A powder X-ray diffraction method for detection of polyprenylated benzophenones in plant extracts associated with HPLC for quantitative analysis

A robust, direct, rapid and non-destructive X-ray diffraction crystallography method to detect the polyprenylated benzophenones 7-epi-clusianone (1) and guttiferone A (2) in extracts from Garcinia brasiliensis is presented. Powder samples of benzophenones 1 and 2, dried hexane extracts from G. brasiliensis seeds and fruit`s pericarp, and the dried ethanolic extract from G. brasiliensis seeds were unambiguously characterized by powder X-ray diffractometry. The calculated X-ray diffraction peaks from crystal structures of analytes 1 and 2, previously determined by single-crystal X-ray diffraction technique, were overlaid to those of the experimental powder diffractograms, providing a practical identification of these compounds in the analyzed material and confirming the pure contents of the powder samples. Using the X-ray diffraction crystallography method, the studied polyprenylated benzophenones were selectively and simultaneously detected in the extracts which were mounted directly on sample holder. In addition, reference materials of the analytes were not required for analyses since the crystal structures of the compounds are known. High performance liquid chromatography analyses also were comparatively carried out to quantify the analytes in the same plant extracts showing to be in agreement with X-ray diffraction crystallography method. (C) 2010 Elsevier B.V. All rights reserved.

The onset of flood basalt volcanism, Northern Parana Basin, Brazil: A precise U-Pb baddeleyite/zircon age for a Chapeco-type dacite

We report the first U-Pb baddeleyite/zircon date for a felsic volcanic rock from the Parana Large Igneous Province in south Brazil. The new date of 134.3 +/- 0.8 Ma for a hypocrystalline Chapeco-type dacite from Ourinhos (northern Parana basin) is an important regional time marker for the onset of flood basalt volcanism in the northern and western portion of the province. The dated dacite was erupted onto basement rocks and is overlain by a high-Ti basalt sequence, interpreted to be correlative with Pitanga basalts elsewhere. This new U-Pb date for the Ourinhos dacite is consistent with the local stratigraphy being slightly older than the few reliable step-heating (40)Ar/(39)Ar dates currently available for overlying high-Ti basalts (133.6-131.5 Ma). This indicates an similar to 3 Ma time span for the building of the voluminous high-Ti lava sequence of the Parana basin. On the other hand, it overlaps the (40)Ar/(39)Ar dates (134.8-134.1 Ma) available for the stratigraphically older low-Ti basalt (Gramado + Esmeralda types) and dacite-rhyolite (Palmas type) sequences from South Brazil, which is consistent with the short-lived character of this volcanism and its rapid succession by the high-Ti sequence. (C) 2010 Elsevier B.V. All rights reserved.

Effects of milk supplementation with skim milk powder, whey protein concentrate and sodium caseinate on acidification kinetics, rheological properties and structure of nonfat stirred yogurt

Milk supplementation with milk proteins in four different levels was used to investigate the effect on acidification and textural properties of yogurt. Commercial skim milk powder was diluted in distilled water, and the supplements were added to give different enriched-milk bases; these were heat treated at 90 degrees C for 5 min. These mixtures were incubated with the bacterial cultures for fermentation in a water bath, at 42 degrees C, until pH 4.50 was reached. Chemical changes during fermentation were followed by measuring the pH. Protein concentration measurements, microbial counts of Lactobacillus bulgaricus and Streptococcus thermophilus, and textural properties (G`, G ``, yield stress and firmness) were determined after 24 h of storage at 4 degrees C. Yogurt made with milk supplemented with sodium caseinate resulted in significant properties changes, which were decrease in fermentation time, and increase in yield stress, storage modulus, and firmness, with increases in supplement level. Microstructure also differed from that of yogurt produced with milk supplemented with skim milk powder or sodium caseinate. (C) 2009 Elsevier Ltd. All rights reserved.

