Energy-dispersive X-ray fluorescence analysis of a pre-Columbian funerary gold mask from the Museum of Sican, Peru

A funerary gold mask from the Museum of Sican, Ferranafe, Peru was analyzed in 30 different areas using a portable equipment using energy-dispersive X-ray fluorescence. It was deduced from the measurements that the main sheet of the mask and the majority of the pendants have a similar composition and are made of tumbaga, which means a poor gold alloy enriched at the surface by depletion gilding, and have a similar `equivalent` gilding thickness of about 5 mu m. The nose, also on tumbaga, has different composition and a thickness of about 8 mu m. The clamps are on gilded or on silvered copper. The red pigment dispersed on the surface of the mask is cinnabar. Copyright (C) 2009 John Wiley & Sons, Ltd.

X-ray spectroscopy applied to radiation shielding calculation in mammography

The protective shielding design of a mammography facility requires the knowledge of the scattered radiation by the patient and image receptor components. The shape and intensity of secondary x-ray beams depend on the kVp applied to the x-ray tube, target/filter combination, primary x-ray field size, and scattering angle. Currently, shielding calculations for mammography facilities are performed based on scatter fraction data for Mo/Mo target/filter, even though modern mammography equipment is designed with different anode/filter combinations. In this work we present scatter fraction data evaluated based on the x-ray spectra produced by a Mo/Mo, Mo/Rh and W/Rh target/filter, for 25, 30 and 35 kV tube voltages and scattering angles between 30 and 165 degrees. Three mammography phantoms were irradiated and the scattered radiation was measured with a CdZnTe detector. The primary x-ray spectra were computed with a semiempirical model based on the air kerma and HVL measured with an ionization chamber. The results point out that the scatter fraction values are higher for W/Rh than for Mo/Mo and Mo/Rh, although the primary and scattered air kerma are lower for W/Rh than for Mo/Mo and Mo/Rh target/filter combinations. The scatter fractions computed in this work were applied in a shielding design calculation in order to evaluate shielding requirements for each of these target/filter combinations. Besides, shielding requirements have been evaluated converting the scattered air kerma from mGy/week to mSv/week adopting initially a conversion coefficient from air kerma to effective dose as 1 Sv/Gy and then a mean conversion coefficient specific for the x-ray beam considered. Results show that the thickest barrier should be provided for Mo/Mo target/filter combination. They also point out that the use of the conversion coefficient from air kerma to effective dose as 1 Sv/Gy is conservatively high in the mammography energy range and overestimate the barrier thickness. (c) 2008 American Association of Physicists in Medicine.

Metal location and thickness in a multilayered sheet by measuring K alpha/K beta, L alpha/L beta and L alpha/L gamma X-ray ratios

When a multilayered material is analyzed by means of energy-dispersive X-ray fluorescence analysis, then the X-ray ratios of K alpha/K beta, or L alpha/L beta and L alpha/L gamma, for an element in the multilayered material, depend on the composition and thickness of the layer in which the element is situated, and on the composition and thickness of the superimposed layer (or layers). Multilayered samples are common in archaeometry, for example, in the case of pigment layers in paintings, or in the case of gilded or silvered alloys. The latter situation is examined in detail in the present paper, with a specific reference to pre-Columbian alloys from various museums in the north of Peru. (C) 2009 Elsevier B.V. All rights reserved.

Fracture and fatigue of natural fiber-reinforced cementitious composites

This paper presents the results of an experimental study of resistance-curve behavior and fatigue crack growth in cementitious matrices reinforced with eco-friendly natural fibers obtained from agricultural by-products. The composites include: blast furnace slag cement reinforced with pulped fibers of sisal, banana and bleached eucalyptus pulp, and ordinary Portland cement composites reinforced with bleached eucalyptus pulp. Fracture resistance (R-curve) and fatigue crack growth behavior were studied using single-edge notched bend specimens. The observed stable crack growth behavior was then related to crack/microstructure interactions that were elucidated via scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDS). Fracture mechanics models were used to quantify the observed crack-tip shielding due to crack-bridging. The implications of the results are also discussed for the design of natural fiber-reinforced composite materials for affordable housing. (C) 2009 Elsevier Ltd. All rights reserved.

