Study of mural paintings by Fulvio Pennacchi in São Paulo City by mineralogical techniques

The present research deals with two mural paintings made in 1947 with the fresco technique by Fulvio Pennacchi in the Catholic Chapel of the Hospital das Clínicas (São Paulo City, Brazil), namely the Virgin Annunciation and the Supper at Emmaus. This study regards the materials and painting techniques used by the artist, based on historical research,on in situ observations and laboratory analytical techniques (stereomicroscopy,scanning electron microscopy with an energy dispersive spectrometer, X-ray diffractometry, electron microprobe, images obtained with UV-light), aiming to improve the methods of characterization of objects of our cultural heritage, and to enhance its preservation accordingly. The results lead to the identification of the plaster components and of distinct layers in the frescoes, besides further information on grain size, impurities and textures, composition of pigments, and features of deterioration, such as efflorescences. The degree of degradation of the murals painting was assessed by this way. Our data suggest that a single layer of plaster was used by Pennacchi, as a common mortar with fine- and medium-grained aggregates. Differences in texture were obtained by adding gypsum to the plaster.

Estudo do mecanismo de corrosão por pites em água do mar de aços inoxidáveis supermartensíticos microligados com Nb e Ti

Os aços inoxidáveis supermartensíticos (SMSS) são usados em ambientes agressivos devido à sua boa soldabilidade, boas propriedades mecânicas em temperaturas elevadas e superior resistência à corrosão sob tensão. Aplicações na exploração de petróleo demandam superior combinação de propriedades e os aços inoxidáveis duplex e superduplex têm sido aplicados nessa área, a despeito de seus custos elevados. Os SMSS consistem numa alternativa técnica e econômica ao uso daqueles aços. Nesse trabalho, adições de Nb e Ti foram realizadas com o intuito de minimizar o efeito de sensitização, promover o refino de grãos e foram estudados os aspectos microestruturais e a resistência à corrosão por pites em água do mar. A formação e a evolução dos pites foram acompanhadas por ensaios de corrosão, microscopia óptica e eletrônica, focalizando suas morfologias. O aço com Ti apresentou o melhor desempenho quanto à corrosão, com o maior potencial de corrosão e menor potencial de pite entre os aços em estudo. O aço com Nb, apesar de apresentar potencial de corrosão superior ao do aço sem adição, teve um potencial de pite inferior ao do mesmo.

Biocompósitos de matriz glioxal-fenol reforçada com celulose microcristalina

Glioxal pode ser obtido a partir de biomassa (como da oxidação de lipídeos) e não é tóxico ou volátil, tendo sido por isso utilizado no presente trabalho como substituto de formaldeído na preparação de resina fenólica do tipo novolaca, sendo usado como catalisador o ácido oxálico, que também pode ser obtido de fontes renováveis. A resina glioxal-fenol foi utilizada na preparação de compósitos reforçados com celulose microcristalina (CM, 30, 50 e 70% em massa), uma celulose com elevada área superficial. As imagens de microscopia eletrônica de varredura (MEV) das superfícies fraturadas demonstraram que os compósitos apresentaram boa interface reforço/matriz, consequência da elevada área superficial da CM e presença de grupos polares (hidroxilas) tanto na matriz como na celulose, o que permitiu a formação de ligações hidrogênio, favorecendo a compatibilidade entre ambas. A análise térmica dinâmico-mecânica (DMTA) demonstrou que todos os compósitos apresentaram elevado módulo de armazenamento à temperatura ambiente. Além disso, o compósito reforçado com 30% de CM apresentou baixa absorção de água, comparável à do termorrígido fenólico, que é utilizado em escala industrial. Os resultados demonstraram que compósitos com boas propriedades podem ser preparados usando elevada proporção de materiais obtidos de biomassa.