Discrimination of geomorphic surfaces with multivariate analysis of soil attributes in sandstone - basalt lithosequence

O conceito de superfície geomórfica permite uma interligação entre os diferentes ramos da ciência do solo, tais como geologia, geomorfologia e pedologia. Esta associação favorece a compreensão da distribuição espacial dos solos na paisagem, e torna possível compreender o comportamento dos atributos do solo, que estão principalmente relacionadas com a estratigrafia e formas do relevo. Assim, este estudo visa à aplicação da estatística multivariada para categorizar superfícies geomórficas em uma litossequência arenito-basalto, de modo a fornecer uma base para a avaliação do solo em áreas afins. A área de estudo está localizada no município de Pereira Barreto, São Paulo, Brasil. A área escolhida possui 530 hectares, onde foram localizadas e mapeadas três superfícies geomórficas (I, II e III). Na área, 134 amostras foram coletadas nas profundidades de 0,0-0,2 m e 0,8-1,0 m, foram determinados os conteúdos de areia, silte e argila, pH em CaCl2, conteúdo de MO, P, Ca, Mg, K, Al e H+Al. Com base nos resultados, foram realizadas a análise univariada e multivariada de variância, clusters e principal componente, a fim de comparar as três superfícies geomórficas. A análise estatística univariada dos atributos do solo não foi eficiente na identificação das três superfícies geomórficas. Utilizando-se os atributos físicos e químicos do solo, as técnicas estatísticas multivariada permitiram à separação dos três grupos de corpos naturais do solo que foram equivalentes as três superfícies geomórficas mapeadas. Estes resultados são interessantes, pois demonstram a viabilidade da utilização de classificação numérica das superfícies geomórficas para ajudar no mapeamento de solo.

Structural characterization and Curie temperature determination of a sodium strontium niobate ferroelectric nanostructured powder

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

Solid-liquid transition in Nb powder determined by third harmonic susceptibility

Measurements of the third harmonic of the AC-susceptibility were employed to determine the boundaries of the linear regime of the magnetic response of Nb powder. Non-linear contributions to the magnetic response reveal the occurrence of a structured phase, disappearing as the vortex lattice melts to the liquid state. A systematic study of the third harmonic was conducted to determine how its onset temperature depends on experimental parameters, such as the frequency and amplitude of the excitation field. The melting line (ML) has been extracted from the onset temperature measured at low-frequencies and low-excitation fields in the presence of DC magnetic fields. The study indicates that the ML can be described by a 3D vortex-glass model, except at lower fields, where the system experiences a depinning crossover, and the best description of the experimental data is provided by a 3D Bose-glass model. (c) 2008 Elsevier B. V. All rights reserved.

Magnetic response of superconducting mesoscopic-size YBCO powder

In this work it is reported the magnetic behavior of submicron and mesoscopic-size superconducting YBCO powders, prepared by a modified polymeric precursors method. The grain size and microstructure were analyzed using scanning electron microscopy ( SEM). Measurements of magnetization and AC-susceptibility as a function of temperature were performed with a quantum design SQUID magnetometer. Our results indicated significant differences on the magnetic propreties, in connection with the calcination temperature and the pressure used to pelletize the samples. This contribution is part of an effort to study vortex dynamics and magnetic properties of submicron and mesoscopic-size superconducting samples. (C) 2008 Elsevier B. V. All rights reserved.

Powder Diffraction of Components Subject to Corrosion in Fuse Cutouts with CeramicInsulation

Aiming identification of the components most affected by corrosion under saline environment conditions, we have carried out X-ray diffraction measurements in ceramic and bond materials, all in the powder form. The ceramic is analyzed before and after thermal annealing at 1000 degrees C, showing the same DRX peaks, although better defined after annealing. Identification suggests the presence of Al(6)Si(2)O(13) (Mullite) and SiO(2) (Quartz). Analysis of the junction (bond) material shows similar peaks, but a metallic preponderance is observed. Thermal annealing of the junction is done at much lower temperature, because it melts in the range 135 degrees C-170 degrees C, when a whitish smoke begins to show up along with strong sulfur odor.