Relative roles of biogenic emissions and Saharan dust as ice nuclei in the Amazon basin

Some aerosol particles, known as ice nuclei, can initiate ice formation in clouds, thereby influencing precipitation, cloud dynamics and the amount of incoming and outgoing solar radiation. In the absence of biomass burning, aerosol mass concentrations in the Amazon basin are low(1). Tropical forests emit primary biological particles directly into the atmosphere; secondary organic aerosols form from the emission and oxidation of biogenic gases(2). In addition, particles derived from biomass burning in central Africa, marine aerosols, and windblown dust from North Africa(3-5) often reach the central part of the Amazon basin during the wet season. The contribution of these aerosol sources to ice nucleation in the region is uncertain. Here we present observations of the concentration and elemental composition of ice nuclei in the Amazon basin during the wet season. Using transmission electron microscopy combined with energy-dispersive X-ray spectroscopy, we show that ice nuclei are primarily composed of carbonaceous material and dust. We show that biological particles dominate the carbonaceous fraction, whereas import of Saharan dust explains the intermittent appearance of dust-containing nuclei. We conclude that ice-nucleus concentration and abundance can be explained almost entirely by local emissions of biological particles supplemented by import of Saharan dust. Using a simple model, we tentatively suggest that the contribution of local biological particles to ice nucleation is increased at higher atmospheric temperatures, whereas the contribution of dust particles is increased at lower temperatures.

On the release of metronidazole from natural rubber latex membranes

The controlled release of drugs can be efficient if a suitable encapsulation procedure is developed, which requires biocompatible materials to hold and release the drug. In this study, a natural rubber latex (NRL) membrane is used to deliver metronidazole (MET), a powerful antiprotozoal agent. MET was found to be adsorbed on the NRL membrane, with little or no incorporation into the membrane bulk, according to energy dispersive X-ray spectroscopy. X-ray diffraction and FTIR spectroscopy data indicated that MET retained its structural and spectroscopic properties upon encapsulation in the NRL membrane, with no molecular-level interaction that could alter the antibacterial activity of MET. More importantly, the release time of MET in a NRL membrane in vitro was increased from the typical 6-8 h for oral tablets or injections to ca. 100 h. The kinetics of the drug release could be fitted with a double exponential function, with two characteristic times of 3.6 and 29.9 h. This is a demonstration that the induced angiogenesis known to be provided by NRL membranes can be combined with a controlled release of drugs, whose kinetics can be tailored by modifying experimental conditions of membrane fabrication for specific applications. (C) 2010 Elsevier B.V. All rights reserved.

Ethanol steam reforming for production of hydrogen on magnesium aluminate-supported cobalt catalysts promoted by noble metals

The performance of noble metal (Pt, Ru, Ir)-promoted Co/MgAl(2)O(4) catalysts for the steam reforming of ethanol was investigated. The catalysts were characterized by energy-dispersive X-ray spectroscopy, Xray diffraction, UV-vis diffuse reflectance spectroscopy, temperature-programmed reduction, temperature-programmed oxidation and X-ray absorption near edge structure (XANES). The results showed that the formation of inactive cobalt aluminate was suppressed by the presence of a MgAl(2)O(4) spinel phase. The effects of the noble metals included a marked lowering of the reduction temperatures of the cobalt surface species interacting with the support. It was seen that the addition of noble metal stabilized the Co sites in the reduced state throughout the reaction. Catalytic performance was enhanced in the promoted catalysts, particularly CoRu/MgAl(2)O(4), which showed the highest selectivity for H(2) production. (C) 2009 Elsevier B.V. All rights reserved.

Raman spectroscopy analysis of structural photoinduced changes in GeS(2) + Ga(2)O(3) thin films

Photoexpansion and photobleaching effects have been observed in amorphous GeS(2) + Ga(2)O(3) (GGSO) thin films, when their surfaces were exposed to UV light. The photoinduced changes on the surface of the samples are indications that the structure has been changed as a result of photoexcitation. In this paper, micro-Raman, energy dispersive X-ray analysis (EDX) and backscattering electrons (BSE) microscopy were the techniques used to identify the origin of these effects. Raman spectra revealed that these phenomena are a consequence of the Ge-S bonds` breakdown and the formation of new Ge-O bonds, with an increase of the modes associated with Ge-O-Ge bonds and mixed oxysulphide tetrahedral units (S-Ge-O). The chemical composition measured by EDX and BSE microscopy images indicated that the irradiated area is oxygen rich. So, the present paper provides fundamental insights into the influence of the oxygen within the glass matrix on the considered photoinduced effects. (C) 2010 Elsevier B.V. All rights reserved.

