated CMB as the most important microbiological indicator, followed by C-CO2. The tools CCA and CDA proved to be essential in the study of soil quality indicators.
Resumo em português Os óleos vegetais comestíveis foram introduzidos na dieta humana em substituição as gorduras animais nas últimas décadas sendo amplamente consumidos em todo o mundo. O presente artigo descreve o desenvolvimento de uma metodologia para análise de aldrin, dieldrin, endrin e endosulfan em óleos vegetais por cromatografia gasosa de alta resolução (HRGC) utilizando-se extração em fase sólida (SPE). As médias de recuperação dos pesticidas estiveram entre 70 e 110%. Resumo em inglês Vegetable oil were introduced in human diet in the last decade to change the use of animal fats. The chemical products althrought utilized in correct manner can cause residues in food bring to healt there be a necessity of a constant monitoring of the concentration level the several agricultural products. The answer to this necessity has motivated the development of several of a methodology for simultaneous analysis of aldrin, dieldrin, endrin and endosulfan in vegetable oils by HRGC, using solid phase extraction (SPE) using silica and XAD-2. The recovery was 70-110%
Resumo em inglês The conformational equilibrium for two 5,5' biphenyl lignin models have been analyzed using a quantum mechanical semiempirical method. The gas phase and solution structures are discussed based on the NMR and X-ray experimental data. The results obtained showed that the observed conformations are solvent-dependent, being the geometries and the thermodynamic properties correlated with the experimental information. This study shows how a systematic theoretical conformational analysis can help to understand chemical processes at a molecular level.
Resumo em inglês Coffee is one of the beverages most widely consumed in the world and the "cafezinho" is normally prepared from a blend of roasted powder of two species, Coffea arabica and Coffea canephora. Each one exhibits differences in their taste and in the chemical composition, especially in the caffeine percentage. There are several procedures proposed in the literature for caffeine determination in different samples like soft drinks, coffee, medicines, etc but most of them need a (mais) sample workup which involves at least one step of purification. This work describes the quantitative analysis of caffeine using ¹H NMR and the identification of the major components in commercial coffee samples using 1D and 2D NMR techniques without any sample pre-treatment.