Production of a low young modulus titanium alloy by powder metallurgy

Titanium alloys have several advantages over ferrous and non-ferrous metallic materials, such as high strengthto-weight ratio and excellent corrosion resistance. A blended elemental titanium powder metallurgy process has been developed to offer low cost commercial products. The process employs hydride-dehydride (HDH) powders as raw material. In this work, results of the Ti-35Nb alloy sintering are presented. This alloy due to its lower modulus of elasticity and high biocompatibility is a promising candidate for aerospace and medical use. Samples were produced by mixing of initial metallic powders followed by uniaxial and cold isostatic pressing with subsequent densification by isochronal sintering between 900 up to 1600 °C, in vacuum. Sintering behavior was studied by means of microscopy and density. Sintered samples were characterized for phase composition, microstructure and microhardness by X-ray diffraction, scanning electron microscopy and Vickers indentation, respectively. Samples sintered at high temperatures display a fine plate-like alpha structure and intergranular beta. A few remaining pores are still found and density above 90% for specimens sintered in temperatures over 1500 °C is reached.

Surface Corrosion of Ti-16Si-4B Powder Alloy Implanted With Nitrogen by Plasma-Based Technique

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

Determination of the properties of an experimental glass polyalkenoate cement prepared from niobium silicate powder containing fluoride

Objectives. The purpose of this paper is to modify the conventional calcium fluoro-aluminosilicate glass, which is used in the formation of glass ionomer cements (CIGs) by the niobium addition and to study the properties of GICs obtained.Materials and methods. Sol-gel process was used to prepare the powder at lower temperature than fusion method. Glass-ceramic powder obtained in this way was used to prepare the GICs. The properties such as working and setting times, microhardness and diametral tensile strength were evaluated for the experimental GICs and a commercial luting cement.Results. The ideal powder:liquid (P:L) ratio determined to prepare the experimental GICs was equal to 1:1. The cements prepared using this ratio showed working and setting times similar to the commercial GICs. in mechanical tests it was observed that microhardness and diametral tensile strength of the experimental GICs decreased significantly with the reduction of P:L ratio. on the other hand, the results obtained in microhardness tests indicated that the presence of niobium was a positive factor.Significance. The chemical process allows the development of glass-ceramic powder at 600 degrees C which is the goal of the present paper. It was concluded that GICs containing niobium might be used in dental applications and these results encourage further researches on other compositions. (c) 2007 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Physicochemical characterization of collagen fibers and collagen powder for self-composite film production

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

INFLUENCE of ENCAPSULATING MATERIALS on WATER SORPTION ISOTHERMS of VACUUM-DRIED PERSIMMON PULP POWDER

Water sorption isotherms for vacuum-dried persimmon pulp (PP) powder were determined in the temperature range of 20-50C, and the effects of maltodextrin (MD) or gum arabic (GA) addition on the water sorption behavior of the dried powders were analyzed. Several models were evaluated to fit the experimental data and the Guggenheim-Anderson-de Boer model was selected as the most adequate to describe the observed behavior. Addition of encapsulants affected the isotherms: at the same water activity, PP powder with added GA (PP + GA) or MD (PP + MD) presented lower equilibrium water content than pure PP and were less affected by temperature variations. Samples of PP + MD presented lower equilibrium moisture content than those of PP + GA. The isosteric heats of sorption of pulp powders with encapsulants were higher (less negative) than those of PP, suggesting that there are more active polar sites in PP than in pulp powder containing encapsulants.PRACTICAL APPLICATIONSThe choice of persimmon to carry out this work was due to the large persimmon production available in Brazil; moreover, persimmon pulp is rich in vitamin C, vitamin A and iron, as well as in phenolic compounds. Drying of fruit pulps with high sugar content presents technical difficulties because the hygroscopicity and thermoplasticity of the resulting powders when exposed to high temperature and relative humidity. For this reason, addition of high-molar-mass biopolymers, such as maltodextrin or gum arabic, is a strategy to aid drying and to improve storage stability. Knowledge of water sorption isotherms and net isosteric heats of sorption is important to various food processing operations, including drying, storage and packaging. They are useful in calculating time and energy consumptions during drying, modeling moisture changes during storage and predicting shelf life of food products.

Role of enthalpy and entropy in moisture sorption behavior of pineapple pulp powder produced by different drying methods

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