Effect of the catalyst composition in the Pt-x(Ru-Ir)(1-x)/C system on the electro-oxidation of methanol in acid media

The effect of variations in the composition for ternary catalysts of the type Pt-x(Ru-Ir)(1-x)/C on the methanol oxidation reaction in acid media for x values of 0.25, 0.50 and 0.75 is reported. The catalysts were prepared by the sol-gel method and characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), atomic absorption spectroscopy (AAS) and energy dispersive X-ray (EDX) analyses. The nanometric character (2.8-3.2 nm) of the sol-gel deposits was demonstrated by XRD and TEM while EDX and AAS analyses showed that the metallic ratio in the compounds was very near to the expected one. Cyclic voltammograms for methanol oxidation revealed that the reaction onset occur at less positive potentials in all the ternary catalysts tested here when compared to a Pt-0.75-Ru-0.25/C (E-Tek) commercial composite. Steady-state polarization experiments (Tafel plots) showed that the Pt-0.25(Ru-Ir)(0.75)/C catalyst is the more active one for methanol oxidation as revealed by the shift of the reaction onset towards lower potentials. In addition, constant potential electrolyses suggest that the addition of Ru and Ir to Pt decreases the poisoning effect of the strongly adsorbed species generated during methanol oxidation. Consequently, the Pt-0.25 (Ru-Ir)(0.75)/C Composite catalyst is a very promising one for practical applications. (c) 2007 Elsevier B.V. All rights reserved.

Synthesis, Characterization, and Electrocatalytic Activity toward Methanol Oxidation of Carbon-Supported Pt(x)-(RuO(2)-M)(1-x) Composite Ternary Catalysts (M = CeO(2), MoO(3), or PbO(x))

Carbon-supported platinum is commonly used as an anode electrocatalyst in low-temperature fuel cells fueled with methanol. The cost of Pt and the limited world supply are significant barriers for the widespread use of this type of fuel cell. Moreover, Pt used as anode material is readily poisoned by carbon monoxide produced as a byproduct of the alcohol oxidation. Although improvements in the catalytic performance for methanol oxidation were attained using Pt-Ru alloys, the state-of-the-art Pt-Ru catalyst needs further improvement because of relatively low catalytic activity and the high cost of noble Pt and Ru. For these reasons, the development of highly efficient ternary platinum-based catalysts is an important challenge. Thus, various compositions of ternary Pt(x)-(RuO(2)-M)(1-x)/C composites (M = CeO(2), MoO(3), or PbO(x)) were developed and further investigated as catalysts for the methanol electro-oxidation reaction. The characterization carried out by X-ray diffraction, energy-dispersive X-ray analysis, transmission electron microscopy, X-ray photoelectron spectroscopy, and cyclic voltammetry point out that the different metallic oxides were successfully deposited on the Pt/C, producing small and well-controlled nanoparticles in the range of 2.8-4.2 nm. Electrochemical experiments demonstrated that the Pt(0.50)(RuO(2)-CeO(2))(0.50)/C composite displays the higher catalytic activity toward the methanol oxidation reaction (lowest onset potential of 207 mV and current densities taken at 450 mV, which are 140 times higher than those at commercial Pt/C), followed by the Pt(0.75)(RuO(2)-MoO(3))(0.25)/C composite. In addition, both of these composites produced low quantities of formic acid and formaldehyde when compared to a commercially available Pt(0.75)-Ru(0.25)/C composite (from E-Tek, Inc.), suggesting that the oxidation of methanol occurs mainly by a pathway that produces CO(2) forming the intermediary CO(ads).

Immobilization of Catalysts of Biological Interest on Porous Oxidized Silicon Surfaces

The present paper deals with the immobilization of redox mediators and proteins onto protected porous silicon surfaces to obtain their direct electrochemical reactions and to retain their bioactivities. This paper shows that MP-11 and viologens are able to establish chemical bonds with 3-aminopropyltriethoxylsilane-modified porous silicon surface. The functionalization of the surfaces have been fully characterized by energy dispersive X-ray analysis (EDX) and X-ray photoelectron spectroscopy (XPS) to examine the immobilization of these mediators onto the solid surface. Amperometric and open circuit potential measurements have shown the direct electron transfer between glucose oxidase and the electrode in the presence of the viologen mediator covalently linked to the 3-aminopropyltriethoxylsilane (APTES)-modified porous silicon surfaces.

