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Novel synthesis of superparamagnetic Ni-Co-B nanoparticles and their effect on superconductor properties of MgB2

A new procedure for the preparation of amorphous Ni-Co-B nanoparticles is reported, with a detailed investigation of their morphology by X-ray diffraction and transmission electron microscopy, as well as their magnetic properties. Many factors, such as chemical composition, anisotropy, size and shape of the particles, were controlled through chemical synthesis, resulting in the control of morphological and magnetic properties of the nanoparticles. Controlling pH values with ethylenediamine and using sodium dodecyl sulfate surfactant lowered the size of the nanoparticles to below 10 nm. Such a small structure and chemical disorder in nanocrystalline materials lead to magnetic properties that are different from those in their bulk-sized counterparts. The obtained nanoparticles can be used for different purposes, from pharmaceutical applications to implementations in different materials technology. The focus of this research is the synthesis of Ni-Co-B nanoparticles in a new way and studying the reaction of Ni-Co-B nanoparticles with Mg and B precursors and their effect on MgB2 properties. New nanostructures are formed in the reaction of Ni-Co-B nanoparticles with Mg: Mg2Ni, Co2Mg and possibly Mg2Co.

Can environmental constraints determine random patterns of plant species co-occurrence?

Plant community ecologists use the null model approach to infer assembly processes from observed patterns of species co-occurrence. In about a third of published studies, the null hypothesis of random assembly cannot be rejected. When this occurs, plant ecologists interpret that the observed random pattern is not environmentally constrained - but probably generated by stochastic processes. The null model approach (using the C-score and the discrepancy index) was used to test for random assembly under two simulation algorithms. Logistic regression, distance-based redundancy analysis, and constrained ordination were used to test for environmental determinism (species segregation along environmental gradients or turnover and species aggregation). This article introduces an environmentally determined community of alpine hydrophytes that presents itself as randomly assembled. The pathway through which the random pattern arises in this community is suggested to be as follows: Two simultaneous environmental processes, one leading to species aggregation and the other leading to species segregation, concurrently generate the observed pattern, which results to be neither aggregated nor segregated - but random. A simulation study supports this suggestion. Although apparently simple, the null model approach seems to assume that a single ecological factor prevails or that if several factors decisively influence the community, then they all exert their influence in the same direction, generating either aggregation or segregation. As these assumptions are unlikely to hold in most cases and assembly processes cannot be inferred from random patterns, we would like to propose plant ecologists to investigate specifically the ecological processes responsible for observed random patterns, instead of trying to infer processes from patterns

Obtenção de nanocompósitos a partir da co-coagulação da borracha nitrílica e hidrotalcita