Synthesis of Fe/Ti oxides from a single source alkoxide precursor under inert atmosphere

The heterometal alkoxide [FeCl{Ti2(OPr i)9}] (1) was employed as a single source precursor for the preparation of Fe/Ti oxides under inert atmosphere. Three different synthetic procedures were adopted in the processing of 1, either employing aqueous HNO3 or HCl solutions, or in the absence of mineral acids. Products were characterised by powder X-ray diffractometry, scanning electron microscopy combined with energy dispersive X-ray spectroscopy (SEM/EDS) and Raman, electron paramagnetic resonance (EPR) and Mössbauer spectroscopies. Oxide products contained titanium(IV) and either iron(III) or iron(II), depending on reaction conditions and thermal treatment temperatures. An interesting iron(III)→iron(II) reduction was observed at 1000 ºC in the HNO3-containing system, leading to the detection of ilmenite (FeTiO3). SEM/EDS studies revealed a highly heterogeneous metal distribution in all products, possibly related to the presence of a significant content of carbon and of structural defects (oxygen vacancies) in the solids.

Obtaining high purity silica from rice hulls

Many routes for extracting silica from rice hulls are based on direct calcining. These methods, though, often produce silica contaminated with inorganic impurities. This work presents the study of a strategy for obtaining silica from rice hulls with a purity level adequate for applications in electronics. The technique is based on two leaching steps, using respectively aqua regia and Piranha solutions, which extract the organic matrix and inorganic impurities. The material was characterized by Fourier-transform infrared spectroscopy (FTIR), powder x-ray diffraction (XRD), x-ray fluorescence (XRF), scanning electron microscopy (SEM), particle size analysis by laser diffraction (LPSA) and thermal analysis.

Porcine skin as a source of biodegradable matrices: alkaline treatment and glutaraldehyde crosslinking

In this work, the modifications promoted by alkaline hydrolysis and glutaraldehyde (GA) crosslinking on type I collagen found in porcine skin have been studied. Collagen matrices were obtained from the alkaline hydrolysis of porcine skin, with subsequent GA crosslinking in different concentrations and reaction times. The elastin content determination showed that independent of the treatment, elastin was present in the matrices. Results obtained from in vitro trypsin degradation indicated that with the increase of GA concentration and reaction time, the degradation rate decreased. From thermogravimetry and differential scanning calorimetry analysis it can be observed that the collagen in the matrices becomes more resistant to thermal degradation as a consequence of the increasing crosslink degree. Scanning electron microscopy analysis indicated that after the GA crosslinking, collagen fibers become more organized and well-defined. Therefore, the preparations of porcine skin matrices with different degradation rates, which can be used in soft tissue reconstruction, are viable.

Caracterização mecânica e térmica da borracha natural formulada e vulcanizada dos clones: GT 1, IAN 873, PB 235 e RRIM 600

Neste trabalho estudou-se o desempenho mecânico e térmico de compostos de borracha natural (Hevea brasiliensis) de 4 diferentes clones (GT 1, IAN 873, PB 235 e RRIM 600) cultivados no Estado de São Paulo, assim como de uma mistura destes clones e de uma borracha comercial, GEB-1. Estas borrachas foram formuladas e vulcanizadas com tempos de 5, 7 e 9 minutos. A caracterização foi realizada por calorimetria exploratória diferencial, termogravimetria, ensaios de resistência à tração, análise dinâmico-mecânica, medidas de dureza Shore A, microscopia eletrônica de varredura e espectroscopia na região do infravermelho. Os resultados permitiram concluir que o tempo de vulcanização e o tipo de clone não influenciaram na temperatura de transição vítrea (Tg) dos compostos. Os valores de Tg obtidos por DMA foram de cerca de -62 °C, e os resultados ensaios de dureza apresentaram valores próximos de 60 para todos os compostos estudados. Os ensaios de resistência à tração mostraram que o melhor desempenho mecânico foi obtido pelo clone RRIM 600. De acordo com os resultados obtidos neste trabalho, todos os clones atingiram as propriedades reportadas na literatura, podendo ser utilizados, em princípio, nas indústrias de artefatos de borracha separadamente ou na forma de mistura.