Production of hydrogen via steam reforming of biofuels on Ni/CeO(2)-Al(2)O(3) catalysts promoted by noble metals

The catalytic activity of Ni/CeO(2)-Al(2)O(3) catalysts modified with noble metals (Pt, Ir, Pd and Ru) was investigated for the steam reform of ethanol and glycerol. The catalysts were characterized by the following techniques: Energy-dispersive X-ray, BET, X-ray diffraction, temperature-programmed reduction, UV-vis diffuse reflectance spectroscopy and X-ray absorption near edge structure (XANES). The results showed that the formation of inactive nickel aluminate was prevented by the presence of CeO(2) dispersed on alumina. The promoting effect of noble metals included a decrease in the reduction temperatures of NiO species interacting with the support, due to the hydrogen spillover effect. It was seen that the addition of noble metal stabilized the Ni sites in the reduced state along the reforming reaction, increasing the ethanol and glycerol conversions and decreasing the coke formation. The higher catalytic performance for the ethanol steam reforming at 600 degrees C and glycerol steam reforming was obtained for the NiPd and NiPt catalysts, respectively, which presented an effluent gaseous mixture with the highest H(2) yield with reasonably low amounts of CO. (c) 2009 International Association for Hydrogen Energy. Published by Elsevier Ltd. All rights reserved.

Preparation and characterization of ordered intermetallic platinum phases for electrocatalytic applications

Ordered intermetallic phases of Pt with several transition metals have been prepared and their electrocatalytic properties studied. In light of these tests it is proposed that these catalysts could be used as electrodes in fuel cells, as they combine an excellent capacity to adsorb organic fuels at the Pt sites with low susceptibility to being poisoned by intermediates and reaction products at the transition-metal sites. An experimental procedure used to obtain the four intermetallic phases Pt-M (M = Mn, Pb, Sb and Sn) is described. The phases thus produced were characterized by X-ray diffraction, scanning electron microscopy with surface analysis by energy-dispersive X-ray spectrometry, scanning tunneling microscopy and X-ray photoelectron spectroscopy. The data thus obtained support the conclusion that the method described here is highly effective for the preparation of Pt-M phases featuring a range of structural and electronic modifications that will allow a useful relation to be established between their physicochemical properties and predicted electrocatalytic activity. (C) 2007 Elsevier Ltd. All rights reserved.

Microstructure and Mineral Composition of Dental Enamel of Permanent and Deciduous Teeth

Purpose: This study evaluated and compared in vitro the microstructure and mineral composition of permanent and deciduous teeth`s dental enamel. Methods: Sound third molars (n = 12) and second primary molars (n = 12) were selected and randomly assigned to the following groups, according to the analysis method performed (n = 4): Scanning electron microscopy (SEM), X-Ray diffraction (XRD) and Energy dispersive X-ray spectrometer (EDS). Qualitative and quantitative comparisons of the dental enamel were done. The microscopic findings were analyzed statistically by a nonparametric test (Kruskal-Wallis). The measurements of the prisms number and thickness were done in SEM photomicrographs. The relative amounts of calcium (Ca) and phosphorus (P) were determined by EDS investigation. Chemical phases present in both types of teeth were observed by the XRD analysis. Results: The mean thickness measurements observed in the deciduous teeth enamel was 1.14 mm and in the permanent teeth enamel was 2.58 mm. The mean rod head diameter in deciduous teeth was statistically similar to that of permanent teeth enamel, and a slightly decrease from the outer enamel surface to the region next to the enamel-dentine junction was assessed. The numerical density of enamel rods was higher in the deciduous teeth, mainly near EDJ, that showed statistically significant difference. The percentage of Ca and P was higher in the permanent teeth enamel. Conclusions: The primary enamel structure showed a lower level of Ca and P, thinner thickness and higher numerical density of rods. Microsc. Res. Tech. 73:572-577, 2010. (C) 2009 Wiley-Liss. Inc.

Interfacial interactions in concretes with silica fume and SBR latex

This paper deals with the effect of silica fume and styrene-butadiene latex (SBR) on the microstructure of the interfacial transition zone (ITZ) between Portland cement paste and aggregates (basalt). Scanning electron microscope (SEM) equipped with energy dispersive X-ray analysis system (EDX) was used to determine the ITZ thickness. In the plain concrete a marked ITZ around the aggregate particles (55 mu m) was observed, while in concretes with silica fume or latex SBR the ITZ was less pronounced (35-40 mu m). However, better results were observed in concretes with silica fume and latex SBR (20-25 mu m). (C) 2008 Elsevier Ltd. All rights reserved.