Partículas nanoestruturadas têm sido amplamente utilizadas como carga de reforço em matrizes elastoméricas, sendo substitutos eficazes das cargas convencionais, já consagradas, como o negro de fumo, mica, sílica. Em especial, as argilas têm mostrado grande potencial ao que se refere a melhor dispersão na matriz polimérica, em função de sua elevada razão de aspecto. Dentro do vasto universo de argilominerais, as argilas aniônicas, também conhecidas hidróxido duplo lamelar (HDL), apresentam como vantagem a possibilidade de ser projetada estruturalmente para as mais diversas finalidades, ao se modificar os ânions ou os cátions, ou até mesmo combiná-los na estrutura lamelar. E dentre os métodos existentes para se preparar compósitos a base de elastômero/argila, a co-coagulação do látex, é uma forma bastante eficaz e economicamente viável, uma vez que a borracha obtida após processo de coagulação já contém a carga incorporada. Este trabalho se dedicou a avaliar o processo de co-coagulação do látex de NBR e HDL, visando a obtenção de nanocompósitos. Para tanto HDL de composição Mg/Al-CO3 foi modificado com ânions DS, DBS e ST e foram preparadas suspensões aquosas, utilizando como ferramentas de dispersão ultraturrax e ultrassom de ponteira. As variáveis de processo avaliadas foram tipo e teor de HDL, tempo de mistura látex/suspensão aquosa de HDL, quantidade de coagulante e velocidade de agitação. Por fim, os coágulos obtidos foram formulados para avaliar a influência dos HDL na cinética de vulcanização e também para determinação das propriedades mecânicas convencionais. Os resultados obtidos comprovaram que a metodologia de dispersão de hidrotalcita ao látex nitrílico de modo prévio ao processo de coagulação é uma alternativa viável para a obtenção de nanocompósitos. O uso do ultrassom de ponteira como ferramenta na dispersão aquosa de HDL contribuiu para maior estabilidade da suspensão e o ajuste nos parâmetros do sistema de coagulação, levaram a obtenção de grumos uniformes do ponto de vista macroscópico e microscópico. As micrografias dos coágulos não vulcanizados obtidas por MEV-FEG confirmaram as informações apuradas a partir dos difratogramas de raios-X que apontou a formação de um sistema parcialmente esfoliado, em função da ausência dos picos característicos da hidrotalcita, além de indicarem a coexistência de partículas em dimensões micrométrica a nanométricas em uma mesma estrutura. A composição química do HDL, com a presença de átomos de magnésio e alumínio combinados com grupos hidroxila favoreceu a redução tanto o tempo de indução como de pré-cura. As propriedades mecânicas que se mostraram mais sensíveis ao grau de dispersão da carga foram a dureza, a deformação permanente à compressão (DPC) e o módulo de tração a 300% de deformação (E300), em especial para os compósitos contendo 10% m/m de HDL natural e modificado com estearato. A resistência à chama dos nanocompósitos de NBR-HDL vulcanizados apresentou um ligeiro aumento quando comparados à NBR pura, visto que esta é uma característica própria da hidrotalcita, decorrente da sua composição química

Elemental analysis of soil samples for forensic purposes by inductively coupled plasma spectrometry - precision considerations

Major and trace elemental composition provides a powerful basis for forensic comparison of soils, sediments and rocks. However, it is important that the potential 'errors' associated with the procedures are fully understood and quantified, and that standard protocols are applied for sample preparation and analysis. This paper describes such a standard procedure and reports results both for instrumental measurement precision (repeatability) and overall 'method' precision (reproducibility). Results obtained both for certified reference materials and example soils show that the instrumental measurement precision (defined by the coefficient of variation, CV) for most elements is better than 2-3%. When different solutions were prepared from the same sample powder, and from different sub-sample powders prepared from the same parent sample, the CV increased to c. 5-6% for many elements. The largest variation was found in results for certified reference materials generated from 23 instrument runs over an 18 month period (mean CV=c. 11%). Some elements were more variable than others. W was found to be the most variable and the elements V, Cr, Co, Cu, Ni and Pb also showed higher than average variability. SiO2, CaO, Al2O3 and Fe2O3, Rb, Sr, La, Ce, Nd and Sm generally showed lower than average variability, and therefore provided the most reliable basis for inter-sample comparison. It is recommended that, whenever possible, samples relating to the same investigation should be analysed in the same sample run, or at least sequential runs.

Ranking of length-class seasonal and regional effects on dietary compositions of the co-occurring Pagrus auratus (Sparidae) and Pseudocaranx georgianus (Carangidae)

Using an effective combination of multivariate testing and ordination analyses, this study compares the extents to which the diets of two co-occurring fish species (Pagrus auratus and Pseudocaranx georgianus) are related to body size (length class), season and region and the rank order importance of those effects. Thus, volumetric dietary compositions were determined for these species on the lower west coast of Australia, where both are abundant, and for P. auratus from the mid west coast and P. georgianus from the south coast. The diet of P. auratus on the lower west coast was strongly related to body size and slightly less to season. With increasing body size, its diet shifted from predominantly ophiuroids to larger prey, such as brachyuran crabs, teleosts, echinoids and ultimately asteroids, probably reflecting a shift from foraging over soft sediments to areas over and around reefs. Seasonal changes on the lower west coast were restricted mainly to small P. auratus, while larger fish underwent seasonal changes further north. Analyses using a common size range of medium to larger P. auratus demonstrated that dietary composition differed more between regions than seasons. The relationships between diet and length class of P. georgianus on both the lower west and south coasts were less pronounced than for P. auratus and seasonal changes were restricted to the south coast, where amphipod consumption increased markedly in summer. The diet of P. georgianus was related far more to region than length class and season, with more small teleosts, small crabs, carideans and littorinids and less amphipods, isopods and small bivalves being ingested on the lower west than south coasts. Although crabs and teleosts were important typifying prey of P. auratus and P. georgianus, when co-occurring, the former predator tended to ingest greater volumes of larger and often less mobile prey. This reflects differences in dentition, jaw morphology and feeding behaviour and reduces the potential for competition for food resources. The results imply that P. auratus and P. georgianus are opportunistic feeders and that the effects of length class, season and region on dietary composition and their rank orders can vary markedly between species and for length class and season between regions for the same species.