Characterization of thiol-functionalised silica films deposited on electrode surfaces

Thiol-functionalised silica films were deposited on various electrode surfaces (gold, platinum, glassy carbon) by spin-coating sol-gel mixtures in the presence of a surfactant template. Film formation occurred by evaporation induced self-assembly (EISA) involving the hydrolysis and (co)condensation of silane and organosilane precursors on the electrode surface. The characterization of such material was performed by IR spectroscopy, thermogravimetry (TG), elemental analysis (EA), atomic force microscopy (AFM), scanning electron microscopy (SEM) and cyclic voltammetry (CV).

Membranas biológicas homólogas preservadas em solução alcalina seguida de liofilização, glicerina a 98% e por liofilização para implantação em eqüinos

Objetivou-se, neste trabalho, avaliar as alterações físico-químicas proporcionadas pelo tratamento de centros tendinosos diafragmáticos homólogos em solução alcalina seguida de liofilização, para implantação na fáscia interna do músculo reto do abdome de eqüinos. As amostras foram tratadas em períodos de 24, 48, 72, 120 e 144 horas, liofilizadas e analisadas quanto à homogeneidade, flexibilidade e resistência à sutura das amostras. Posteriormente foram caracterizadas por calorimetria exploratória diferencial e microscopia eletrônica de varredura. Para a implantação nos eqüinos, foram utilizadas amostras tratadas por 72 horas seguidas de liofilização, amostras conservadas em glicerina 98% e amostras apenas liofilizadas, que foram retiradas após uma, nove e 18 semanas para avaliar a existência de aderências. Verificou-se que a homogeneidade e a flexibilidade são diretamente proporcionais ao aumento do tempo de tratamento em solução alcalina, enquanto que a resistência é inversamente proporcional ao aumento de tempo, sendo o tratamento por 72 horas intermediário para estas características. A calorimetria exploratória diferencial mostrou que o tratamento não desnatura o colágeno presente nas amostras. Na microscopia eletrônica de varredura, observou-se que o aumento de tempo de tratamento proporciona expansão de zonas menos densas do material. Em relação à formação de aderências, as amostras apenas liofilizadas apresentaram grau máximo na formação da classificação proposta, seguida pelas amostras conservadas em glicerina 98% com grau médio e as amostras tratadas em solução alcalina e liofilizadas, que foram classificadas em grau mínimo. Concluiu-se que o tratamento por 72 horas seria mais apropriado para implantação e que a integração tissular com a parede abdominal foi melhor em relação às amostras apenas liofilizadas e às conservadas em glicerina.

Eletrodos modificados por hidróxido de níquel: um estudo de revisão sobre suas propriedades estruturais e eletroquímicas visando suas aplicações em eletrocatálise, eletrocromismo e baterias secundárias

The present review paper describes the main features of nickel hydroxide modified electrodes covering its structural and electrochemical behavior and the newest advances promoted by nanostructured architectures. Important aspects such as synthetic procedures and characterization techniques such as X-Ray diffraction, Raman and Infrared spectroscopy, Electronic Microscopy and many others are detailed herein. The most important aspect concerning nickel hydroxide is related to its great versatility covering different fields in electrochemical-based devices such as batteries, electrocatalytic systems and electrochromic electrodes, the fundamental issues of these devices are also commented. Finally, some of the newest advances achieved in each field by the incorporation of nanomaterials will be shown.

Low temperature synthesis of CdSiO3 nanostructures

We report the synthesis of single-phase, crystalline CdSiO3 nanostructures at 580ºC; to the best of our knowledge, this is the lowest temperature at which this material is reported to form. The desired phase does not form below 580ºC, since the diffraction peaks are shifted to lower angles in the material treated at 570ºC when compared to JDPDS Card No. 85-0310. The source of silicon has strong influence on the product morphology: Na2SiO3 yields single-phase CdSiO3 in needle-shaped nanostructures, while high surface area mesostructured SiO2 yields coralloid-shaped particles. Low angle X-ray diffractometry reveals that the mesostructured nature of the silica precursor is not maintained in the resulting CdSiO3. Scanning electron microscopy suggests that in this case a transition occurs between the spherical morphology of the precursor and the needle-shape morphology of the material prepared from Na2SiO3. The surface area of the silica precursor has a strong influence in the reaction, since the use of commercial silica with a lower surface area does not yield the desired product.

The venom apparatus and other morphological characters of the ant Martialis heureka (Hymenoptera, Formicidae, Martialinae)

We describe and illustrate the venom apparatus and other morphological characters of the recently described Martialis heureka ant worker, a supposedly specialized subterranean predator which could be the sole surviving representative of a highly divergent lineage that arose near the dawn of ant diversification. M. heureka was described as the single species of a genus in the subfamily, Martialinae Rabeling and Verhaagh, known from a single worker. However because the authors had available a unique specimen, dissections and scanning electron microscopy from coated specimens were not possible. We base our study on two worker individuals collected in Manaus, AM, Brazil in 1998 and maintained in 70% alcohol since then; the ants were partially destroyed because of desiccation during transport to São Paulo and subsequent efforts to rescue them from the vial. We were able to recover two left mandibles, two pronota, one dismembered fore coxa, one meso-metapropodeal complex with the median and hind coxae and trochanters still attached, one postpetiole, two gastric tergites, the pygidium and the almost complete venom apparatus (lacking the gonostylus and anal plate). We illustrate and describe the pieces, and compare M. heureka worker morphology with other basal ant subfamilies, concluding it does merit subfamilial status.

Comparative descriptions of eggs from three species of Rhodnius (Hemiptera: Reduviidae: Triatominae)

The authors describe and compare the morphological and ultrastructural characteristics of eggs from the three most recent described species of the genus Rhodnius Stål, 1859, which have not previously been studied. These species are Rhodnius colombiensis (Mejia, Galvão & Jurberg 1999), Rhodnius milesi (Carcavallo, Rocha, Galvão & Jurberg 2001) and Rhodnius stali (Lent, Jurberg & Galvão 1993). The results revealed that there are similarities in the exochorial architecture of optical microscopy and scanning electron microscopy; these include the predominance of hexagonal cells that are common to all Rhodnius species and variable degrees of lateral flattening, which is common not only to species of this genus, but also to the Rhodniini tribe. Differences in overall colour, the presence of a collar in R. milesi, a longitudinal bevel in R. stali and the precise length of R. colombiensis can be useful distinguishing features. As a result of this study, the key for egg identification proposed by Barata in 1981 can be updated.

Description of the immatures of the ant, Myrmelachista catharinae

The Neotropical ant genus Myrmelachista Roger comprises 69 described species and subspecies, and still is a poorly studied group. Larvae play a paramount role in colony nutrition in social hymenopterans and bear considerable value in the reconstruction of group phylogenies, however, they are generally neglected. Larvae of different instars of Myrmelachista catharinae Mayr (Hymenoptera: Formicidae) are herein described in detail by light and scanning electron microscopy. The number of larval instars was estimated as three based on the frequency distribution of maximum head capsule widths. The described larvae confirmed some traits typical of the genus: general shape of body and mandibles, general aspect and distribution of body hairs, and the number of sensilla on the palps and galea. Differently from other Myrmelachista larvae previously described, M. catharinae presented two distinct kinds of second instars, some additional types of body hairs, different number of antennal sensilla, and a distinct labrum shape. M. catharinae presented ten pairs of spiracles, which is the first record for this genus.

DESCRIPTION OF THE IMMATURES OF WORKERS OF THE ANT CAMPONOTUS VITTATUS (HYMENOPTERA: FORMICIDAE)

Camponotus vittatus Forel is a poorly studied Neotropical ant, which is very common in Brazil. Larval descriptions are useful to systematics, as larval characters aid with genus-level differentiation, and ant larvae lie at the basis of ant social organization. This study presents the first description of the immatures of C. vittatus with the aid of light and scanning electron microscopy. There are three instars based on the frequency distribution of larval head widths. The larvae had some characteristics typical of Camponotus, specifically, a 'pogono-myrmecoid' body shape, 10 pairs of spiracles, antennae with 3 sensilla, mature larvae with pronounced labial pseudopalps, and conspicuous 'chiloscleres' on the labrum. Unique characteristics found would include the greatest diversity of body hair types recorded in an ant larva and 'camponotoid' mandibles with 6 medial denticles over the blade. The number of antennal sensilla proved variable.