Analysis of Degradation Data of Poly(L-lactide-co-L,D-lactic actide) and Poly(L-lactide) Obtained at Elevated and Physiological Temperatures Using Mathematical Models

The degradation of resorbable polymeric devices often takes months to years. Accelerated testing at elevated temperatures is an attractive but controversial technique. The purposes of this paper include: (a) to provide a summary of the mathematical models required to analyse accelerated degradation data and to indicate the pitfalls of using these models; (b) to improve the model previously developed by Han and Pan; (c) to provide a simple version of the model of Han and Pan with an analytical solution that is convenient to use; (d) to demonstrate the application of the improved model in two different poly(lactic acid) systems. It is shown that the simple analytical relations between molecular weight and degradation time widely used in the literature can lead to inadequate conclusions. In more general situations the rate equations are only part of a complete degradation model. Together with previous works in the literature, our study calls for care in using the accelerated testing technique.

Processing, microstructure and mechanical properties of air plasma-sprayed ceria-yttria co-stabilized zirconia coatings

Thermal barrier coatings (TBCs) are widely adopted to protect mechanical components in gas turbine engines operating at high temperature. Basically, the surface temperature of these components must be low enough to retain material properties within acceptable bounds and to extend component life. From this standpoint, air plasma-sprayed (APS) ceria and yttria co-stabilized zirconia (CYSZ) is particularly promising because it provides enhanced thermal insulation capabilities and resistance to hot corrosion. However, essential mechanical properties, such as hardness and Young's modulus, have been less thoroughly investigated. Knowledge of Young's modulus is of concern because it has a significant effect on strain tolerance and stress level and, hence, on durability. The focus of the present study was to determine the mechanical properties of APS CYSZ coatings. In particular, X-ray diffraction (XRD) is adopted for phase analysis of powders and as-sprayed coatings. In addition, scanning electron microscopy (SEM) and image analysis (IA) are employed to explore coating microstructure and porosity. Finally, the Young's modulus of the coating is determined using nanoindentation and a resonant method. The results obtained are then discussed and a cross-check on their consistency is carried out by resorting to a micromechanical model. © 2010 Blackwell Publishing Ltd.

Targetting of the ventro-intermediate nucleus using ultra-high field (7T) MRI for gamma knife surgery purposes: A pilot in vivo study on healthy subjects.

INTRODUCTION: Gamma Knife surgery (GKS) is a non-invasive neurosurgical stereotactic procedure, increasingly used as an alternative to open functional procedures. This includes targeting of the ventro-intermediate nucleus of the thalamus (e.g. Vim) for tremor. We currently perform an indirect targeting, as the Vim is not visible on current 3Tesla MRI acquisitions. Our objective was to enhance anatomic imaging (aiming at refining the precision of anatomic target selection by direct visualisation) in patients treated for tremor with Vim GKS, by using high field 7T MRI. MATERIALS AND METHODSH: Five young healthy subjects were scanned on 3 (T1-w and diffusion tensor imaging) and 7T (high-resolution susceptibility weighted images (SWI)) MRI in Lausanne. All images were further integrated for the first time into the Gamma Plan Software(®) (Elekta Instruments, AB, Sweden) and co-registered (with T1 was a reference). A simulation of targeting of the Vim was done using various methods on the 3T images. Furthermore, a correlation with the position of the found target with the 7T SWI was performed. The atlas of Morel et al. (Zurich, CH) was used to confirm the findings on a detailed analysis inside/outside the Gamma Plan. RESULTS: The use of SWI provided us with a superior resolution and an improved image contrast within the basal ganglia. This allowed visualization and direct delineation of some subgroups of thalamic nuclei in vivo, including the Vim. The position of the target, as assessed on 3T, perfectly matched with the supposed one of the Vim on the SWI. Furthermore, a 3-dimensional model of the Vim-target area was created on the basis of the obtained images. CONCLUSION: This is the first report of the integration of SWI high field MRI into the LGP, aiming at the improvement of targeting validation of the Vim in tremor. The anatomical correlation between the direct visualization on 7T and the current targeting methods on 3T (e.g. quadrilatere of Guyot, histological atlases) seems to show a very good anatomical matching. Further studies are needed to validate this technique, both by improving the accuracy of the targeting of the Vim (potentially also other thalamic nuclei) and to perform clinical assessment.

Characterization of Atrazine-Loaded Biodegradable Poly(Hydroxybutyrate-Co-Hydroxyvalerate) Microspheres

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Desenvolvimento de uma rota química alternativa de síntese de SrCo0,8Fe0,2O3- e LaNi0,3Co0,7O3- para aplicação na reação de oxidação do CO

This thesis focuses on the coprecipitation synthesis method for preparation of ceramic materials with perovskite structure, their characterization and application as catalytic material in the reaction of converting CO to CO2 developing a methodological alternative route of synthesis from the middle via oxalate coprecipitation material SrCo0,8Fe0,2O3-d. In order to check the influence of this method, it was also synthesized using a combined citrate - EDTA complexing method. The material was characterized by: X-ray diffraction (XRD), Rietveld refinement method, thermogravimetry and differential thermo analysis (TG / DTA), scanning (SEM) and transmission (TEM) electron microscopy, particle size distribution and surface analysis method BET. Both methods led to post-phase synthesis, with pH as a relevant parameter. The synthesis based on the method via oxalate coprecipitation among particles led to the crystalline phase as those obtained using a combined citrate - EDTA complexing method under the same conditions of heat treatment. The nature of the reagent used via oxalate coprecipitation method produced a material with approximately 80 % lower than the average size of crystallites. Moreover, the via oxalate coprecipitation method precursors obtained in the solid state at low temperature (~ 26 oC), shorter synthesis, greater thermal stability and a higher yield of around 90-95 %, maintaining the same order of magnitude the crystallite size that the combined citrate - EDTA complexing method. For purposes of comparing the catalytic properties of the material was also synthesized by the using a combined citrate - EDTA complexing method. The evaluation of catalytic materials SrCo0,8Fe0,2O3-d LaNi0,3Co0,7O3-d was accompanied on the oxidation of CO to CO2 using a stainless steel tubular reactor in the temperature range of 75-300 oC. The conversion CO gas was evaluated in both materials on the results shaved that the firm conversion was loves for the material LaNi0,3Co0,7O3-d

Experimental results and thermodynamic analysis of a natural gas small scale cogeneration plant for power and refrigeration purposes

In this work, experimental results are reported for a small scale cogeneration plant for power and refrigeration purposes. The plant includes a natural gas microturbine and an ammonia/water absorption chiller fired by steam. The system was tested under different turbine loads, steam pressures and chiller outlet temperatures. An evaluation based on the 1st and 2nd Laws of Thermodynamics was also performed. For the ambient temperature around 24°C and microturbine at full load, the plant is able to provide 19 kW of saturated steam at 5.3 bar (161 °C), corresponding to 9.2 kW of refrigeration at -5 °C (COP = 0.44). From a 2nd law point-of-view, it was found that there is an optimal chiller outlet temperature that maximizes the chiller exergetic efficiency. As expected, the microturbine presented the highest irreversibilities, followed by the absorption chiller and the HRSG. In order to reduce the plant exergy destruction, it is recommended a new design for the HRSG and a new insulation for the exhaust pipe. © 2013 Elsevier Ltd. All rights reserved.

Produção de etanol a 40-42ºC em uma co-cultura de Saccharomyces cerevisiae e Issatchenkia orientalis

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Caracterização físico-química e avaliação toxicológica preliminar do copolímero sulfato de condroitina-co-N-isopropilacrilamida para uso farmacêutico

A Indústria Farmacêutica utiliza polímeros em forma de nanopartículas em formulações de liberação controlada e vetorizada por possuírem baixo custo em relação a demais métodos de preparações de formas farmacêuticas, aparentemente não serem reconhecidos pelo sistema de defesa do organismo, proporcionar melhora da eficácia, diminuição da toxicidade e da dose de fármaco administrado. O sulfato de condroitina-co-Nisopropilacrilamida (SCM + NIPAAm) é um copolímero proposto para este fim, a partir da reação de um polímero sintético, o poli N-isopropilacrilamida (PNIPAAm), com características termossensíveis, com um natural, o Sulfato de Condroitina (SC), com características bioadesivas. Assim, a copolimerização pode ser capaz de somar estas propriedades e aperfeiçoar o seu uso como um veículo para liberação controlada. Este trabalho objetivou, portanto, realizar a caracterização fisico-quimica das partículas de sulfato de condroitina e Nisopropilacrilamida e do copolímero SCM+NIPAAm (2,5 % e 5%) e do SCM+PNIPAAm 2,5% e uma avaliação toxicológica parcial de um destes copolímeros que apresentar as melhores propriedades de um eficiente carreador de fármacos, selecionado a partir dos ensaios de caracterização físico-química. Para determinar a estrutura química dos sistemas particulados e analisar os seus componentes químicos, foi realizada a Espectroscopia de Ressonância Magnética Nuclear (RMN) e Espectroscopia do Infravermelho com Transformada de Fourrier (FTIR); Para analisar a morfologia das partículas, foi usado a Microscopia Eletrônica de Varredura (MEV); A Termogravimetria/ Termogravimetria Derivada e Análise Térmica Diferencial (TG/DTG) foi usada para avaliar o comportamento térmico dos sistemas particulados, bem como auxiliar na análise de Cinética de Degradação (CD, método de Flynn-Wall-Ozawa); Foi ainda realizado a técnica de degradação in vitro e a determinação carga superficial e tamanho de partículas (análise do Potencial Zeta, PZ). Para avaliar a toxicidade, foi realizado o bioensaio em microcrustáceo Artemia salina (24 e 48 h), viabilidade celular (citotoxicidade) em células PC-12 (método do MTT) e também a toxicidade aguda oral em camundongos. As análises de RMN, FTIR e MEV demonstraram semelhança quanto ao aspecto estrutural e morfológico entre os copolímeros estudados. As análises de TG demonstraram que o SCM+NIPAAm 5% apresentou maior estabilidade térmica em relação aos demais copolímeros avaliados, uma vez que sua decomposição polimérica ocorre em temperaturas superiores, em torno de 233ºC. O DTA demonstrou valores de temperaturas concordantes com os eventos térmicos de decomposição apresentados pelas curvas das análises TG. Sua estabilidade foi confirmada através da CD e estudo de degradação in vitro, apresentando, respectivamente, Ea > 100 kJ mol^-1 e perda de 48% da sua massa inicial após três meses. Além disso, SCM+NIPAAm 5% apresentou diâmetro de partícula inferior a 200 nm e índice de polidispersão de 0,35, além do PZ > -30mV, caracteristicas de um promissor candidato a carreador de fármacos. Em relação às avaliações toxicológicas, o SCM+NIPAAm 5% não apresentou toxicidade no bioensaio de A. salina (CL₅₀ > 1000) e no modelo celular avaliado, dentro das concentrações e circunstâncias de exposição estudadas. O SCM+NIPAAm 5%, na dose oral de 2000 mg/kg, não apresentou nenhum sinal evidente de toxicidade em camundongos, o que foi corroborado pela ausência de alterações anatomo-histopatológicas. A copolimerização do Sulfato de Condroitina e N-isopropilacrilamida na concentração estudada, dada suas características físico-químicas e toxicológicas preliminares, apresenta propriedades que contribuem para a proposta de um sistema que constitui uma nova forma de liberação controlada, especialmente de fármacos.

Estudo da atividade de água em co-produtos da indústria de sucos: sementes de maracujá, casca de laranja e cascas de manga

Pós-graduação em Engenharia e Ciência de Alimentos - IBILCE